NOTOS measurements are usually done on 13 and/or 5 mm diameter pellets (XAS) and capillaries (XRD/XAS). Please calculate the linear absorption coefficient μ before preparing your sample. In the case of XAS measurement, we recommend not exceeding 1.5 cm-1 total absorption to avoid distortion and dumping of the EXAFS oscillations. For XRD calculate the relative absorption (μr) at the wavelength (energy) at which patterns will be collected. Note, to minimize absorption correction μr should be <1 (no correction needed) and never higher than 4.5. μr must take into account the packing density (packing fraction, generally 40-60%).

The following web pages and program provide tools to calculate μ:

• XAFSmass — XAFSmassQt 1.5.0 documentation
• 11-BM Resources (X-ray Absorption) (anl.gov)
• NIST X-Ray Form Factor, Atten. Scatt. Tables Form Page

Quartz and borosilicate capillaries of diameter 0.5, 0.7, 1.0, and 1.5 mm are commonly used at the beamline. Please consider also the wall absorption when preparing your samples:

As a general policy, users need to bring and use their own capillaries to run the experiment.  Capillaries can be ordered from several companies like Hilgenberg, WJM-Glas Müller or CTS Capillary Tube Supplies.

The same policy applies for the use of coin cells in electrochemistry experiments. To order your coin cells, please contact Michael Knapp and Almuth Pfleging.

In case of necessity, NOTOS counts on a minimum storage of capillaries and coin cells. In the case of use during your experiment, you need to return number of pieces used in the shortest time.

Please contact the local contact and try to coordinate with her/him to avoid any change of setup and/or configuration outside the standard working hours.

Data treatment on the beamline can be performed using standard programs like:

• Athena (https://bruceravel.github.io/demeter/)
• GSAS (https://www.aps.anl.gov/Science/Scientific-Software/GSASII)

while a fast data reduction and visualization can be done using the Fast data Analyser (FDA) a Python utility written by C. Marini, oriented to the analysis of X-ray absorption spectra and XRD patterns. A paper is in preparation. The latest version of the code (0.9.3) can be downloaded at this link: https://git.cells.es/cmarini/fda_free/-/blob/master/fda_free.093.7z . Please read the file "README.TXT" to install and run the program.

Capillary setup

Quartz capillary setup available at PD-XAS station

Temperature control for capillaries

FMB Oxford hot air blower

Temperature range: RT – 1223K (RT – 900°C).

To be used with samples in capillaries (quartz ones for temperatures above 700°C).

Detailed description of the equipment can be found at the manufacturer's website.

Oxford cryostream 700 series

Temperature range: 80K – 450K.

To be used with samples in capillaries.

Detailed description of the equipment can be found at the manufacturer's website.

Self-supported pellet cell for gas and temperature experiments

In situ measurements will be perfomed by a cell already in use at SpLine beamline at ESRF. This cell will allows measurement on sample in self supported pellet form in trasmission configuration. The maximum working temperature is 500˚C at ambient pressure.

Reactive Gas System

Since NOTOS will be highly devoted to Catalysis, in-situ processes and other dynamic characterization of materials, an integrated, user-friendly and versatile reactive gas system is under development.

The gas system is expected to be ready on mid-2022.

The gas lines being considered are the following:

1: For not dedicated gas lines, gas for calibration is indicated in bold letters. All dilutions are done in He.
2: No pressure control from Patm to 4bar. In a second stage of the gas system design it is planned to implement a back-pressure controler up to 80 bar.
3: Up to 6 bar for propane
4: Up to 8 bar for propylene
5: Gas for calibration: He

For additional information, doubts or suggestions please contact the beamline staff.

Capillary gas flow cell

We offer a capillary gas flow cell that has been designed and produced by ITQ with the participation of ALBA. This equipment has been developed as part of the RTI2018-096399-A-I00 R&D project, funded by MCIN/AEI/10.13039/501100011033/ and "ERDF A way of making Europe".

For this cell:

• All gases are compatible except NH₃
• Gas in continuous flow or in pulses (microvolumes)
• Atmosferic pressure only (tests at higher pressures ongoing)
• T from RT to 650ºC
• No capillary spinning