LINXS’ new webinar series aims to get users ready for beamtime

– With this initiative, we want to emphasise the importance of both sample preparation and pre-scanning for a successful beamtime experiment, says LINXS Co-Director, Emanuel Larsson, who is organising the new webinar series, Preparing for Beamtime, together with LINXS themes: Heritage Science, and Environment and Climate.

He explains that such a series is well needed, as researchers from both academia and industry are becoming more interested in using X-ray and neutron techniques, coupled with a growing competition for beamtime at various synchrotrons and neutron facilities.

Emanuel Larsson is LINXS Co-Director and a researcher at the Department of Experimental Medical Science at the Faculty of Medicine, Lund University.

– From working with beamtime experiments for many years, my feeling is that new users might often miss the first step of a successful experiment: that of getting to know your sample and how it should be mounted and prepared. Instead, the urge is to go directly to the synchrotron or the neutron facility, where you might get disappointed if you do not get workable data directly, says Emanuel Larsson.

The series will focus on different lab-based techniques to pre-scan, prepare different samples, as well as testing out sample environments prior to final beamtime. Different speakers – from various synchrotron and neutron facilities, heritage science and environmental science – will cover and elucidate key preparatory work in relation to techniques such as X-ray and neutron tomography, diffraction, scattering and spectroscopy. The aim is to build knowledge on how one can optimise the sample and sample environments – and ultimately become more adept at performing experiments at large scale facilities.

Image credit: Martina Trocchi & Alessia Nava, Sapienza University of Rome, Italy

– With pre-scanning you create a feedback loop which gives you an option to resolve potential sample issues, Emanuel explains. Very often, they relate to the sample contrast, where you are not able to see the structure or composition of a material properly. Another problem can be that your sample gets destroyed or dries out during longer scanning periods. Both are problems that need to be handled before you arrive at the large-scale facility.

Example of food pharma experiment highlights methodology

He highlights an example of a food-pharma freeze-drying experiment him and his colleagues worked with, since the methodology can also be translated to other sciences.

At first, they scanned the sample in its native form with a diameter of 2 cm, but the pre-scans revealed that it was too thick to get the desired contrast. Then they cut the sample with a razor blade, but this induced cracks in the sample, leading them to produce new samples with a diameter of 5 mm instead. That lead to another problem: the structure was no longer representative of freeze-drying. After several more pre-scans and tests, they finally came up with a working solution: to use a cylindrical knife to cut out an inner part of 5 mm from the original sample with a diameter of 2 cm and put that part in a vial – which then produced the desired contrast along with representative structure of freeze-drying.

– The interesting thing is that as a bonus to the lab-based pre-scans, whose initial goal was merely to prepare for beamtime, we also managed to produce two publications on these results, in addition to the final beamtime at ForMAX beamline at MAX IV.

Comissioning a new sample environment for freeze-drying. Left) in a lab scanner, RX Solutions, Division of Solid Mechanics, Lund University. Right) Same sample environment comissioned at the ForMAX beamline at MAX IV.

He continues:

– Pre-scanning and sample preparation goes hand in hand and is a re-iterative process, because more often than not you have to cut your sample or change its diameter, or you need to test the functionality of your sample environment in advance. It allows you to iron out any problems and create the most optimal conditions for further experiments, says Emanuel Larsson.

Increases chances of getting beamtime

Doing your homework doesn’t only set you up for better experiments, it can also increase your chances of getting beamtime in the first place – since many experienced users would attach lab-based results to their beamtime application, in order to show its feasibility. Because the reality today is that many beamlines are heavily overbooked, sometimes resulting in fierce competition. And although it is not a requirement, it is almost an unwritten rule that you attach pre-scan results to your proposal these days.

– The end goal with this series is to revolutionise how you approach beamtime, prepare for experiments, and collaborate with beamline scientists. We hope that it will aid researchers to get creative with their samples and sample environments – and become open to try and solve research problems ahead of beamtime.

First speaker: Dr. Diego Dreossi from the Elettra Synchrotron, Italy

The webinars series will feature around one to two talks a month. It starts on 24th September, with a talk by Dr. Diego Dreossi from the Elettra Synchrotron, Italy. He will discuss how various instruments can be used to perform X-ray microtomography, which is a well-established technique for visualizing and analyzing the three-dimensional internal structure of objects, in the laboratory, with special focus on defining the resolution one needs, through visualizing details of a certain size (spatial resolution); distinguish regions that are very similar to each other (contrast resolution), and monitoring something that is happening (temporal resolution).

About the webinar series: Preparing for beamtime

The Preparing for Beamtime webinar series details the laboratory preparation work that should happen prior to beamtime to ensure that users are well-prepared for their time in synchrotrons or neutron facilities. The goal of this webinar series is to emphasise the importance of lab-based pre-scans with relevant techniques before beamtime. In some cases, multiple techniques may be needed to confirm a finding.

Speakers will cover different techniques, including imaging, diffraction, scattering, and spectroscopy of various selected applications. They will focus on how lab-based scans and preparatory work, including testing sample environments, can help strengthen beamtime proposals and make the most of each moment during a beamtime.

It is hosted by the Environment & Climate and Heritage Science themes.

Read more about the webinar series