Historical Materials BAG

The BAG proposal scheme is beneficial to the Cultural Heritage community as the synergy between existing ‘expert’ user groups is enhanced, and easier and more efficient access is provided to new groups. This is expected to result in an increase in excellent output from the Cultural Heritage community, to reinforce a scientific network of expert users structured around the ESRF, and to initiate new European collaborations in Cultural Heritage.

The “Responsible Scientists” (RSs) of the BAG will act as an interface between users and the main scientific contacts at the ESRF. The RSs will make sure before each beamtime that a planning and declaration is made for the samples and that they are shipped to the ESRF and received in case users will not directly bring them in person. They will also ensure that beamtime is equally distributed between all groups, manage which members can physically join the experiment, ensure a general smooth running of operations, and that each team plays its part  in the dissemination of data.

Currently, the RSs are:

• Victor Gonzalez, CNRS - ENS Paris-Saclay
• Letizia Monico, CNR-SCITEC
• Frederik Vanmeert, Rijksmuseum
• Clement Hole, ESRF

Contact RSs

Scientific contacts at ESRF:

• Main ESRF contact for the BAG organization: Marine Cotte (ID21)
• ID13: Manfred Burghammer
• ID22: Catherine Dejoie

The Historical Materials BAG contains 16 groups from 8 European countries (Italy, France, Belgium, the Netherlands, Spain, the United Kingdom, Czech Republic and Switzerland):

• CNRS - ENS Paris-Saclay: V. Gonzalez
• CNR-SCITEC and SMAArt Centre/University of Perugia, Department of Chemistry Biology and Biotechnology: L. Monico, S. Carboni Marri, A. Romani
• Courtauld Institute of Art: A. Nevin, A. Burnstock
• Politecnico di Milano: D. Comelli
• Rijksmuseum: F. Broers, F. Vanmeert, K. Keune
• Lab-BC - C2RMF: I. Reiche
• Universitat Politècnica de Catalunya: N. Jiménez, N. Salvado
• ESRF and LAMS (CNRS, Sorbonne university): M. Cotte
• IRCP: G. Wallez
• University of Antwerp: K. Janssens
• TU Delft: M. Alfeld
• Institute of Heritage Science ISPC-CNR: M. A. Suzuki
• Institute of Inorganic Chemistry of the CAS ALMA: S. Svarcova
• University of Applied Sciences and Arts Institute of Materials and Constructions, Lugano: P. Moretti
• University of Cambridge Department of Chemistry: E. Purdy
• University of the Basque Country Analytical Chemistry: M. Maguregui

The following beam lines and experimental conditions are available to the BAG partners.

High-angular resolution XRD at ID22: 

• Samples: (poly)crystalline powders or historical samples

• Sample requirements: the samples are contained in capillaries

• Environmental conditions: ambient

• Energy: ca. 35 keV

• Scan range: 3 – 20° 2θ

• Typical analysis time: ca. 40 min/powder or ca. 2 hours/historical sample

• Instrumental function collected on a Si standard (FWHM of (111) peak) ~ 0.0027° (2theta)

 

High-spatial resolution 2D µXRD imaging at ID13:

• Samples: thin sections (preferable) or cross-sections

• Sample requirements: XRD measured in transmission

• Environmental conditions: ambient

• Energy: ca. 13 keV

• Beam size: ca. 2x2 µm²

• Data collection mode: transmission

• Typical analysis time: 10-30 min/sample ( ~10ms per pixel)

• Additionally XRF data can be collected simultaneously

In order to facilitate the smooth operation of the experiments, no changes to the experimental parameters will be made during a beam time allocation.

As a partner of the BAG, you agree to follow the standard ESRF rules (safety, sample declaration, GDPR, travel rules, data policy, ...).

Useful links:

esrf user policies and rules

esrf publications

In particular, for each publication, please :

   -  Mention the beamline(s) on which you obtained data, the BAG program and acknowledge the assistance from ESRF staff. You can use a sentence such as:

We acknowledge the European Synchrotron Radiation Facility for provision of synchrotron radiation facilities and we would like to thank xyz for assistance in using beamline ID13/ID22 (proposal HG-172 [if your beamtime was before August 2023], HG-213 [from Aug 2023], HG-237 [from Dec 2024] pilot of a BAG project supported by the European Union’s Horizon 2020 research and innovation programme under grant agreement No 870313, Streamline). 

