The REALCAT platform comprises two fully automated, flexible, modular robotic workstations from Chemspeed: Catimpreg and Autoplant.

Catimpreg is mainly designed to run automatically parallel syntheses of catalysts by coprecipitation and impregnation. It possesses an XYZ arm with a rotating alpha-axis and automatic tool exchange to perform automatically the following synthesis steps :

• Gravimetric solid dispensing (from mg to g) of a wide range of solid (powder, extrudates,...).
• Volumetric liquid dispensing (1 mPa.s - 200 mPa.s) and viscous liquid dispensing (>500 mPa.s).
• pH and density measurement and adjustment.
• Heating, reflux, vacuum, filtration...
• Efficient mixing by orbital shaking while preserving the extrudates.

Inert atmosphere for sensitive reagents or inert reaction conditions can be assured in the Catimpreg workstation either by inertization of the reactors (vacuum-inert gas cycles) or by inertization of the entire workstations enclosed hood.

At ambient pressure, liquid phase catalyst testing is possible using the Chemspeed Catimpreg workstation, equipped with 36 reactors. This robot allows catalytic performance tests by parallel or successive reactions...

Autoplant is mainly designed to automate parallel hydrothermal synthesis of catalyst and polymerization reactions. As Catimpreg workstation, it is possessing an X, Y and Z arm with rotating alpha-axis and automatic tool exchange to perform automatically the following synthesis steps: reagent preparation, solids and liquids dosing, filtration, extraction, evaporation, vortexing and reflux.

Eight fully automated and instrumented high pressure reactors (100 mL) are installed in the workstation. Each reactor is equipped with high pressure pump, gas flow and pressure controller. Injection of liquid and/or gas reagent, pressure (up to 80 bar) and temperature (-10°C to +250°C) in each reactor can be controlled individually. The reactor heads include an integrated reflux condenser and houses connectors for temperature and pH probes and liquid sampling. In addition, each reactor includes one feed vessel that is intended for the storage of reagents added to the reactor via the syringe pump in the course of an application. Different stirrer designs (anchor or twisted blade) can be used and are easily exchanged according to the reagent nature (gas, liquid or solid). Indirect online viscosity measurements can be carried out.

As in Catimpreg inert atmosphere for sensitive reagents or inert reaction conditions can be assured in the Autoplant workstation either by inertization of the reactors (vacuum inert gas cycles) or by inertization of the entire workstations enclosed hood. Moreover, hood is equipped with 4 gloves for some manually tasks under inert atmosphere. It is also equipped with H₂O and O₂ detectors permitting to control the atmosphere inside the workstation.

This robotic platform allows testing in parallel of 8 catalysts for a variety of solution phase homogeneous and heterogeneous catalyzed reactions. It also provides all the flexibility to optimize integrated reaction sequences.

The M4 TORNADO is an energy dispersive micro X-ray spectrometer that can be used for elemental analysis of materials but also for coating analysis (determination of thickness and composition). The special analytical task for the M4 Tornado is the analysis of small sample points (point or multi-points) but also for elemental distributions in a line (LineScan) and areas (Mapping). This unit is able to analyze a wide range of samples (solid, powder and liquid). The elements that can be determined by this instrument unit range from sodium (Na) to uranium (U). Quantification of element is based on Fundamental-Parameter model (Standardless) suitable for variable sample types and applications.

This instrument includes :

• A large sample chamber (600 x 350 x 260 mm) allowing to work under vacuum.
• A precise X-Y-Z stage controlled by joystick to position precisely the sample.
• Two X-Ray tubes: Rh (poly-capillary) and W (collimator) and 5 filters.
• X-Ray optics: poly-capillary optics with two size of excitation areas: 20 µm and 200 µm and a collimator for W (spot size of 1 mm).
• A Silicon-Drift-Detector (SDD) X Flash.
• An optical microscope: 2 cameras to position the sample accurately et 1 for the chamber observation.

Sample acquisition time varies according to the sample nature and its composition (from few seconds to few minutes). The machine can operate for one sample analysis or for an automatic multi-wells analysis.

