Automated Synthesis (AS)
(The technology is expected to be available by the end of 2024.)
The Automated Synthesis technology is currently under construction. This technology enables the use of various modules to support chemical synthesis, the purification of organic materials in particular, and their analysis. The modules of AS can be utilized for fully automated synthesis of chemical building blocks after the completion of the ChemASAP platform (platform for automated synthesis and analysis). Scientists with in-depth knowledge of chemistry and synthesis can use the platform by incorporating their own protocols, while scientists without expertise can apply for access to the platform and corresponding capacities to plan experiments. Until all modules are fully integrated, the use of different sub-areas (single modules) will be offered by KNMFi.
Module Type 1: Modules for synthesis and synthesis preparation and post-processing
(1-1) Reactor for photochemical reactions (Day-light LEDs):
- 48 reaction positions can be used in parallel for the illumination with white daylight LEDs
- Stirring and air cooling integrated
(1-2) Gas injection modules
- Gas injection with reproducible methods by automation
- 1-9 injections in parallel, without time limitation (to saturation)
- Different gases, current standard: CO2 injection
(1-3) Echo-acoustic dispensing
- Non-contact transfer of fluids down to 2.5 nL
- Mild enough to transfer cells, samples and reagents
- Direct dilution for reliable dose-response and standard curves
- Rapid transfer from any source well to any destination well: Cherry Picking, Sample Pooling, Combination Screening
- Possible Fields of Application: Synthetic Biology, Genomics, Drug Discovery, Combinatorial Chemistry
(1-4) Genevac evaporation system:
- Vacuum centrifugation for solvent removal
- Centrifugation without vacuum also possible
- Compatible with different vessels:
– All well plate formats
– Eppendorf tubes
– 1.8 ml GC/MS Vials
– Falcon tubes
Module Type 2: Modules suitable for the purification of organic substances
(2-1) Liquid chromatography - mass spectrometry (LC-MS)
Shimadzu analytical LC/MS and LC-SFC/MS
- Equipped with a CTC PAL autosampler
- Equipped with PDA (UV/VIS), ELSD and mass spectrometer detectors
- Will be integrated into the xPlanar robotic platform for automatic sample loading
- LC/MS is equipped with a C-18 column and runs on acetonitrile/water
- LC-SFC/MS is equipped with a diol column and runs on supercritical CO2 with methanol as modifier
- Setup identical to preparative systems for easy method transfer from analytical to preparative system
(2-2) Sublimation apparatus
- Sublimation efficiency up to 97%
- Typical charge capacity: 0.25 g ... 5 g
- Defined temperature gradient; Evaporation zone: 100 °C - 800 °C
- Three independent temperature zones
- Base pressure < 10-6 mbar
- All separation parameters (vacuum, temperatures) are recorded for evaluation
- Software allows parameters and gradients to be defined in method files
Module Type 3: Modules for the analysis of (in)organic compounds
(3-1) Gas chromatography (GC-BID)
- Equipped with a CTC PAL autosampler
- Equipped with dual barrier ionization discharge (BID) detectors
- Separation of gases and volatile organic compounds (VOC) such as: H2, O2/Ar, N2, CO2, CO, CH4, methanol, ethanol, isopropanol, formaldehyde, formic acid, benzene, etc. (except He because carrier and plasma gas is He)
(3-2) Gas chromatography - mass spectrometry (FID-MS)
- Equipped with a CTC PAL autosampler
- Equipped with flame ionization detector (FID) and mass spectrometer detectors
- Already integrated into the xPlanar robotic platform for automatic delivery to autosampler
- Dual injectors for choice of separation on two different columns
- Both detectors record FID and MS data simultaneously, independent of the injector/column used
(3-3) Supercritical Fluid Chromatography (SFC)
Shimadzu preparative LC/MS and LC-SFC/MS
- Equipped with autosampler and fraction collector
- Injection volume of max. 20 mL per run
- Equipped with PDA (UV/VIS), ELSD and Mass Spectrometer detectors
- Will be integrated into the xPlanar robotic platform for automatic delivery to autosampler and automatic removal of fractions from fraction collector
- LC/MS is equipped with a C-18 column and runs on acetonitrile/water
- LC-SFC/MS is equipped with a diol column and runs on supercritical CO2 with Methanol as modifier
(3-4) Fluorescence spectrometer FLS1000
- Steady state and time-resolved photoluminescence spectroscopy
- Modular, functionality partly available with upgrades
- Fluorescence and phosphorescence spectrometer, measuring spectra from the ultraviolet to the mid-infrared spectral range (up to 5,500 nm)
- Lifetimes spanning from picoseconds to seconds
(3-5) Flexible, mobile mass spectrometer for gas analysis
- Gas phase mass spectrometric analysis
- From headspace vials or in-line process
- m/z range from 2 to 300 amu
(3-6) NMR Spectrometer
- AVANCE NEO 400 MHz console
- Magnetic system: ASCEND 400 MHz SB
- Broadband-optimized 5 mm double-resonance observe SmartProbe head with 1H decoupling and 1H observation.
- From 19F and 31P to 109Ag, exception: 171Yb bis 9Be.