   -  You can mention the reference publication:

Cotte, M.; Gonzalez, V.; Vanmeert, F.; Monico, L.; Dejoie, C.; Burghammer, M.; Huder, L.; de Nolf, W.; Fisher, S.; Fazlic, I.; Chauffeton, C.; Wallez, G.; Jiménez, N.; Albert-Tortosa, F.; Salvadó, N.; Possenti, E.; Colombo, C.; Ghirardello, M.; Comelli, D.; Avranovich Clerici, E.; Vivani, R.; Romani, A.; Costantino, C.; Janssens, K.; Taniguchi, Y.; McCarthy, J.; Reichert, H.; Susini, J. The “Historical Materials BAG”: A New Facilitated Access to Synchrotron X-ray Diffraction Analyses for Cultural Heritage Materials at the European Synchrotron Radiation Facility. Molecules 2022, 27, 1997. https://doi.org/10.3390/molecules27061997

    - Mention the DOI for the data measured at ESRF (beginning with "10.15151/"). Rather than using the DOI automatically generated and sent via email at the end of each experiment session to all participants of the session, we recommend you to mint your own DOI, for your own lists of datasets. Please watch this how-to video. Please be aware that minting a DOI will make your dataset public immediately.

    - Cite the ESRF's address (in the case of an ESRF author) as follows: ESRF, The European Synchrotron, 71 Avenue des Martyrs, CS40220, 38043 Grenoble Cedex 9, France

    - Remember to register your publication in the Joint ESRF/ILL library database. Register directly through this link, or by sending an email with the publication reference to the library

    - Send your author version to the Joint ESRF/ILL Library administrator in the case your publication is not Open Access.

Users are strongly encourage to arrive sufficiently early enough at the ESRF to prepare their samples prior the beginning of the experiment. The ESRF contribution for the four reimbursed users applies for the duration of the X-ray experiment, plus up to three additional days (three days total for offline experiments).

 

At ID22, samples should be sealed in glass capillaries. Capillaries are available at ID22 but if you plan to perform a remote experiment, you are asked to prepare and ship the capillaries.  This is an example of a company selling capillaries:
https://www.capillarytubes.co.uk/acatalog/Borosilicate_Glass_Capillary_Tubes-p1.html

Up to 70 capillaries can be mounted together and individually and automatically installed in the sample stage using a robot.

 

At ID13, it is strongly adviced to prepare samples as thin sections (thickness to be determined based on the transmission of the sample matrix at ~12.82keV). Typically, for paint samples, a thickness of 10um is recommended. A procedure for sample preparation of thin section from existing cross-section is described here. If the sample is fragile and breaks during the sectioning, it is possible to maintain its structure using tape. This tape is particularly recommended for XRD! Tape pieces can be glued to a glass slide for transport to the ESRF and then mounted on appropriate sample holders. The ID21 microtome can be used for preparing thin sections if agreed with ID21 staff in advance.

If it is not possible to prepare thin sections, users analyzing thick cross-sections are encouraged to drill a hole at the back on the sample in the resin block, to minimize X-ray absorption by the embedding resin (see figure). It is also recommend to minimize the lateral size of the resin blocks to mount a maximum of samples together. A Dremell micro-driller is available at the beamline for this purpose.

An alternative to microtoming consists in polishing both sides of the resin block, to reach a thickness of few tens of microns. This procedure has been developed for the analysis of ceramics fragments (Ph. Sciau et al.).

As many samples as possible should be mounted together on ID13 sample holders, that can be found at the beamline, or can be shipped to the users if requested in advance.

Drawings of the ID13 sample holders can be found here: holder 6 holes 8mm, holder 12 holes 5mm and holder 54 holes 2mm.

IMPORTANT POINT FOR MOUNTING SAMPLES FOR ID13:

The maps at ID13 are always recorded with the fast (continuous) motor in horizontal and the slow (step) motor in vertical. It is therefore recommended to mount the stratigraphy such that the layers are vertical (this way, if a map crashes after few lines, at least the entire stratigraphy has already been scanned; see https://www.mdpi.com/article/10.3390/molecules27061997/s1, figure S3, the stratigraphy is vertical).