The ICP-OES is an analytical technique used for quantitative, semi-quantitative or qualitative determination of elements constituting the catalysts. More than 70 elements can be determined by ICP-EOS at trace level. This instrument analysis only digested catalyst by acid or base digestion procedures. An automated digester was associated to ICP in order to digest the solid/powder catalyst surely and precisely.

This instrument includes :

• A source of emission: Argon gas through a torch (axial view) surrounded by a copper coil connected to a radio frequency (RF) generator.
• A concentric nebulizer.
• Optics : diffracting grating and polychromator.
• A coupled charged detector (CCD) covering a spectral range from 167 to 785 nm.
• An autosampler with 3 racks of 60 positions each and an automatic arm to collect samples.

A sample analysis takes about 2 min, ensuring a fast analysis.

Vulcan 42S is an automated digestion system combining the two essential steps in sample preparation prior to analysis by ICP: sample digestion followed by sample work-up.

It performs with precision and security the following steps :

• Volumetric liquid dispensing (up to 5 different acids).
• Heating/cooling and temperature monitoring of a block of 42 positions ensuring thermal uniformity for samples (up to 230 °C ± 1 °C).
• Level volume adjustment of the tube.
• Mixing samples.
• Dilution and/or transfer of a known amount of each sample prior to analysis.

Almost all the digester components are made of plastic avoiding corrosion with the use of acids. Questron use a highly efficient fume removal after neutralizing the acid vapor thereby avoiding contamination between samples.

The Flash Smart equipment is an automated elemental analyzer for carbon (C), hydrogen (H), nitrogen (N), sulfur (S) and oxygen (O) present in solid, liquid and viscous samples. CHNS characterization can be performed in a single analysis run and oxygen determination in a second run, independently. CHNS simultaneous determinations can be performed by "Flash" combustion of the samples weighed in tin containers. The C, N, H and S are detected as: N 2 , CO 2 , H 2 O and SO 2 respectively. The produced gases are then separated on a chromatographic column and detected by a Thermal Conductivity Detector (TCD). Oxygen is determined by pyrolysis. Samples are weighed in silver containers and introduced into the reactor containing nickel-coated carbon. Oxygen is determined as carbon monoxide. After separation from other products it is detected by TCD. The equipment is associated with a high-precision micro-metric balance (Mettler Toledo) for sample preparation. The analyzer configuration includes:

• 32 positions auto-sampler
• Two thermally independent reaction furnaces containing:
  • A combustion reactor for CHNS
  • A pyrolysis chamber for O 2
• Two analytical circuits installed simultaneously and used alternately for CHNS and Oxygen determinations
• A TCD

X-Ray Diffractometer D8 Discover is able to analysis the chemical structure and orientation of a crystal, to identify (comparison with the reference data from ICDD files) and quantify the crystalline phases and determine the crystallite size.

This instrument includes :

• A goniometer located in a X-Ray insulating enclosure. The goniometer is mounted on a podium allowing the measurement in a transmission and reflection mode without disassembly of the accessories.
• An X-Ray tube in Cu (Kα) radiation (λ=0.1538 nm).
• A motorized X-Y-Z stage for easy and automatic move of sample position during a multi-wells analysis.

The analysis duration time varies between 1 min to few minutes according to the precision of the analysis.

Fourier transform infrared spectroscopy Tensor 37 is used for measurements in the mid infrared (MIR) to characterize the chemical composition of liquid or solid samples. The microplate extension HTS-XT allows the application of FT-IR spectroscopy as method for high-throughput screening. This technique is used to determine the nature of chemical bonds present in a sample and to characterize the molecular groups to obtain information for the conformation and possible interactions.

This instrument includes :

• An MIR Source (spectral range from 8000 to 550 cm^-1).
• An Interferometer.
• An HTS-XT compartment for multi-wells plate use (variety of plates with 24, 48 and 96 well can be used for solid and liquid samples).
• It is equipped with 2 detectors: a photoelectric detector (MCT) working in reflection mode and a pyroelectric detector (DTGS) working in transmission mode.
• A second compartment of the IR can be used for a single sample with a KBr pellet. It is equipped with a RT / DLaTGS D301 detector.

