Equipment

The Mastalerz group is equipped with state-of-the-art devices for sample purification and property elucidation. All machines were configured to fit to the research interest of the group and in particular macromolecules such as covalent organic cage compounds and larger polycyclic (hetero)-aromatic hydrocarbons. Furthermore, we have access to several central facilities of Heidelberg University such as the NMR-facility, masspectrometric facility, the microanalysis laboratory, the single crystal X-ray analysis facility as well as joined institutions such as the Centre for Advanced Materials (CAM). In addition several collaborators provide access to techniques such as SEM, battery investigations, 3D-printing and many more.


 

 

Gas Sorption


Gas Sorption Analyzer "Autosorb IQ2"

Equiment Iq 2 B

The Quantachrome Autosorb IQ2 gas sorption analyzer is capable of measuring single gas isotherms at various temperatures on two independent sample stations simultaneously.

Standard low-pressure nitrogen sorption at 77 K can be used to investigate porous materials with respect to their specific surface areas, pore volumes or pore size distributions. Furthermore, the sorption behaviour of gases such as H2, CO2, CH4, etc. gives insights into potential applications of the investigated materials for gas separation and/or storage.

The machine is equipped with two outgas stations for outgas temperatures up to 350 °C.

1000, 10 and 1 torr pressure sensors are used, the latter for accurate measurements in the micropore regime.

A built-in vapour option gives access to vapour sorption experiments of liquids with an adequate vapour pressure at up to 50 °C.

Cooling is fullfilled with external cooling baths such as liquid nitrogen (77 K) or common cooling mixtures.

 

Gas Sorption Analyzer "Autosorb IQ3 " (located at the Centre for Advanced Materials)

Iq3

The Quantachrome Autosorb IQ 3 gas sorption analyzer is capable of measuring single gas isotherms at various temperatures on three independent sample stations simultaneously.

The setup is equipped with a liquid helium cryocooler, which is continuously adjustable in a temperature range from <20 to 320 K allowing to investigate porous materials with argon at 87 K fulfilling the most recent IUPAC recommendations. Thin film materials can be investigated by krypton sorption at 77 or 87 K to obtain information about their surface properties, which is of particular interest in organic electronics and sensor applications.

1000, 10 and especially 0.1 torr pressure sensors represent state of the art sensors regarding the accuracy in the micropore regime.

A built-in chemisoption option gives access to adsorption experiments with high binding affinities which are of importance in e.g. heterogenous catalysis

 

 

 

 

Chromatography


HPLC (analytical) "Nexera LC-40"

Analytische Hplc

The Shimadzu Nexera LC-40 analytical HPLC uses a LC-40D solvent delivery pump (up to 10 mL/min) with a 4-channel LPGE unit and an in-line 5-channel degassing unit and is automated by a SIL-40 autosampler.

A CTO-40C column oven assures the thermal stability of up to 6 analytical HPLC columns in a temperature range of -10 to 100 °C.

Sample elution can be detected with a SPD-M40 photo diode array detector with simultaneous detection in the range of 190-800 nm with a maximum sampling rate 100 Hz.

The system is permanently equipped with a Daicel chiral technologies primary screening column set (IA / IB-N / IC / IG / IE) and can be used with further analytical HPLC columns (SiO2, C-18, C-8, etc.) in both normal as well as reversed phase.

 

 

HPLC (semi-prep. NP-recycling) "Prominence LC-20"

Rp Rec Hplc

The Shimadzu Prominence LC-20 NP-rec.-HPLC is equipped with a preparative LC-20AP pump for flows up to 150 mL/min. A manual Rheodyne sample injection valve allows injections of up to 5 mL for semi-preparative sample separation.

A preparative SiO2 (250 x 21.2 mm) enables the use of common normal phase eluents such as chlorinated solvents, alkanes etc. and mixtures of the beforementioned.

The SPD-M20A photo diode array detector detects full UV/vis spectra in the range of 190-800 nm with a maximum frequency of 100 Hz in-line.

The system is furthermore equipped with a 6-position selection valve which allows repetitive sample elution over the column in a so-called recycling mode imitating an in theory infinite column length for better separation.

The fractions are collected manually.

 

HPLC (semi-prep. RP-recycling) "Prominence LC-20"

Rp Hlpc

Similar to the RP-rec.-HPLC system, the Shimadzu Prominence LC-20 RP-rec.-HPLC is equipped with a preparative LC-20AP pump for flows up to 150 mL/min. A manual Rheodyne sample injection valve allows injections up to 5 mL for semi-preparative sample separation.

Preparative C-18, C-8 and nitrophenyl end-capped RP-columns (250 x 21.2 mm) require the use of common reversed phase eluents such as acetonitrile, water, iso-propanol etc. and mixtures of the beforementioned.

The SPD-M20A photo diode array detector detects full UV/vis spectra in the range of 190-800 nm with a maximum frequency of 100 Hz in-line.

The system is furthermore equipped with a 6-position selection valve which allows repetitive sample elution over the column in a so-called recycling mode imitating an in theory infinite column length for better separation.

The fractions are collected manually.

HPLC (semi-prep. RP/NP) "1200 Series"

Agilent 1

The Agilent 1200 semi-prep. HPLC is equipped with two independent preparative pumps allowing binary gradients of eluents with up to 100 mL/min flow.

Samples are injected using an autosampler with max. volumes of 900 µL. Eluted samples are detected by a 4-channel UV/vis detector (range: 190-750 nm) and the samples are automatically collected.

The setup can be used with both, normal phase and reversed phase eluents depending on the separation necessities.

GPC (recycling, CH2Cl2) "Nexera LC-40"

Ch2cl2 Gpc

The Shimadzu Nexera rec.-GPC is equipped with a preparative LC-40D pump for flows up to 10 mL/min. Sample volumes of up to 500 µL are injected by a SIL-40C autosampler. Eluents are degassed by a DGU-403 degassing unit.

