Research
Equipment

Equipment: Facilities and Equipment for our Research

The equipment of the institute is under the supervision of members of the research groups and is used for the practical work on research projects, external orders and expertises as well as for the execution of laboratory practicals in the course of courses.

Analytical methods

  • Electron microprobe laboratory

    CAMECA SX100

    Our Electron microprobe laboratory comes with a state-of-the-art CAMECA SX100 to perform non-destructive, space-solved element analyses. The microprobe is equipped with 5 automated wavelength-dispersive spectrometers (WDS) and an energy-dispersive spectrometer (EDS), which can be used to make qualitative and quantitative element analysis of the elements Beryllium-Uranium. Detection limits of 10 ppm to 100 ppm can be achieved depending on the element concentration in the sample and measurement time.

  • Laser ablation

    Femtosecond laser ablation

    We developed a novel laser ablation system to be used as micro-analytical tool in the elemental and isotope analysis of solid materials. The system is based on a femtosecond all solid-state Ti-sapphire based Laser operating at a fundamental wavelength tunable between 775-785 nm coupled to frequency conversion setup to produce deep UV laser radiation at wavelength of 196 and 262 nm. The system is combined with ICP based analytical intrumentation (ICP-OES and MC-ICP-MS).

    Contact: Dr. Ingo Horn

  • Multi collector-inductively coupled plasma-mass spectrometry (MC-ICP-MS)

    ThermoFinnigan Neptune MC-ICP-MS

    [Translate to English:] Das Neptune MC-ICP-MS

    The study of isotope compositions of different substances is a broad field of scientific research that helps to elucidate processes of e.g. dissolution and precipitation in environmental studies, may provide an age information of rocks and minerals, or the formation of Earth, Moon, and the solar system, just to name a few.
    For isotope research, multi collector-inductively coupled plasma-mass spectrometry (MC-ICP-MS) represents a versatile and reliable tool for precise analyses of isotope ratios of various elements. The plasma source allows ionization of many elements, either being introduced via an aerosol or a solution.

    The Institute of Mineralogy uses a ThermoFinnigan Neptune MC-ICP-MS instrument equipped with 9 Faraday detectors, one secondary electron multiplier (SEM, fixed), and two compact discrete dynode (CDD) SEMs for isotopes with very low signal intensities (< 106 cps; attached to the L4 and H4 Faraday detector, respectively). One amplifier with a 1012 Ω feedback resistor can be selected for a low signal intensity (typically < 5*10-13 A ≡ 50 mV), and nine amplifiers with 1011 Ω resistors are installed enabling measurement of signals of up to 5*10-10 A (≡ 50 V).

    Contact: Dr. Ingo Horn

  • Trace element analyses

    ThermoScientific Element XR

    Our ThermoScientific Element XR double-focusing sector field-inductively coupled plasma-mass spectrometer (SF-ICP-MS) is equipped with a Faraday detector and a dynode combined with a secondary electron multiplier (SEM). Hence it allows detection of a wide range of signal intensities (the dynamic range of counts per seconds encompasses 1012 cps). This enables the analyses of ultra-trace element levels simultaneously with major elements. Three different modes of mass resolution allow separation of molecular interferences from signal peaks of interest. Except for H, He, C, N, O, and the noble gases, the Element XR at the Institute of Mineralogy is capable of analyzing every element of the periodic table.

    Contact: Dr. Stefan Schuth

  • Optical emission spectrometer

    Varian 715-ES

    The ICP-OES in our institute is an optical emission spectrometer of the type Varian 715-ES from VARIAN with an radial inductively coupled plasma and a patented VistaChip CCD simultaneous detector combined with an echelle raster. We use the ICP-OES for measuring major and trace elements in solution (mainly in 3% HNO3) or couple it to a femtosecond laser. Figure 2 shows elements that can be detected with the OES. The detection limits are different for each element, they are in the range of around 0.05 to 500µg/L. For precise determination of low trace element concentrations, the ELEMENT XR is available at the institute.