The sample acquisition is very fast (few seconds) permitting a rapid characterization of the synthetized catalyst.

Raman spectroscopy is a non-destructive method to determine the chemical structure, the molecules configuration and the crystallinity and also to study intra- and intermolecular force (hydrogen bond) and molecular orientation (polarization) of a solid or liquid, organic or inorganic sample.

Raman Xplora allows a local study on of the sample by focusing on a single point or multiple points (spatial resolution of 1-2 µm) or a mapping (study of the sample distribution on an area of the sample ≈ 1 mm).

Further tools associated to Raman are available to perform an operando study to characterize the catalyst.

This instrument includes :

• Optic microscope Olympus BX41 equipped with 3 objectives (10X STD, 50X LWD, 100X STD).
• High definition camera with transmission and reflection illumination.
• Multiple laser wavelengths (532 nm, 638 nm et 785 nm) and an automated laser wavelength switching.
• A monochromator (Czerny Turner) and a CCD detector cooled by Peltier effect.
• A motorized X-Y-Z stage for easy move of sample position.
• A large range of options and accessories.

Sample acquisition time varies according to the sample nature and its composition (from 1 second to few minutes). The machine can analysis automatically and with efficiency a multi-wells plate (24 samples).

The REALCAT platform is equipped with a combined system for automatic powder analysis by gas adsorption: the 3Flex 3500 gas adsorption analyser configured with a port for micropore analysis and the Tristar 3020 equipped with 3 stations for mesopore analysis. Together, they allow high throughput textural analysis of powders: specific surface area, pore distribution, total pore volume. In addition, a fully automated high throughput sample preparation system, Vac Prep 061, can process up to 6 samples in parallel under vacuum or gas flow.

REALCAT platform is equipped with three compact stand-alone fixed bed reactor Flowrence systems (Avantium) designed to screen heterogeneous catalyst for many and varied reactions. Each Flowrence unit has been tailored for the specific purpose of catalyst screening, for example :

• Flowrence 1219: Fischer-Tropsch reaction and VOC/toluene oxidation.
• Flowrence 1220: Ethanol, methanol, glycerol and methane reforming, deNOx.
• Flowrence 1221: Propylene, alcohol and glycerol oxidation and glycerol or hexose valorisation.

Flowrence contains 4 temperature blocks, each one can be operated at different temperature. Each block can receive 4 stainless steel or quartz reactors, so 16 isothermal fixed bed micro flow reactors can run in parallel and 16 experiments can be conducted simultaneously. Between 50-500 mg of catalyst can be loaded in one reactor. Flowrence can operate at wide conditions range: pressure between atmospheric and 90 bars, temperature between 50°C and 750°C, feed can be either gas, liquid or trickle flow.

All Flowrence systems are equipped with 16 ports multi positions to analyze the gas effluent by online gas chromatograph, Agilent 7890.

Flowrences 1219 and 1221 are also equipped with a liquid sampling robot allowing the collection of the effluents from each reactor separately. The sampling robot temperature is controlled between 10-80°C using an external cooling - heating device. This prevents the evaporation of light compounds or the solidification of heavy compounds, as wax, composites that can be present in the effluent.

The reaction effluents can also be analyzed by off-line mode: by GC-FID FID, GC-FID-MS and HPLC-DAD-MS and HPLC-UV-IR according to their nature.

This instrument is dedicated for quantification of volatile compounds.

This instrument includes :

• Two flame ionization detectors (FID).
• Two injectors split/splitless permitting to analysis simultaneously 2 samples.
• An autosampler AOC-20s with 150 positions.

The analysis methods have a short duration time, few minutes (6-10 min) permitting the analysis of 12 samples per hours using the two channels.

This instrument is dedicated for identification and quantification of volatile compounds.

This instrument includes :

• Two detectors: a flame ionization detectors (FID) and a mass spectrometer simple quadruple QP2010 ULTRA.
• An ionization mode: Electronic impact.
• Two injectors split/splitless permitting to analysis simultaneously 2 samples.
• An autosampler AOC-20s with 150 positions.

Identification is based on a comparison of spectrum with NIST 2011 MASS Spectral Library. The analysis methods have a short duration time, few minutes (6-10 min) enabling analysis of 12 samples per hours using the two channels.