 

SAMPLE SHIPPING

Samples can be shipped to and from the ESRF, following the ESRF shipping rules. This will be at the charge of the users.

 

Q: Is the BAG limited to painting materials?

A: It is true that most samples are painting fragments (historical and models), but it also includes ceramics, wood, paper samples. The only constraint is that the materials should fit the experimental conditions.

 

Q: If I am partner of the BAG project, can I still submit other ESRF proposals?

A: You can always submit standard proposals, in particular: 1) for beamlines other than ID13 and ID22; 2) also for ID13 or ID22, but only if your proposal requires an experimental set-up that is different from the set-up offered through the BAG. If your proposal aims at running standard BAG measurements, the review panels will probably answer that you should run your experiment via the BAG beamtime.

If you want to submit a standard proposal, you may be interested in the how-to document!

 

Q: I am not a partner of the BAG, but work in the field of heritage and would like to have access to the experimental set-ups available via the BAG. Can I get access to beam time through the Historical Materials BAG?

A: Access to ID22 and ID13 through the BAG is only granted to the listed partners. Interested parties should contact one of the partners to discuss possible collaborative access.

 

Q: How should I prepare my samples?

A: see the specific paragraph above.

 

Q: How can I download my data?

A: Please note that your data will be automatically removed from the visitor server after 3 months. Please find detailed explanations here. Follow STRICTLY the instructions, it will work!

 

Q: How can I analyze data?

A: see the different tutorials.

If you want to participate to an experiment, please inform the BAG coordinators as soon as possible such that they can register you on the A form.

The BAG administrative coordinator takes care of submitting the final A-form but each partner is responsible for his/her participation and samples.

Once you are registered on the A-form, you will receive an email from the user office reminding you to important information.

1. User & Safety Declaration Form - obligatory for completion of your registration on the A Form

2. Safety Training - obligatory for completion of your registration on the A Form

3. Obligatory travel requests for reimbursed users - IMPORTANT no reimbursement will be paid if the procedure is not correctly followed - Please read carefully

4. Declaration and tracking of samples (sample sheets) - updated

5. Site entrance for onsite users; required ID documents

6. WiFi NETWORK at ESRF, ILL, EMBL and common buildings

1. USER & SAFETY DECLARATION FORM

You must now please VALIDATE your electronic and personal "User and Safety Declaration Form" for this experimental session. Please log on here:

https://smis.esrf.fr/misapps/SMISWebClient

Tab "Proposals/Experiments": select "A Form" and click on "To Do"

If you do not remember your password, click on the link above and follow the instructions under "Forgot Password?"

2. SAFETY TRAINING

A validated ESRF Safety Training Course is also mandatory. The course is valid for one year once completed

https://smis.esrf.fr/misapps/SMISWebClient

Tab "Safety" and select:

• "User Safety Training" then "Standard Training": if you are coming to the ESRF

• "User Safety Training" then "Remote access training"; if you are NOT coming to the ESRF but you will participate in the experiment remotely.

• "User Safety Training" then "Mail-in training"; if your experiment is a full service Mail-in experiment (exists for MX and industrial experiments only); this mode requires prior agreement and arrangement with the ESRF staff.

3. OBLIGATORY TRAVEL REQUESTS FOR REIMBURSED USERS

All users who wish to request ESRF financial support for travel MUST complete a personal travel request via the 'SAP Concur' e-travel application. No reimbursement or contribution to expenses will be made for travel that has not been requested via this application.

Travel request (for reimbursed users only): https://eu1.concursolutions.com/nui/signin

(log in with your ESRF_User_Portal_username@esrf.fr and select “Sign in with Concur SSO”, then enter your ESRF_User_Portal_username and ESRF User Portal password;
 e.g. for Gérard Dupont with a User Portal username gdupont1819, log in with gdupont1819@esrf.fr and select “Sign in with Concur SSO”, then enter the username gdupont1819 and the ESRF User Portal password)

This travel request must be submitted as soon as possible to avail of the best offers on travel and prices. The SAP Concur application includes an online booking tool for the reservation of your travel tickets, directly invoiced to the ESRF.

