The following sample environments are available at the beamline:

  1. Liquid sample changer coupled to a temperature controlled flow-through capillary cell: A sample changer for liquids based on a 28 port cheminert stream selector (Valco Instruments) is available. This system enables loading 25 samples simultaneously, selecting them remotely and transfering to the flow-through capillary cell (quartz, ID 2 mm and OD 2.1 mm). The capillary can be cleaned and dried in between successive measurements. This capillary cell is operated with minimum air gap and it is temperature controlled by a Peltier stage (the range about 5 to 80 °C ). In addition, different types of capillary cells are available for standard measurements.  One made from bio-compatible polycarbonate with a wall-thickness of either 0.1 mm or 0.05 mm and a diameter of 2.0 mm. The second type is  made of quartz or borosilicate capillaries, with a range of different diameters (1.0 mm - 2.0 mm). The flow-through cell allows accurate measurements of sample and solvent scattering of low scattering liquid samples and obtain reliable background subtraction.
  2. Stopped-flow rapid mixing device: The device is based on a commercial instrument (BioLogic, SFM-4000) with four stepper motor driven syringes and three mixers. A home-made SAXS/WAXS flow-through capillary cell (diameter ~1.3 mm) is adapted to the mixing chamber. The flow can be stopped with millisecond accuracy using a solenoid driven hard-stop. The dead time of mixing is about 2 ms for flow rates exceeding 6 ml/sec. This device can also be used to perform a temperature jump over the range 5 - 70 °C with a few millisecond deadtime.
  3. Stress controlled rheometer: The stress controlled rheometer is a commercial Haake RS6000  and the shaft drives an X-ray transparent Couette cell. The concentric cylinders (inner diameter 20 mm, outer diameter 22 mm, and height 40 mm) are machined out of polycarbonate (lower background) and aluminum or vespel for higher temperatures up to 170 °C and good organic solvents with wall thickness around the beam position ~100 µm. Minimum sample volume required is about 2.5 ml. For only small quantity of the sample, a coaxial capillary shear cell is available (~50 µl) but at the expense of the sensitivity of rheological measurements. For highly viscous samples, a plate-plate type shearing geometry is also available.
  4. Mettler-Toledo heating stage (HS82) : It is used to perform programmed temperature ramping and quenching (20 °C/min, nominal stability of 0.1 °C) primarily in crystallization studies. In addition, this setup can be used to change the sample temperature over a wide range (-50 to 350 °C depending on the sample container availability). The solid samples (in the form of a circular disc - diameter 3 to 10 mm) can be mounted directly and the liquid samples can be contained in sealed capillaries (diameter 1 to 2 mm).
  5. Linkam heating stage: (THMS600/TMS94) It can perform faster temperature ramping and quenching (up to 80 °C/min, nominal stability of 1 °C) primarily in crystallization studies. This setup can also be used to change the sample temperature over a wide temperature range (-100 to 600 °C). An adaptor to mount solid samples (in the form of a circular disc - diameter 3 to 10 mm) and liquid samples (in sealed capillaries of diameter 1 mm) is available
  6. Pressure-jump setup: It is based on a high force piezo stack (Piezo Systems Jena) which can dynamically compress a small volume (~30 µl) and reach a pressure up to 1 kbar in less than 1 ms. Smaller amplitudes of a few 100 bar can be reached in a few 100 µs. This cell also permits to perform static SAXS/WAXS experiment up to 1.5 kbar and 100°C. The pressure windows are polished diamond (thickness ≈ 1 mm) and the stability is within a few bars.
  7. Magnetic field: It is based on permanent magnets arranged periodically as in the undulator. The field can be varied from 0.1 mT to 1.5 T. The direction of the magnetic field can be either perpendicular or parallel to the beam direction. An oven adapted for both capillaries and flat cells is also available to perform measurements in the temperature range of (25 to 300 °C). This setup can be used as an alternative to shear flow for aligning mineral liquid crystal-like samples.
  8. Peltier controlled automatic sample changer:
    • Four position sample changer: The temperature (5 to 100 °C) is controlled by a Peltier element. The samples are contained in liquid tight aluminium cells with thin mica or mylar windows. The sample thickness can be 0.5, 1.0 or 2.0 mm. The setup is available for all users. However, windows have to be provided by the users (supplier info).
    • Industrial sample changer: A more advanced version of the above setup is available explicitly for industrial experiments. 30 sample cells can be placed at the same time. The temperature is controlled by Peltier elements and can be varied from 10 to 120 °C in less than 30 minutes. The gas tight sample cells are made of aluminum with nickel coating and mica windows.
    • Capillary sample changer: This set-up allows to mount 8 sealed capillaries of diameter ranging from 1 to 2mm. The temperature can be varied from 5 to 120 °C. Best adapted for measurements around 12.4keV are quartz capillaries with a diameter of 1.5 or 2.0mm. Please make sure to carefully verify the diameter of the capillaries before using. This ensures faster loading of the samples and facilitates accurate intensity calibration of the scattering curves.
      The setup is less adapted for the study of low scattering liquid samples due to insufficient accuracy of background subtraction using different capillaries for sample and solvent.
  9. Ancillary equipments:
    • Oscilloscopes: Lecroy Wave Surfer (44 Xs, 400 Mhz) and Lecroy 9361
    • Laboratory power supplies:

    Delta SM 70V-22A,
    Lab trisource 30V 1A, 5V 1A, ±15V 0.2A,
    Olotronix trisource 30V 1A, 5V 1A, ±15V 0.2A.

    KEPCO high voltage bipolar (±1000 V, 40 mA).
    Midec power supply.

 

Further Information