High performance liquid chromatography of Shimadzu dedicated to quantification of compounds in liquid sample. This equipment includes two detectors: refractive index detector (RID-20A) and UV/visible detector with dual wavelength detection in the range 190-700nm (SPD-20A).

This instrument is dedicated for identification and quantification of compounds in liquid samples.

This instrument includes :

• Two detectors: diode array detector (DAD) (λ=190 à 800 nm) and a mass spectrometer simple quadruple (MS).
• Two ionization modes: ElectroSpray Ionisation (ESI) and Atmospheric Pressure Chemical Ionization (APCI).
• A binary pump.
• An autosampler with 96 or 384 positions.

The Screening Pressure Reactor (SPR) is an automated high pressure, high temperature reactor that accelerates catalyst discovery and reaction optimization.

This high throughput system is able to screen hundreds of reaction conditions, explore new synthetic routes, optimize reaction yield and identify alternate reaction conditions to reduce costs or identify a suitable solvent. The SPR has very wide applications like: hydrogenation/dehydrogenation, oxidation, acid/base reactions, biomass processing, petrochemicals, fine chemicals...

Main characteristics :

• High throughput runs: catalysts testing in parallel (up to 96 samples) and examine multiple variables simultaneously for rapid and high information content screening.
• Flexible reaction scales: 1 mL x 96 glass vials or 6 mL x 24 stainless steel vials.
• Wide process window: temperatures up to 400 °C and pressures up to 200 bar.
• Automated operation: temperature, pressure, and flow profiles controlled automatically based on a user defined recipe.
• Powerful mixing: High intensity vortexing (up to 800 rpm) provides for good solid/gas/liquid contacting during reaction and limits mass transfer issues.

Lissy-1G - Zinsser

Flowrence 1219 et 1221 unit can produce up to 256 samples per day dedicated for off-line analysis. The preparation of samples (dilution, level adjustment, internal standard addition.) produced by Flowrence prior to analysis by GC or HPLC is made automatically by a robotic system Lissy-1 G, Zinsser.

This instrument includes :

• A syringe for liquid handling system, dilution and addition of internal standard and sample transfer from Flowrences 8 ml vial to 2 ml GC vials.
• A crimping station.
• A vortexer.
• A cooling/heating system maintaining the sample at the required temperature.

Multi-R ® is a high-throughput equipment for gas-phase heterogeneous catalysts screening commercialized by the Teamcat Solutions company. Its patented innovative concept [1] protects the smart use of customized gas chromatography inlets as catalytic reactors. The whole system is composed of 3 main parts: the feed, the reactional unit and the analytical system. The reaction section represents the core level of the Multi-R where reactants are introduced in a heated topbox in order to maintain all chemicals under gas phase in the inlet stream. The flow is then the splitted into the 4 reactors, each reactor being thermally independent. This technical configuration enables a variety of experimental design in order to develop new catalytic processes and/or characterization of surface chemical properties carrying out model reactions. Quantification of products is realized with online analyzer, which configuration is adapted depending on the stream complexity after reaction.

[1] Patent WO 2015118263 ; CNRS, Lille Ecole Centrale, Univ Lille Sciences Tech; F. Dumeignil, S. Paul, L. Duhamel, J. Faye, P. Miquel, M. Capron, J.L. Dubois; Device for evaluation of at least one performance criterion of heterogeneous catalysts The Multi-R is able to:

• Accurately and quickly control the reactors temperature (up to 400 °C)

• Pressure control in the reactors (up to 7 bar)

• Program the ramp of the temperature of the reactors at up to 20 °C/min

• Fast data acquisition

This instrument can determine the absolute molar masses and sizes of the polymers or biopolymers without the need for reference standards or column calibration. That will ensure a control or verification of the synthetized polymer.

The analytical instrument is composed of a HPLC (Shimadzu) connected to 3 detectors :

• A multi- angle light scattering (MALS) detector miniDAWN TREOSTM (Wyatt).
• A differential Refractive Index (dRI) detectors serve as accurate and versatile concentration detectors: Optilab T-rEX (refractometer with EXtended range) (Wyatt).
• An UV detector (Shimadzu).

