SAXS beamline

SAXS support laboratory

  Our 70 m2 big support laboratory is divided in two parts, in which the bigger share of 43 m2 is occupied by the chemistry lab. This unit serves mainly for sample preparation and analysis for both, in house research and external SAXS user groups. In the X-ray laboratory a SWAXS camera for simultaneous small and wide angle scattering (Hecus X-ray Systems, Graz, Austria: www.hecus.at) allows on-site testing of samples before moving on to the SR beamline.

The chemistry lab is equipped with:
  • Micro centrifuge (max. 13200 rpm; model 5415D from Eppendorf , Hamburg, Germany)
  • Chemical fume hood, equipped with a carbon filter for general organic solvents (model GS8000 from Strola, Italy)
  • Vacuum drying oven (min. pressure 1 mbar; max. T: 200 °C, precision +/- 0.4°C; Binder WTB, Tuttlingen. Germany)
  • Balance (min.-max.: 0.001 - 220g; model 770 from Kern & Sohn, Balingen, Germany)
  • Magnetic stirrer with heating plate and thermometer, temp max 260°C
  • Vortex for microtubes (model MR 3001 and REAX; both from Heidolph, Schwabach, Germany)
  • Two water baths :

-Unistat CC, freely programmable in the range from -30 to 100°C (Huber, Offenburg,  Germany);

-Lauda M3, available for heating only (Lauda-Könighofen, Germany)

  • Ultrasonic bath with water heater (VWR International, Milano, Italy)
  • Ultrasonic processor equipped with a 3 mm probe (Sonics VCX130, SY-LAB Geräte GmbH, Germany)
  • HPLC pump, Pharmacia LKB; working range, 0,01-9,99 ml/min, 0,1-40MPa
  • HPLC pump, Gilson 307; working range, 0,01- 5 ml/min, 0,1-60MPa
  • Three syringe pumps, low pressure; flow rate range, 1µl/hr – 2120 ml/hr
  • Four syringe pumps, high pressure: P max ~ 60 bar
  • Three high pressure infusion modules: P max ~ 690 bar
  • UV-VIS spectrometer:  Besides a standard 10 mm path length cuvette holder, the UV-VIS spectrophotometer (Cary 60, Agilent Technologies) is equipped with a Slide-Mounted External Specular Reflectance accessory which allows specular reflectance measurements to be made at a fixed angle of 30°. This accessory is suitable for studies of the film thickness on metallic substrates and measurements of epitaxial film thickness. Interchangeable masks for examining small samples or small areas of large samples are provided (3 mm, 6 mm and 13 mm diameters). The instrument can also be used for in situ measurement on liquid samples, through two optic fibers: a Torlon fiber probe, diameter  10 mm, for aggressive solutions, and a  µprobe, 3.5 mm diameter, 10 mm fixed path length, for smaller volumes (approx. 500 µl).                                                          Specifications: double beam Czerny-Turner monochromator, wavelength range 190–1100 nm, fixed spectral bandwidth 1.5 nm, minimum scan rates of 24,000 nm/min (full wavelenght scan time < 3s), maximum measurement rate 80 data points/sec
   

 

  • FT-IR spectrometer (Alpha-T, Bruker Optics): equipped with the following modules for the analysis of different types of samples:  standard sample holder for transmission measurements,; single reflection diamond ATR sampling module for powder and solid analysis, which, due to the wide free working area around the crystal (approx. 350°), allows the analysis of large samples. Specifications: One-reflection Diamond crystal, spectral range: 375 - 7,500 cm-1, working distance (max. sample height): >20 mm; sampling module for contactless reflection measurements in front of the spectrometer. Specifications: spectral range: 375-7.500cm-1, measurement spot: 6 mm diameter, appr. 15 mm in front of the spectrometer


Further, four working benches (one with a water sink), a fridge (+ 4°C) and a separate freezer (- 20 °C), standard glassware, syringes and needles of different sizes, µ-pipettes (p10 - p100 - p200 - p1000), as well as some standard chemical reagents (e.g., chloroform, ethanol, methanol); deionized water (milli-RO and ultrapure milli-Q water) is available.

View of the X-Ray laboratory and Chemistry laboratory:

 
Ultima modifica il Giovedì, 24 Marzo 2022 17:46