Polymer- und Membransynthese

Geräte zur Polymer- und Membransynthese, Aufarbeitung und Charakterisierung am HI ERN verfügbar

Im Folgenden sind Geräte zur Polymer- und Membransynthese, Geräte zur Polymeraufarbeitung und Geräte zur Polymer- und Membrancharakterisierung aufgeführt. In den Tabellen sind nur fest installierte Geräte zur Synthese, Aufarbeitung und Charakterisierung der Monomere, Polymere und Membranen dargestellt.

1. Geräte für organische (Polymer-)Synthesen (nur ortsfeste Installationen)

    

Gerät

Hersteller

Eigenschaften

Synthese Möglichkeiten

Automatisiertes Labor-Synthesegerät / Mehrzweck-Batch-Reaktor

  • Glasteile: Infraserv Höchst
  • Steuereinheit: HiTec Zang GmbH
  • Reaktorvolumen: 1000 mL (bis zu 4000 mL möglich)
  • Temperaturbereich -40 bis+200°C
  • Schutzgasatmosphäre
  • Automatische Dosierung
  • Fernsteuerbar
  • Modular anpassbar

Breites Spektrum an organischen Synthesen wie:

  • Monomersynthesen
  • Polymerisationen (radikal, anionisch, kationisch, Polykondensationen, Polyadditionen)
  • Polymermodifikationsreaktionen wie: Sulfonierungen, Phosphonierungen, C-C-Kupplungsreaktionen, Friedel-Crafts-Acylierungen (und viele mehr)

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. Geräte zur organischen (Polymer-)Aufarbeitung (nur ortsfeste Installationen)

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. Geräte zur Polymer- und Membrancharakterisierung

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

Letzte Änderung: 24.08.2022