This equipment is available as part of the REALCAT platform but is located in another building.

The QPix robot offers the possibility to automatically select and sow bacterial colonies in 96 well plates. Allowing aerobic and anaerobic microorganism cultures as bacterial sources, this instrument gives the possibility to study a broad microorganism strain range. Due to its very high operation speed, as well as its precise multimode camera (visible, fluorometry...), the QPix enables the precise and fast selection of a large number of biocatalysts from a complex mixture based on size, shape, color, fluorescence and their proximity to neighbors. The biocatalysts can then be studied more precisely with the other platform robots.

This instrument includes :

• A 96 needles head for the high-speed selection and sowing of microbial colonies: from 3000 to 3500 colonies/hour.
• Different optimized-organism-specific pins for a wide range of microorganisms picking (E. Coli, B. subtilis, Streptomyces, Yeast, phages, etc.).
• An automatized medium detection system for picking calibration, offering high picking efficiency and precision during the whole operation.
• An automatized colonies selection system using white light (trans-illumination) with a CCD camera for automatic picking (can be upgraded into fluorescence mode).
• A smart-intelligent colony selection software (picks only single colonies selected on basis of size, shape, color, fluorescence and proximity to neighbors).

The Beckman Biomek FX high throughput robotic station is dedicated to the new biocatalyst production process in the molecular biology field. Totally automated, it allows the conception of large biocatalysts banks by directed evolution or random mutagenesis. These biocatalysts can then be sown using the colony picker and screened using the Biomek FX HTS station, in order to reveal better activities, or even new ones, toward a specific chemical reaction.

This instrument includes :

• A thermocycler T-Robot 96-wells plates PCR.
• An UV/Vis spectrophotometer for DNA and proteins quantification.
• A 96 needles head and a separated 8 needle head for fast pipetting operations.
• A negative pressure filtration system for DNA and protein purification in 96-wells plates using a wide range of purification columns.
• Two Peltier systems for sample thermal incubation (4-100°C).

The MALDI Tof/Tof performs a molecular analysis of the biocatalyst and compounds produced in the platform. This device has been selected for its broad range of applications, from proteomics to polymer analysis, glycomics or clinical and microbiological profiling.

This instrument includes :

• A Smartbeam-IITM Bruker laser, with 2 kHz MS acquisition speed MS, and a variable focusing system controlled between 10 and 100 µm.
• A PAN / Flash detector^TM system offering a wide mass range resolving power up to 26000.
• Linear or reflectron modes, positive or negative modes.
• A MALDI Perpetual^TM ion source with laser-based self-cleaning in less than 15 minutes.
• FlashDetector^TM combined with a new 4 GHz digitizer that provides 2 ppm mass accuracy for highest confidence.
• A LIFT^TM technology system for fast and sensitive MS/MS experiments.

The Realcat platform is equipped with a UPLC system coupled to an innovative hybrid quadrupole IMS (Ion Mobility) orthogonal acceleration time-of-flight (ToF) mass spectrometer. This instrument allows the composition analysis of a reactional medium before and after catalysis, in order to quantify the different transformations of reagents/products. It also allows the analysis of the fermentation medium produced in the Biolector or Bioreactors in order to follow the production or the consumption of metabolites by microorganisms. Thanks to the IMS technology, this instrument permits the separation and structural elucidation of stereoisomers.

This instrument includes :

• A binary solvent manager for a wide range of LC applications.
• An autosampler.
• A column heater and a PDA detector.
• An ESI/ETD-MS/MS SYNAPT G2-Si HDMS (High Definition Mass Spectrometer) equipped with an Ion Mobility Separation (IMS) for stereoisomers separation.

The Biolector is a high-throughput robot designed to study fermentations performed by prokaryotic or eukaryotic cells. Using a 48-wells microplate (FlowerPlate® & Round Well Plate) offering an average culture volume of 1 mL/well, this equipment allows the parallel and online monitoring of a large number of fermentation parameters affecting the cellular growth and metabolite expression. Among these, we can cite the online measurement of biomass concentration, pH, O₂ dissolved, NAD(P)H and other riboflavins concentration, the concentration of a wide range of fluorescent molecules (GFP, YFP, DsRed, etc.), and temperature (25-50°C). The Biolector also offers the possibility to control the O₂ and the CO₂ concentration in the head space atmosphere for aerobic and anaerobic fermentations.