    A reliable CETAC ASX 510 autosampler is available for high sample numbers. The ICP-OES is working with a 2 ml conical quartz glass nebulizer, a cyclone spray chamber, and torches made of quartz glass.

    Contact: Alexandra Tangen

  • Laboratories

    Clean-air workstations

    We have clean-air workstations that were installed by MK test facilities in 2002 and modernized by Arias GmbH in 2016. Each workplace is equipped with three pipettes (BioHit; 20 -200 µL, 100 - 1000 µL, 500 - 5000 µL). In addition, we offer workstations with two PicoTrace heating plates each for sample digestions. A third workstation is equipped with a PicoTrace heating plate for use with the PicoTrace DAS high-pressure high-temperature digestion system for temperatures up to 230 °C. The system can also be operated with perchloric acid, which is neutralized in an acid neutralization unit. All eight heating plates can be programmed via Arias control modules (including heating and cooling ramps as well as defined operating times).

    Further devices:

    • separate systems for the production of water with a degree of purity 18.2 MΩ (Millipore Milli-Q Reference or Advantage systems)
    • distillations for the production of low blank HNO3 (quartz glass distillate) and HCl (PicoTrace dome distillate)
    • microwave digestion system MLS Start + Terminal 640 Programmable for up to 12 samples, vessels made of Teflon® or quartz glass can be used
    • an acid neutralization unit can be connected to the microwave if required. programmable centrifuge, max. 5000 rpm / 4472 g (Type 3-15, Sigma Laboratory Centrifuges)
    • programmable heatable ultrasonic bath (water temperature adjustable from 20 to 80 °C) (Omnilab)
    • Scales: Sartorius CP2201-OCE (max. 2.2 kg), and Sartorius CP225D-OCE (max. 220 g), placed in a separate workstation equipped with three pipettes (BioHit) and an ionizer (Sartorius)
    • 4-channel peristaltic pump (Masterflex system, Cole-Parmer Instrument Company)
    • programmable overhead shaker, which can hold vessels with volumes of 15 or 50 mL (Intelli-Mixer RM-2-System, laboratory technology)
    • vacuum filter system for aqueous samples (Sartorius, System 16510)

    Contact: Dr. Stefan Schuth | Alexandra Tangen

  • IR spectroscopy

    FTIR spectrometer

    At the institute three FTIR-spectrometers are available:

    • Bruker Vertex 80v: spectral range 50-30000 cm-1
    • Bruker IFS66v: spectral range 50-10000 cm-1, it has additionally a Raman-module FRA 106 with NdYag-laser (1000 nm) fitted. In addition, it is possible to measure temperature-dependent up to 600°C with a special sampleholder/oven-combination
    • Bruker IFS88: spectral range 50-30000 cm-1, it is equipped with an IR microscope II. In addition it can be used with an heating/cooling stage in the temperature-range from -196 to 600°C or an high-temperature-heating-stage up to 1200°C

    Contact: Prof. Dr. Claus Rüscher | Prof. Dr. Harald Behrens

  • Karl Fischer titration

    Mitsubishi Titrator CA100

    The procedure has proven itself for the determination of the water content of solids such as minerals, glass and rocks:

    • Programmer-controlled heating of samples in a platinum sample holder using a hf generator
    • measurement of released water

    Contact: Prof. Dr. Harald Behrens

  • UV-VIS spektrometrie

    Colorimetric determination of Fe2+/Fe3+

    The procedure has proven itself for the determination of the water content of solids such as minerals, glass and rocks:

    • sample dissolution in concentrated HF
    • the Fe2+/Fe3+ ratio is preserved using the reversible reaction with
      V5+: Fe2+ + V5+ ⇔ Fe3+ + V4+
    • measurement of the absorption in visible light (Shimadzu UV 1800) caused by a red Fe2+-2,2-Bipyridil-complex
    • determination of total Fe in the same solution via complete reduction of Fe3+

