Polymer and membrane synthesis

Polymer and membrane synthesis, workup and characterization devices available at HI ERN

In the following, devices for polymer and membrane synthesis, devices for polymer workup and devices for polymer and membrane characterization are listed. Only permanently installed devices for the synthesis, processing and characterization of the monomers, polymer and membranes are shown in the tables.

1. Devices for organic (polymer) syntheses (fixed installations only)

    

Name of device

Producer

Characteristics

Synthesis possibilities

Automatized lab synthesis device / multi-purpose batch reactor

  • Glassware: Infraserv Höchst
  • Control unit: HiTec Zang GmbH
  • Glass reactor volume: 1000 mL (up to 4000 mL possible)
  • Temperature range -40 to +200°C
  • Protective gas-Automatic dosing
  • Remote controllable
  • Modularly customizable

Broad range of organic syntheses such as:

  • Monomer syntheses
  • Polymerizations (radical, anionic, cationic, polycondensations, polyadditions)
  • Polymer modification reactions such as:
    Sulfonations, phosphonations, C-C coupling reactions, , Friedel-Crafts acylations (and many more)

Glovebox

GS Glovebox Systemtechnik

  • Work under protective gas
  • 2 Glove pairs for parallel work
  • Refrigerator
  • ColdWell
  • Balance for weighing of e. g. catalysts
  • Chemical work under inert atmosphere for highly toxic substances and/or air
  • sensitive substances

Microwave reactor small (Model: Discover)

CEM

  • 12 Pressure vessels à 100 mL on turntable
  • Temperature range RT to +300°C
  • Pressure up to 50 bar
  • T and t-programmable
  • Individual glassware assembly possible in MW resonator

Broad range of organic syntheses such as:

  • Monomer syntheses
  • Polymerizations (radical, polycondensations, polyadditions, Suzuki polycondensations)
  • Polymer modification reactions such as:
    C-C coupling reactions, (and many more)

Microwave reactor big (Model: MARS)

CEM

  • 12 Pressure vessels à 100 mL on turntable
  • Temperature range RT to +300°C
  • Pressure up to 50 bar
  • T and t-programmable
  • Individual glassware assembly possible in MW resonator

Broad range of organic syntheses such as:

  • Monomer syntheses
  • Polymerizations (radical, polycondensations, polyadditions, Suzuki polycondensations)
  • Polymer modification reactions such as:
    C-C coupling reactions, (and many more)

2. Devices for organic (polymer) workup (fixed installations only)

Name of Device

Producer

Purpose

Characteristics

Rotation evaporator System R-300

Büchi Labortechnik GmbH

Distilling off solvents from reaction mixtures

  • Glass flask volume up to 4000 mL
  • Vacuum down to 10 mbar (via membrane pump)
  • Heatable bath (up to 80°C when water is bath liquid)

Flash chromatography device C-815

Büchi

Separation of reaction product mixtures (liquid chromatography)

  • Separation of reaction mixtures up to 100 g
  • Pressure range 0-50 bar
  • 1/4 L/min solvent pumping rate

Ultrafiltration device MaxiMem

PS Prozesstechnik GmbH

Separation/concentration of polymer solutions via ultrafiltration or nanofiltration

  • Pressure range up to 60 bar
  • Temperature depending on thermostat
  • Flat membrane module with 215 cm2 area
  • Spiral-wound module with 0.3 m2 area
  • Tubular membrane module with length 600 or 1200 mm and outer diameter 10 mm

3. Devices for polymer and membrane characterization

Name of device

Producer

Purpose

Characteristics

JNM-ECZ500R 500 MHz FT NMR System

JEOL (Germany) GmbH

  • Determination of absolute chemical composition and structure of chemical compounds (low- and high-molecular compounds
  • Investigation of the kinetics of chemical reactions-Investigation of the dynamics of molecules
  • Investigation of interactions between molecules
  • Frequency 500 MHz
  • Measurable nuclei: 1H, 13C, 19F, 31P, 6Li, 7Li, 196Pt, 15N, 17O (also as DEPT)
  • Coupling experiments: 1H/13C, 1H/19F, 13C/19F: HSQC, HMBC

    1H/1H: COSY, NOESY, TOCSY
  • 100 x Autosampler
  • Temp. range from -90 to +120°C

Spectrum 3 FTIR with ATR device

PerkinElmer

  • Determination of absolute
  • Determination of relative chemical composition and structure of chemical compounds
  • ATR module (attenuated total reflection) for investigation of films (e. g. membranes), liquid samples and powders
  • Wave number range: 8300 – 350 cm-1
  • Spectral resolution: 0.4 to 64 cm-1
  • Signal/noise ratio: >50,000 peak-peak

UV-vis Spectral Photometer UV-1900i

Shimadzu

  • Determination of concentrations and concentration changes of solutions containing UV-active chemical compounds (after calibration)
  • Determination of diffusion coefficients of UV-active species by time-dependent changes of concentration e. g. in a diffusion cell
  • Touchscreen operation
  • 2-beam operation
  • Resolution 1 nm
  • -Spectral range 200 – 1,100 nm
  • Scan speed up to 29,000 nm/min
  • Stray light of max. 0.5% (198 nm)
  • Measurements of changes over time at a specified wavelength

