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Social Sciences & Humanities Open Marketplace

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Description of the object/monument identity: The title and a short description and context/known history of the artwork/monument are included. Additional information on the artwork can be also included or linked such as inventory number, photograph(s) and physical dimensions. Location of the Site / Museum: Location of the permanent position/storage of the artwork/monument Owner of the object / Scholar - keeper: Information about the owner or the keeper or scholar owing permission for analysis. Date/period: Information about the date or period that the artwork/monument was created/constructed including information about the creator. Type of object: Information about the type of the object such as polychromy on sculpture, panel painting etc. Type of material(s) for examination: Type(s) of materials for examination. e.g. substrate, coatings, pigments or other materials related to surface finishing decoration.

Framework, analytical context (motivation - aim of the analytical campaign); Short presentation of the main objectives of the analysis of the artworks/monument Preliminary analysis: Information about any preliminary visual examination and analysis of the artwork using other techniques such as photography, multispectral imaging, XRF, LIBS etc. The prelimenary analysis provides information on the condition and the characteristics of the artwork useful for an effective planning and appropriate selection of measurement points for Raman analysis. Possible source of error: wrong selection of measurement position, relating to previous measurements as LIBS (if ignored or not well-documented) Known conservation history / archives / oral communication: Research in digital resources, archives and even oral communication with experts concerning information of past analytical data or conservation interventions Possible source of error: possible interference of (aged) conservation materials

Scope: (scientific analysis? Archaelogical excavation? conservation in course? Demonstration? Promotion? Service?) Analysis expected outcome: Identification of inorganic compounds through elemental analysis. Skills requirements (level of training of the operator): Scientist specialised in XRF Spectroscopy

Bearing in mind the high penetrating power of X-Rays, Choose carefully the support/check also the back of the artwork to avoid interferences. Determine and mark carefully the security restricted area and define the set-up geometry (X-ray beam direction) for safety of the operators and public.

The equipment specifications of the instrument and the overall apparatus are documented such as type of equipment, manufacturing company, anode (Rh, Ro, Ag, Au, W etc.), XRF tube operational range parameters (Voltage, Current, acquisition time), optical system (camera) /objective lens used and any other component used.

The measurement conditions are documented and stored. In particular, the measurement distance from the object (contact / short / long / remote), the spot size (dimensions of the analysed area) and the measurment resolution/accuracy

Use (or Acquire) high resolution images of the entire object and of the details under study as references. Τhe detailed reference images will be used to document the ROIs of analysis.

A protocol for safe application (for the user and the object damage protection) is necessary to ensure safe operating procedures to avoid human exposure to X-ray radiation

Select the sites of analysis. The point of analysis (3 to 5 mm diameter) has to be optically flat to inhibit diffuse reflection. Acquire high resolution detailed reference images of the entire object or of the part under study (in case of a monument). Use the detailed reference images to document the points of analysis. Possible source of error: Diffuse reflection results from a combined process including reflection, refraction and diffraction of the incident radiation due to interactions with particles of the sample. Diffuse reflection spectra appear to be similar to transmission spectra derived from poorly prepared KBr disks.

The instrument head must access the point of analysis, taking into account that the working distance must be optimized checking the signal amplitude. A tentative spectrum is obtained on the specimen / area under examination acquiring the number of scans that seems appropriate. The scans may be increased according to the final output. Depending on surface morphology and composition, it may be necessary to optimize the acquisition parameters to improve the spectral profile.

Record data taken on representative sites on the CH object. A preliminary evaluation of the spectrum is relevant (assessement of major, minor elements present) Store data and metadata files The measurment conditions (Voltage, current, acquisition time, any filter used) are documented in a text file for all the measurements or in form of metadata file for each spectrum file.

Assess the spectra and assign the peaks to major, minor or trace elements

Interpret the detected elements for the characterisation of materials

Organize data and metadata in standard format for open access repositories. The metadata should incorporate descriptions of the equipment, instrumental setup and measurement conditions and information related to the artwork/monument. Finally, the (meta)data should follow the FAIR principles.

Prepare a document that includes the objectives of the project/study, information on the artwork, technical /exprimental information, selection of representative data obtained, results and conclusions on the overall work.

Publish the results according to the licencing/IPR / reuse restrictions

Laura Cartechini

X-ray fluorescence spectroscopy is a well-established method for the in situ investigation of archaeological objects and artworks through the characterization of the chemical (elemental) composition of materials. The fact that the method is essentially non-destructive makes it particularly attractive and widely used by heritage scientists, art historians, archaeologists, curators and conservators. The benefits of XRF include fast analysis, applicability to any type of object or composite material of various shapes and dimensions, suitability for the detection of major to trace elements and semi quantitative capabilities.

In situ X-Ray fluorescence analysis for the characterisation of materials on cultural heritage objects

Media

Workflow steps(16)

1 Describe the artwork

2 Describe the project

3 Describe the method - Use (scope)

4 Describe the method. Operational environmental and safety conditions for the measurement

5 Describe the method - Equipment specifications

6 Describe the method. Measurement range, spot size and spatial resolution/ accuracy

7 Describe the method. Reference image (scale / multiscale / map / 2D / 3D)

8 Describe the measurement: Pre-processing/ safe limits

9 Describe the measurement. Pre-processing / selection and annotation of measurement sites on reference images

10 Describe measurement. Pre-processing / preliminary tests - Measurement setup

11 Describe measurement. Measurement / Spectra acquisition / Storage of data and metadata files

12 Post-process and interpret data. Peak / spectral bands assessment

13 Post-process and interpret data. Material identification/peak assignment

14 Disseminate the results. Data and metadata storage, publication and sharing

15 Disseminate the results. Prepare report

16 Disseminate the results. Publish the results