No reimbursement or contribution to travel expenses will be made for travel requests made less than 2 weeks (10 working days) before the arrival date (except in the case of late invitations).

Expense claims for travel must be submitted within 30 days of the return trip via 'SAP Concur' and generated from the associated approved travel request.

Detailed information on our updated travel regulations for users and the 'SAP Concur' application are available here.

4. DECLARATION AND TRACKING OF SAMPLES - SAMPLE SHEETS

Sample sheets are required for all samples that will be brought or sent to the ESRF, for all types of experiments. Please ensure that your team have created and submitted the sample sheets for your proposal and that these are correctly declared on the A Form by the main proposer.

All samples and equipment that will be brought or sent to the ESRF must also be declared in our customised sample tracking systems, to keep track of what is on our site and when:

• ISPyB: for all experiments with proposal number starting with MX, IX or FX

• ICAT: for all other experiments and for equipment (other than small apparatus for MX, IX and FX experiments)

If you are sending samples or equipment to the ESRF, you MUST send them via a recognised courier (FedEx, UPS, DHL, …), NOT via the regular postal service, and you MUST affix the ISPyB/ICAT label and address the parcel to the ESRF Stores.

5. SITE ENTRANCE

Please make sure that your authorisation for site entrance has been validated by the Safety Group (can be checked via the User Portal in tab "Proposals/Experiments", "A Form" >> "View A Form" >> "site entrance OK").This authorisation is mandatory to enter the site.

IDENTITY DOCUMENT TO BE PRESENTED AT THE SITE ENTRANCE

The EPN site is a restricted area: you will be asked to report in at the site entrance on arrival and you will need to produce a proof of identification.

A valid passport or a valid national identity card (i.e. not expired) are the ONLY acceptable form of identification for all those wishing to access the site.

NB: from 1st September 2018, a driver’s licence is no longer accepted as ID for entering the site.

6. WiFi NETWORK at ESRF, ILL, EMBL and common buildings

Two ways to connect:

1. Via the EPN_Visitors network with your User Portal login and password.

2. Via the Eduroam network for users who have a valid account in another Eduroam compliant institution.

WiFi access at IBS: via Eduroam if you have a valid account in another Eduroam compliant institution.

The heritage BAG, proposal HG-172, is a pilot for the new access models implemented thanks to support of the European Union’s Horizon 2020 research and innovation programme under grant agreement No 870313, Streamline.

Jupyter notebooks have been written for the analysis of ID13 XRD maps, thanks to the support of The Photon and Neutron Open Science Cloud (PaNOSC) European project.

The BAG database and FAIR practices are developed thanks to the SHARE OSCARS grant. OSCARS is a four-year EU-funded project (Horizon Europe Research and Innovation programme, grant agreement No. 101129751) that strives to foster the uptake of Open Science in Europe by consolidating the achievements of world-class European research infrastructures in the ESFRI roadmap and beyond into lasting interdisciplinary FAIR data services and working practices. The project aims to strengthen the role of the Science Clusters in the ERA by developing domain-based Competence Centres and by fostering the implementation of Open Science projects funded through a cascading grant mechanism.

 

 

 

The reference publication for the "Historical materials BAG" has been published in Molecules, in open access.

Please refer to it as:

Cotte, M.; Gonzalez, V.; Vanmeert, F.; Monico, L.; Dejoie, C.; Burghammer, M.; Huder, L.; de Nolf, W.; Fisher, S.; Fazlic, I.; Chauffeton, C.; Wallez, G.; Jiménez, N.; Albert-Tortosa, F.; Salvadó, N.; Possenti, E.; Colombo, C.; Ghirardello, M.; Comelli, D.; Avranovich Clerici, E.; Vivani, R.; Romani, A.; Costantino, C.; Janssens, K.; Taniguchi, Y.; McCarthy, J.; Reichert, H.; Susini, J. The “Historical Materials BAG”: A New Facilitated Access to Synchrotron X-ray Diffraction Analyses for Cultural Heritage Materials at the European Synchrotron Radiation Facility. Molecules 2022, 27, 1997. https://doi.org/10.3390/molecules27061997