Three semi-prep. PSS SDV columns (300 x 21.2 mm) with 100 Å porosity in CH2Cl2 are used for separations of molecules between 100-10000 Da. The separation temperature is held stable between -10° and 100 °C by a CTO-40C column oven.

The SPD-M40A photo diode array detects full UV/vis spectra in the range of 190-800 nm with a maximum sampling frequency of 100 Hz in-line. Photo-labile samples can be detected by a RID-20A refractive index detector.

The system is furthermore equipped with a 6-position selection valve which allows repetitive sample elution over the column in a so-called recycling mode imitating an in theory infinite column length for better separation.

Fractions are collected by an FRC-10A fraction collector.

GPC (recycling, CHCl3) "Prominence LC-20"

Thf Gpc

The Shimadzu Prominence rec.-GPC is equipped with a preparative LC-20D pump for flows up to 10 mL/min. Samples volumes of up to 500 µL are injected by a SIL-20AHT autosampler. Eluents are degassed by a DGU-20A3R degassing unit.

Three semi-prep. PSS SDV columns (300 x 21.2 mm) with 100 Å porosity in CHCl3 are used for separations of molecules between 100-10000 Da. The separation temperature is held stable up to 85 °C by a CTO-20A column oven.

The SPD-M20A photo diode array detector detects full UV/vis spectra in the range of 190-800 nm with a maximum frequency of 100 Hz in-line.

The system is furthermore equipped with a 6-position selection valve which allows repetitive sample elution over the column in a so-called recycling mode imitating an in theory infinite column length for better separation.

Fractions are collected by an FRC-10A fraction collector.

GPC (recycling, THF) "Prominence LC-20"

Chcl3 Gpc

The Shimadzu Prominence rec.-GPC is equipped with a preparative LC-20AD pump for flows up to 10 mL/min. Samples volumes of up to 500 µL are injected manually by a Rheodyne valve. Eluents are degassed by a DGU-20A3R degassing unit.

Three semi-prep. PSS SDV columns (300 x 21.2 mm) with 100 Å porosity in THF are used for separations of molecules between 100-10000 Da. The separation temperature is held stable up to 85 °C by a CTO-20AC column oven.

The SPD-M20A photo diode array detector detects full UV/vis spectra in the range of 190-800 nm with a maximum frequency of 100 Hz in-line.

The system is furthermore equipped with a 6-position selection valve which allows repetitive sample elution over the column in a so-called recycling mode imitating an in theory infinite column length for better separation.

Fractions are collected by an FRC-10A fraction collector.

GC-mass spectrometer "7890A/5975C"

Gc Ms

The coupled gas chromatography-mass spectrometry systems 7890A/5975C from Agilent technologies includes a 7890A gas chromatograph with a 50 m long column (diameter 0.32 mm) and a heating range of 40 to 450 °C. Injection is performed by a 7683B injector with up to 8 slots.

The 5975C mass selective detector (MSD) uses a triple-axis-detector in EI mode for samples up to 1050 Da.

 

Spectroscopy


UV/vis spectrometer "V-730"

Uv Vis

The Jasco V-730-ST UV/vis spectrometer enables absorption measurements in a spectral range of 190-1100 nm in both, solution and thin films.

Fluorescence spectrometer "FP-8300"

Fluoro

The Jasco FP-8300 fluorescence spectrometer is able to acquire excitation as well as emission spectra in a spectral range of 200-750 nm. The samples can be measure in solution, thin film or by special attachments as solids as well as at low temperature.

 

Spectral polarimeter "J-1500"

Cd

The Jasco J-1500 spectral polarimeter is capable measuring circular dichroism (CD), linear dichroism and UV/vis absorption simultaneously in a range of 163-950 nm. An EXIG-531 wavelength extension kit gives access to a wavelength range of 800-1600 nm by an InGaAs detector.

A PTC-510 Peltier cooling attachment allows sample tempering between -40 °C and 130 °C. The operating conditions are held stable during operation by a Julabo F250 circulation cooler and FLMS-526 N2 gas flow meter.

 

FT-IR-spectrometer "Tensor 27"

Ir

The Bruker Fourier transform infrared spectrometer Tensor 27 enables the investigation of molecular vibrations in a typical range between 500 and 4000 cm-1. Standard transmission as well as attenuated total reflection (ATR, ZnSe) detection is possible by corresponding sample stages.

 

Electrochemical Analyses


Electrochemical analysis station "PGSTAT101"

Cv

The Metrohm Autolab PGSTAT101 potentiostat is used for electrochemical investigations such as cyclic or square wave voltammetry (CV and SWV) and many more, by the attachment of a electrochemical sample cell for volumes of ~5 mL. The sample cell can be constantly flushed with inert gases and Pt or CC working electrodes are used in standard set-ups with an Ag reference- and a Pt-sheet counter electrode.

 

Quartz Crystal Microbalance (QCM)


Quartz crystal microbalance and dissipation (QCM-D) "Explorer"

Qcm

The Q-sense explorer quartz crystal microbalance and dissipation (QCM-D) can detect as little as 1.8 ng/cm2 sample in liquids and gas flows with working temperatures between 15-65 °C with its QE 401 electronic device. Samples are by default investigated on gold coated quartz crystals in either a QCP 101 standard sample chamber, a QFM 401 flow chamber, a QEM 401 electrochemical chamber or a QWM 401 sample chamber with optical window. 

An Ismatex Reglo Digital peristaltic pump is used for liquid handling and the sample plates can be pre-treated in an ESA 006 ozone chamber.

 

 

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Letzte Änderung: 20.07.2021
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