    Contact: Prof. Dr. Harald Behrens 

  • CS analyzer

    ELTRA CS 800 analyzer

    Analyses of carbon and sulfur concentrations in metals, plants, and rocks are performed at the institute by using an ELTRA CS800 instrument. The sample material is weighed into a ceramic crucible. Iron and tungsten chips are then added to support later melting and oxidation of the sample. The crucible is transferred into  a sealed furnace which consists of an induction coil with the crucible resting in the centre of the coil. Induction of a strong magnetic field melts the iron and tungsten additives and ultimately also the sample material, and addition of oxygen oxidizes the released carbon and sulfur as CO2 and SO3, respectively. These gases are transferred to and detected by an infrared detection unit. The measured intensities are then converted into concentrations of C and S or CO2 and SO3.

    Contact: Dr. Stefan Schuth

  • Impedance spectroscopy

    Novocontrol Alpha-Analyzer

    A small AC-voltage is applied on solid materials using a Novocontrol Alpha-Analyzer in the frequency range of 1 MHz down to 10-3 Hz to determine the dielectric properties of the material by measuring the resulting electrical current. A Novocontrol ZG4 connection unit allows the 4-point-probe of dielectric sample characteristics. A high temperature sample holder in combination with a Nabertherm tube furnace, offers the possibility of temperature depending measurements from 20 °C to 1000 °C.

    Contact: Prof. Dr. Harald Behrens

Structural methods

  • Differential thermal analysis/thermogravimetry (DTA/TG)

    Setaram Setsys Evolution 1750

    Determination of water contents of solids, determination of phase transitions, glass transition temperatures, decomposition temperatures and energy balances of chemical reactions.

    Method:

    • Computer-controlled heating of samples in corundum crucibles up to 1600°C
    • analysis of mass variations using a microbalance with a precision of ±0,04 µg
    • simultaneously temperature difference measurements to a reference using Pt-Rh-thermocouples for determination of characteristic energy conversions
    • experiments can be performed in different gas-atmospheres or under vacuum

    Contact: Prof. Dr. Claus Rüscher

  • Characterization of pore space

    "Wood's metal"

    The method yield supplementary information to Hg-porosimetry and tomography. Pathway for fluids in rocks and other ceramic materials can be determined. Pores and holes in porous materials can be characterized by intrusion of alloys such as "Wood's Metal" (50 Bi, 25 Pb, 12.5 Sn and 12.5 Cd in wt%; melting point of 78°C) or „Rose`s metal“ (50 Bi, 25 Pb, 25 Sn in wt%; melting point of 94°C). At a pressure of 550 bar connective pores with equivalent diameters as small as 20 nm are intruded with the molten alloy. Sample size of 5 mm; temperatures typically up to 120°C. After cooling polished sections are prepared and analyzed using an electron microscope.

  • Rasterelectrone microskope

    Jeol JSM-6390A

    Scanning electron microscopy plus qualitative and quantitative element-analysis for scientific investigation of solid-state materials in geosciences, civil engineering and cultural heritage preservation.

    Contact: Prof. Dr. Josef-Christian Buhl

  • Raman spectrometer

    Bruker Senterra Raman spectrometer

    The Bruker Senterra Raman spectrometer is predominantly designed as an high-performance analytical instrument. It is equipped with an Olympus BX series with the FlexFocus™ system for confocal debth profiling and a set of objectives with long and short working distances. The CCD is an ANDOR DU420-OE with a thermoelectric cooling system with the  highest sensitivity between 400 – 900 nm.

    Contact: Dipl. Geow. Marcel Dietrich

  • X-ray powder diffraction

    Bruker D4 Endeavor und Bruker D8 Advance

    X-ray powder diffraction is used for qualitative and quantitative phase analysis of powdery samples for scientific material-analysis. For this purpose two modern diffractometer Bruker D4 Endeavor and Bruker D8 Advance are available. The D4 Endeavor is characterised by its ease of use and its high sample effort, while the D8 Advance can be used for special tasks, like small angle diffraction and temperature-depending diffraction.