Electrochemical workstation Zennium X

Zahner-elektrik

  • Recording of impedance spectra
  • Cyclovoltammetry
  • Frequency range 10 µHz – 12 MHz
  • Max. current +/- 4 A
  • Controlled voltage +/- 15 V +/- 5 V
  • Compliance voltage: +/- 32 V

Autotitrator OMNIS device

Metrohm

  • Automatized titrations such as:
    - acid-base titration
    - redox titration
    - other potentiometric titrations such as chloride titration with AgNO3 (precipitation titration)
  • Automatized and computer-controlled titration
  • Storage of titration methods in the software
  • 4 titration units can be operated in parallel

DSC device STARe DSC3+

Mettler-Toledo

  • Determination of endothermal or exothermal thermodynamic changes in solid or liquid samples upon heating such as:
    - glass transition
    - crystallization
    - melting/freezing
    - boiling/condensing
    - chemical reactions/chemical degradation-General thermal degradation
  • T range from -150 to +700 °C (with liq. N2 cooling option)
  • Heating rate 0.02 to 300 K/min
  • Cooling rate 0.02 to 50 K
  • Signal time constant 1.8 sec
  • TAWN sensitivity 11.9
  • 56 thermoelements
  • STARe software for controlling and data evaluation

DMA device DMA1

Mettler-Toledo

  • Determination of thermomechanical properties of samples in dependence of T such as:
    - extensional storage modulus
    - extensional loss modulus_
    - extensional loss factor
    - specific temperatures such as glass transition temperature
    - curing behavior of resins
    - Creep and relaxation processes under either constant force or constant deformation
    - thermal expansion coefficient
  • Power area 0.0001 N – 10 N-T range
  • 190 to +600 °C-Tan Delta range 0.0001 to 50
  • Path area +/- 1 mm
  • Stiffness range 50 N/m to 105 N/m

TGA-FTIR-GC-MS coupling device TGA 8000 – FT-MIR SPECTRUM 3 – Clarus 690 GC – Clarus SQ 8 T MS

PerkinElmer

  • Determination of thermomechanical properties of samples in dependence of T such as:
    - extensional storage modulus
    - extensional loss modulus_
    - extensional loss factor
    - specific temperatures such as glass transition temperature
    - curing behavior of resins
    - Creep and relaxation processes under either constant force or constant deformation
    - thermal expansion coefficient
  • TGA:
    - T range -20 to 1200 °C

    - heating rate 0.01 to 500 K/min
    - weight up to 1,300 mg
    - sensitivity 0.1 µg
    - vacuum option up to 1.3*10-8 bar
    - freely programmable heating/cooling/isothermal programs
    - gas control: mass flow controller
    - currently available gas atmo-spheres: N2, air; gas mixing for up to 3 gases possible
  • FT-MIR:
    - wave number range 8300 – 350 cm-1
    - Spectral resolution 0.4 to 64 cm-1
    - signal/noise ratio >50,000:1
    - Wavelength accuracy: 0.008 at 1600 cm-1

    - Scan: 1 minute, 4cm-1 resolution
  • GC:
    - 2-channel GC with autosampler with 108 sample positions, four washing liquids,variable injection speed, injection volume 0.1μl-50μl
  • MS:
    - SMARTsource ion source
    - Ionization voltage 10-100 eV variable
    - durable "marathon" filament
    - Electron impact ionization
    - Quadrupole system with pre-filter
    - Mass range 1-1200 Da
    - variable scan rate up to 12,500 Da/s
    - Data acquisition rate up to 100 points/s
    - Mass stability +/- 0.1 m/z over 48 hours
    - Full Scan, SIM and SIFI technology
    - Turbo molecular pump 255 l/s
    - WRG large-range gauge with software-based vacuum display
    - Clarifi detector - more durable, more sensitive electron multiplier

GPC/SEC system 1 with components from different OEMs for DMAc-soluble polymers

PSS Polymer Standards Service

  • Determination of molecular weights and molecular weight distributions of oligomers and polymers
  • Automatic sampler with up to 100 places
  • Refractive index detector with T range from 5°C above RT to 55°C
  • UV detector with wavelength range 190 – 600 nm
  • Combinable with light scattering detector of GPC system 2
  • Heated column oven from 4 to 80°C

GPC/SEC system 2 with components from different OEMs for THF-soluble polymers

PSS Polymer Standards Service

  • Determination of molecular weights and molecular weight distributions of oligomers and polymers
  • Automatic sampler with up to 100 places
  • Refractive index detector with T range from 5°C above RT to 55°C-UV detector with wavelength range 190 – 600 nm
  • Light scattering detector with 7 angles between 35° and 145°, light source: 35 mW laser diode, 635 nm, including software package for data evaluation
  • Heated column oven from 4 to 80°C

Last Modified: 14.07.2022