This instrument includes :

• 48-wells plates equipped with pH et pO₂ monitoring system, dedicated to small volume fermentations (1 mL/well).
• An hermetic chamber for aerobic and anaerobic microbial fermentations.
• A light scattering system for online biomass monitoring.
• A fluorimeter equipped with several filters for the online monitoring of fluorescent molecules.

Realcat is equipped with an exclusive fermentation screening robotic platform. It includes a Biolector Pro from M2PLabs, allowing the online monitoring of 32 fermentation conditions in parallels, in Batch or Fed-Batch systems. Like the Biolector, the Biolector Pro offers an average fermentation volume of 1 mL/well and the monitoring of all the classical physico-chemical parameters of the microbial cultures (pH, T°C, pO₂, biomass, etc.). However, unlike the Biolector, the Biolector pro allows a fine control of the pH through on-time base or acid solutions addition using a patented microfluidic system implemented inside the wells. This system can also serve a Fed-Batch system for continuous substrate addition to the reaction medium. Finally, this Biolector Pro is installed inside a fully automatized pipetting platform Biomek NX^p from Beckman Coulter, for on-time sample taking and addition for later offline analysis.

This instrument includes :

• A Biolector Pro using microfluidic 32-wells plates for Fed-Batch fermentations.
• An hermetic chamber for aerobic and micro-aerobic microbial cultures.
• A Biomek NX^P pipetting station for sample taking, addition, and preparation.

Six parallel stirred tank bioreactors of 500 ml each are available on the platform to study various microbial fermentation parameters. These reactors are designed to complete the setting of the parameters started at smaller scale (biolector), in order to prepare the scale-up of the project (pre-pilot).

This instrument includes :

• An online DO, pH an pO₂ measurement system.
• A temperature (25-50 °C) and stirring control system.
• An online gas monitoring system (Tandem).
• A nitrogen gas input system for anaerobic fermentations.

The Beckman Biomek FX high throughput station is dedicated to the screening of large biocatalyst banks (enzyme or microorganisms), in order to evaluate their performances and select the best ones. To achieve this goal, the robot allows the complete characterization of the biocatalyst, as well as the fine study of its catalytic capabilities. These tests can be efficiently performed thank to the coupled UV, visible and fluorescent spectrometers. The presence of these three detection modes offers the opportunity to study a wide range of compounds in many chemical reactions. Finally, this station allows to screen around 2000 enzymes per day stored in 96- or 384-wells plates.

This instrument includes :

• A UV/Vis, fluo and lumino spectrophotometer enzyme activity measurement.
• A 96 needles head and a separated 8 needle head for fast pipetting operations.
• A positive pressure filtration system for protein purification in 96-wells plates using a wide range of purification columns (C18, IMAC, etc.).
• A magnetic system for sample purification using dedicated magnetic beads.
• Two shaking Peltier systems for pour for reaction mixing and thermal incubation (4-100°C).
• An automatized MALDI plate preparation system for very fast mass spectrometry analysis of 384 samples per batch.

The Cary 3500 is a UV-Vis spectrophotometer dedicated to the measurement of high temperature liquid phase reactions. Equipped with a multizone multicell chamber that allows up to four temperature experiments, across eight cuvette positions, simultaneously, it helps determining the optimal operating temperature of catalyst such as thermostable enzymes. Its agitation system also allows for the use of heterogeneous catalysts such as supported enzymes or chemical heterogeneous catalysts, and is therefore very suitable for the analysis of reactions that are part of the new concept of hybrid catalysis.

The Cary 3500 is able to :

• Accurately and quickly control the samples temperature from 0 to 110 °C, with 4 different temperatures over 8 cuves.
• Ramp the temperature of the sample at up to 30 °C/min
• Measure absorbance over a 190–1100 nm wavelength range
• Collect up to 250 points per second and cover 150,000 nm/min of wavelength variation