    Contact: Prof. Dr. Josef-Christian Buhl

Experimental methods

  • Crystal growth lab

    Crystal growth lab

    A Nabertherm muffle furnace for temperatures up to 1400°C as well as three special furnaces for six steel autoclaves are available for the preparation of polycrystalline samples and single-crystals under dry and hydrothermal conditions. Two drying cabinets type Heraeus Kelvitron and a completely equipped wet-chemical laboratory for pre- and post-treatment of samples, complete the instrumentation.

    Contact: Prof. Dr. Josef-Christian Buhl

  • IHPV gas pressure vessel

    Internally heated gas pressure vessel (IHPV) with H2-control

    Both vessels (WHITE and GREEN) are equipped with a Shaw-membrane to monitor the internal H2 pressure; a rapid quench device allows cooling rates of  ~150°C/s. An Ar-H2 mixture is used as pressure medium to adjust redox conditions inside the vessel. One vessel (WHITE) is equipped with a high-pressure low-flow metering valve to conduct decompression experiments with continuous decompression rates (~0.0002 to >10 MPa/s). The maximum heating rate is 80°C/min. The vessels are PC-operated (using itools) allowing e.g. to regulate the temperature path and logging of Ptotal, T, P(H2).
    The vessels are used to perform high pressure-temperature experiments (850 to 1250°C; up to 500 MPa) at various redox conditions (log fO2 = FMQ+0 to FMQ+3) e.g. to investigate magmatic processes in earth’s crust or upper mantle and to synthesize high pressure materials. Decompression experiments can be conducted at geologically relevant P-T conditions to study degassing of volcanic systems.

    Contact: Prof. Dr. Harald Behrens

  • Autoclaves

    Argon-CSPV

    The autoclaves of Tuttle-type (Cold Seal Pressure Vessel) are externally heated by a tube furnace and are pressurized with argon. Maximum temperatures are at 850°C at the maximum pressure of 500 MPa which can be applied in this system. Oxygen fugacity in the interior of water-filled capsules is about two orders of magnitude above the Ni/NiO buffer. Two vertically oriented autoclaves are equipped with a magnetic system allowing rapid heat and rapid quench of samples. With a three-zone furnace temperature gradients can be imposed to the autoclave.
    The Ar-CSPV’s can be used for experiments at high pressure and temperature under oxidizing conditions, e.g., to simulate hydrothermal and magmatic processes in the Earth’s crust and in the upper mantle. Hydrothermal synthesis of minerals may be possible as well.

    Contact: Prof. Dr. Harald Behrens

    H2O-CSPV

    The autoclaves of Tuttle-type (Cold Seal Pressure Vessel) are thick walled high temperature alloys with blind hole and externally heated by a tube furnace. The wall to hole relationship is around 5:1 the closure nut is located outside the hot zone of the furnace. The autoclaves are pressurized with water (H2O) and used for maximum temperatures of 900°C at 100 MPa, and 800°C at the maximum pressure of 500 MPa. Oxygen fugacity in the interior of watersaturated capsules is controlled at Ni/NiO buffer. Compressed air is applied for the cooling device of the autoclaves.
    The H2O-CSPV’s can be used for experiments at high pressure and temperature under oxidizing conditions, e.g., to simulate hydrothermal and magmatic processes in the Earth’s crust and in the upper mantle. Hydrothermal synthesis of minerals may be possible as well.

    Contact: Prof. Dr. Harald Behrens

Workshop and preparation

Our workshop is equipped with a three-axis CNC milling machine type DMG 635 and a Deckel FP4M. Further machines are a CNC lathe of type Gildemeister NEF 320 and several older models. The main use of this machine is the production of parts for the high pressure temperature apparatuses of experimental petrology and scientific instruments.

Workshop manager

Non-public person