General

This guide is designed as a starting point for sample preparation for experiments at SXRMB. Please talk to beamline staff about your specific samples and unique requirements to ensure high quality data collection is possible.

Sample preparation of WHMIS controlled products must be done in a laboratory. The Canadian Light Source has several user accessible labs. Basic lab access requires the completion of CLS Laboratory Safety Training. Most lab space and equipment can be reserved using the user portal. To find more details about available lab spaces and equipment, click here.

Non-WHMIS controlled products may be prepared in the SXRMB sample preparation room.

Sample Types

SXRMB can be used to characterize a variety of sample types, including powders, liquids, thin films, pellets, foils, geological, biological samples and more. See below for further insight into types of samples used on each endstation. Your samples must be approved in the user portal prior to bringing them on-site for measurement.

Solid State Endstation

To prepare powder samples for measurement on the solid state endstation, please see the following guide:
Mounting Samples onto the Solid State Sample Plate

When mounting samples on the back of the plate, use a YAG crystal below the bottom screw, and a YAG crystal at the bottom of the plate to assist with beam location. Ensure there is a couple centimetres of space between the lower screw and the YAG crystal, or the plate won't hang properly in the chamber. On the front of the plate, typically only one YAG crystal is needed at the bottom of the plate (as in the image on the left), since there is a crystal built into our sample chamber just above the plate location.

If your samples are pellets, films, foils, felts, and more, you may also be able to simply attach your samples to our sample plates using carbon tape. Please contact us about your samples in advance!

Microprobe Endstation

If you have powder samples, they can be prepared similarly to the solid state endstation. Extra care needs to be taken to ensure the powder is spread uniformly and flat, because uneven surfaces will affect the quality of your XRF mapping experiments and lead to shadow effects. When preparing a powder sample on carbon tape, use a tool with a flat and smooth surface to press on and smooth the sample surface. For a bulk sample, its surface should be polished.

Please see the following guideline for the microprobe sample preparation:

Microprobe sample preparation

The beamline scientists will show you where samples can be placed on the microprobe sample plate in order to fall within the motor limits of our sample stage. For a bulk sample with a certain thickness, the thickness should be measured with a digital caliper so that the beam's focus plane can be adjusted according to the sample surface.

Have other types of samples? We have measured thin layers, films, geological and biological samples. We have even measured the cross-section of a T-rex rib bone! Samples need to be able to fit on our plate and in our vacuum chamber set up. Please contact us about your samples to discuss feasibility.

Ambient Table Endstation

The ambient table endstation accommodates a variety of set-ups and sample types, including liquid and solid in situ experiments. This endstation can also be configured for transmission measurements.

Ambient Table Gas Chamber

If running samples using the SXRMB ambient table gas chamber, the sample holder plate shown below is used, allowing for transmission measurements (if the beam is able to pass through the sample).

For this holder, make sure your sample fills the entire slot to ensure the beam is passing through the sample.

The following video provides guidelines for the preparation of solid samples for transmission:

• SSRL XAS Solid Sample Plate Preparation

Liquid Sample Holder

Aqueous solutions are often excellent samples for fluorescence and transmission measurements because their uniformity ensures high-quality data.

Here’s the SXRMB liquid sample cup used to measure XAS:

Six Shooter Sample Holder

This sample holder is used in our tube furnace. Typically we recommend 10 mg of total powder per hole. Dilutions with boron nitride will likely be necessary for a good transmission signal. Calculators and software such as Hephaestus may be used to calculate the necessary mass of sample needed for a desired edge jump.

Custom User Set-Ups

Please contact us to discuss your research ideas, sample preparation, and possible configurations. Users are encouraged to bring forward ideas for new endstation setups if the beamline does not currently have an experimental setup that will suit their needs.

High-Energy X-ray Photoelectron Spectroscopy Endstation

The High-Energy XPS endstation is ideal for profiling thin film samples, but can also accommodate other solid sample types, similar to the solid state endstation.

There are copper or aluminum sample plates available for this endstation.

Please contact us about your sample to discuss feasibility.

Sample Storage

Samples mailed to SXRMB can be stored until beamtime. Some options include:

• Refrigerator (5°C)
• Freezer (-20°C)
• Extra cold freezer (-80°C)
• Desiccator

Need a storage location not listed? Please contact beamline staff to figure out a solution.

Sample Disposal

Please take your samples with you when your beamtime is finished.