Equipment

Microreactor systems

Description                                              

Different microreactors are available at our research group. We use both complete systems and self-made systems by combining one or more pumps with a tubular reactor and/or a microchip. Within our lab, flow reactions with O2, CO2, H2, and CHF3 are possible. In-line work can be done by a Zaiput liquid/liquid separator and in-line analysis by an in-line FTIR (Bruker).

Complete systems

Labtrix® Start (Chemtrix)
Internal volume: 1, 5 or 10 µl depending on the reactor chip used
Temperature range: -15°C to 195°C
Pressures up to 25 bar
Wetted materials: glass, PEEK, PTFE, Techtron

KiloFlow® (Chemtrix)
Internal volume: 13 ml
Temperature range: 10°C to 150°C
Pressures up to 20 bar
Wetted materials: glass, PEEK, ETFE, perfluoroelastomer

X-CubeTM (ThalesNano)
Temperature range: 20°C to 200°C
Pressures up to 150 bar
Wetted material: stainless steel
Compatible with gases (H2, O2, ...)
Compatible with catalyst cartridges (Pd/C, Raney Ni, ...)

H Cube Mini (ThalesNano)
Temperature range: 20°C to 100°C
Pressure 1 bar to 100 bar
Flow rate 0.3-3 ml/min
Maximum hydrogen production rate 25-30 Nml/min
Water reservoir capacity 100 ml

Vapourtec Easy-MedChem V3
An adjustable packed bed column reactor – ambient to 150°C
A tube reactor assembly – ambient to 150°C
User interface with manual control software
3 V-3 pumps

Africa (Syrris)
Fully automated, flexible and easy-to-use microreactor system
Wide temperature range
Reagent pump module with flow rate range of 2.5-2500 µl/min

Pumps

ReaXus-Model 6010R (Teledyne ISCO)
High performance reciprocating peristaltic pump
Accurate flow rate control up to 10 ml/min
Pressure capability up to 6000 psi (414 bar)

WADose (Flusys)
Compact high-pressure dosing peristaltic pump (dual piston)
Dosing range 0.001-40 ml/min
Viscosity range up to 40 mPa.s
Pressure range atm-400 barg
Pump head material PEEK

FlowSyn Binary Pump Module (Uniqsis)
Peristaltic pump
Flow rates from 5 µl/min up to 10 ml/min
Glass static mixer + Teflon 5 ml coil reactor
10 bar BPR

Intelligent Pump AI-12 (Flom)
Peristaltic pump
Double-plunger reciprocating method
Maximum discharge pressure 5MPa
Range of flow rate setting 0.1-50 ml/min
Pressure limiter upper limit 0-10 MPa

Syringe pumps e.g. Fusion 101 (Chemyx)

Reactors

  • Glass chips: e.g. Glass static reactor 1.6 mL (Uniqsis)
  • PTFE tubing with multiple radii
  • PFA tubing with multiple radii
  • PEEK tubing with multiple radii

Bruker Avance-III 400 MHz NMR Spectrometer equipped with BRUKER 5 mm BBFO 400 MHz Z-gradient high resolution probenmr 2

Description

State-of-the-art NMR spectrometer equipped with an observe broadband high resolution probe, fitted with an actively shielded single axis Z-gradient for 5 mm sample diameters and 400 MHz standard-bore or wide-bore magnets. The inner NMR coil can be tuned to observe 19F or any nucleus in the range from 31P to 15N. The outer NMR coil is tuned for either 1H decoupling or observation. The probe is fitted with a 2H lock channel and automatic tuning and matching (ATM).

Signal/Noise

19F sensitivity  ≥250:1  (TFT sample, with 1H decoupling)

31P sensitivity  ≥140:1  (TPP sample)

13C sensitivity  ≥160:1  (ASTM sample)

15N sensitivity  ≥20:1  (90% formamide sample)

1H sensitivity  ≥250:1  (0.1% EB sample, 2ppm noise)

Pulse Widths

19F pulse width  ≤15μs  (TFT sample)

31P pulse width  ≤15μs  (TPP sample)

13C pulse width  ≤10μs  (ASTM sample)

15N pulse width  ≤18μs  (90% formamide sample)

1H pulse width  ≤15μs  (0.1% EB sample)

Lineshape

13C spinning lineshape  ≤0.2/2/4 Hz  (50%/0.55%/0.11%, ASTM)

1H spinning lineshape  ≤0.6/6/12 Hz  (50%/0.55%/0.11%, 1% CHCl3)

Z-gradient

The probe is fitted with an actively shielded single axis Z-gradient.

Maximum gradient strength is 50 gauss/cm

Variable Temperature Range

Variable temperature range is from -150°C to +150°C*

Liquid chromatography - Mass spectrometry

lcms

Agilent 1100 LC/MSD SL - Agilent 1200 LC - 1100 Series MSD VL

HPLC : UV detection by DAD

MS : ESI -quadrole (single-quad) - electron multiplier

Agilent 1100 Prep LC

HPLC : VWD detection - fraction collector

Perkin Elmer FT-IR system

Description

PerkinElmer FT-IR system, spectrum BX with ATR (attenuated Total Reflectance) accessory (ZnSe crystal)

  • solid and liquid sampling
  • no sample preparation
  • improved sample to sample reproducibility
  • minimized user to user spectral variation

GC-MS Agilent 8890

gcms

Description

The Agilent 8890 Plus GC system is coupled to a quadropole mass selective spectrometer 5977B MSD

Gerstel MPS2 autosampler has various introduction techniques: liquid, dynamic headspace, SPME and thermal absorption

GC-MS Agilent 6890 Plus

gcms2

Description

The Agilent 6890 Plus GC system is coupled to a quadropole mass selective spectrometer 5793 MSD

Gerstel CIS-4 PTV injector

Organic Elemental Analysis 2400 Series II CHNS/O Elemental Analyser

Description

One analyser with three modes of operation : CHN, CHNS and Oxygen

Advanced cumbustion design for handling virtually any type of samples

Frontal chromatography for simple , reliable and accurate measurements

Automated weight entry

Analytical detector range (element range (mgs)):

  • C: 0.001 - 3.6
  • H: 0.001 - 1.0
  • N: 0.001 - 6.0
  • S: 0.001 - 2.0
  • O: 0.001 - 2.0