top of page

Beamline Manual

Sample Preparation
Technique choose
XAS

Position the holder inside the acrylic sample chamber for X-ray exposure.

XRF
Micro-XRF
WAXS
TXRF 1
MX 1

Powder Sample Preparation for TM-XAS Analysis

image_edited.jpg
image.png

 Plastic sample frame

1. Grinding the Sample

Grind the sample in a small agate mortar with a pestle until it becomes a fine powder.

2. Preparing the Sample Frame

Cut a piece of hard paper or a plastic sheet to create a sample frame.

Kapton tape

image.png

Attach Kapton tape to one side of the holder

image.png

✔ Spread evenly
✔ Smooth surface

✔ No pinhole

image.png

3. Applying Kapton Tape

Place a thin Kapton (polyimide) tape on the frame, sticky side facing up. The tape should be thinner than the sample layer.

4. Mounting the Sample
Weigh the appropriate amount of powder to achieve the optimal mass, then spread it evenly across the sticky window area. Ensure the layer is homogeneous and free of pinholes.

Finally, seal the sample area with another piece of Kapton tape.​

Seal the opposite side with Kapton tape

💡Tip: Calculate the required sample mass using the XAFSmass program.         The software and user manual are available at: https://www.cells.es/en/instruments/beamlines/bl22-claess/software-manuals#

Sample Preparation for Bulk XRF

image.png
image.png

1. Press pellets

Prepare cylindrical pellets of various diameters (6, 10, 13, 16, and 20 mm)  using a Specac press machine for 1 minute at 1 ton force.​

image.png
image_edited.jpg

2. Attach to Kapton tape

Adhere each pellet to Kapton tape (Lanmar Inc.) for stability.

3. Mount in magnetic holder

Place the pellet in a magnetic sample holder.

image_edited.jpg

4. Install into acrylic chamber

Sample Preparation for Micro-XRF Analysis

Prepare your samples for precise Micro-XRF measurements. Various types of samples can be analyzed in their original form, including:

  • Historical paintings

  • Heritage artworks

  • Forensic objects

A helium sample chamber is available for Micro-XRF measurements.
Maximum sample size: 3 cm (W) × 5–6 cm (H).

image_edited_edited.jpg
image_edited.jpg

Sample holder for micro-XRF measurement: the left for helium purge and the right for air environment

Sample Preparation for WAXS Analysis

Grind and crush the sample into a fine powder to ensure uniformity. Seal a small amount of the powdered sample between Kapton tape and securely place it onto the XRD sample holder for measurement.

Sample Preparation for TXRF Analysis.

✨ For solid samples

  • ​Grind and sieve the material into fine powder.

  • Digest with acids:  

  • Single (nitric, hydrochloric, hydrofluoric)

  • Mixed (nitric + hydrochloric, hydrogen peroxide, hydrofluoric).

  • Apply heat during digestion to ensures complete breakdown.

  • After spin down, separate the liquid fraction.

  • Add an internal standard (e.g., gallium, yttrium, chromium, zinc) for accurate measurement.

image.png

Steps for solid sample preparation for TXRF analysis

💧 For liquid samples

  • Usually require little or no pretreatment.

  • Deposit a droplet onto a clean sample carrier using a micropipette.

  • Dry the droplet in a beamline oven before measurement.

Sample Carrier Preparation for TXRF Analysis

Suitable substrates for TXRF:

  • Silicon dioxide (quartz glass)

  • Perspex® (polymethyl-methacrylate, PMMA)

  • Glassy carbon

  • Sapphire (Al₂O₃)

  • Silicon wafer (preferred for smooth, polished surface and high reflectivity; available at the beamline.). 

✨Preparation using silicon wafer​​​

1. 🔪Cutting the wafer

  • Use a diamond cutter to scratch the wafer surface.

  • Lift the wafer with a toothpick and gently press opposite sides.

  • Follow the crack lines to complete the cut.

  • Recommended size: ~1 × 2.5 cm for proper placement on the sample stage.

2.  🧼Cleaning and storage

  • Place the cut wafer in a clean container to avoid contamination.

  • Blow the wafer with nitrogen to remove dust particles.

3. ✅ Purity check

  • Verify wafer cleanliness by checking the XRF spectrum.

  • Ensure no contaminants are present before depositing the sample drop.

4. 💧Sample deposition

  • Once purity is confirmed, carefully deposit the sample drop onto the wafer surface.

 👉 Additional resource:

      For a detailed demonstration of silicon wafer cutting, refer to            the YouTube video: “Process of Cutting the Silicon Wafer”
      https://www.youtube.com/watch?v=wHnjxlx7HyM&t=28s

image.png

Steps for cutting the silicon wafer for TXRF measurement

Protein Crystal Preparation for MX Analysis

  • Prepare single protein crystals with a minimum size of 200 μm for optimal X-ray diffraction at the beamline (beam size ≈ 200 μm).

  • Crystal growth conditions vary depending on the chosen precipitants; ensure proper cryoprotectant preparation for cryo-crystallography.

  • Standard tools (loops, vials, tongs) are available at the beamline.

image.png

Single protein crystal prepared for X-ray diffraction.

image.png

Protein crystal cryocooled in a fiber loop for cryo-crystallography.

bottom of page