Slide 1: Analysis of non-infinite samples in Cultural Heritage
BRUKER NANO ANALYTICS' CULTURAL HERITAGE WEBINAR SERIES 2023 Analysis of non-infinite samples in Cultural Heritage Micro-XRF Applications Team Bruker Nano Analytics Innovation with Integrity
Slide 2: Art & Conservation Webinar Series: Questions
BRU KE R N AN O AN ALYTICS ' CU LTU RAL H ERITAG E W EBIN AR SERIES 2 0 2 3 Art & Conservation Webinar Series Analysis of non-infinite samples in Cultural Heritage If you have questions during this webinar, please type your questions, thoughts, or comments in the Q&A box and press Send. We ask for y
Slide 3: Which topics would you like in upcoming webinars?
BRU KE R N AN O AN ALYTICS ' CU LTU RAL H ERITAG E W EBIN AR SERIES 2 0 2 3 Art & Conservation Webinar Series Analysis of non-infinite samples in Cultural Heritage There are many topics involving XRF in Cultural Heritage! We are interested to know which topic(s) you would like to learn more about in
Slide 4: The Speakers
BRU KE R N AN O AN ALYTICS ' CU LTU RAL H ERITAG E W EBIN AR SERIES 2 0 2 3 The Speakers Dr. Roald Tagle Mareike Gerken M.A. Head of XMP Application, Application Scientist XMP specialized in Bruker Nano Analytics, Berlin, Germany Cultural Heritage Bruker Nano Analytics, Berlin, Germany © 2023 Br
Slide 5: Overview
BRU KE R N AN O AN ALYTICS ' CU LTU RAL H ERITAG E W EBIN AR SERIES 2 0 2 3 Overview This webinar focuses on quantitative XRF analysis of non-infinite samples. If you want to know more about quantification of Cultural Heritage related materials subscribe for the on-demand webinar session from Oc
Slide 6: Recapitulating Quantification by means of XRF in Heritage Science
BRUKER NANO ANALYTICS' CULTURAL HERITAGE WEBINAR SERIES 2023 Recapitulating “Quantification by means of XRF in Heritage Science”
Slide 7: Quantitative X-ray fluorescence analysis: A complex matter
BRU KE R N AN O AN ALYTICS ' CU LTU RAL H ERITAG E W EBIN AR SERIES 2 0 2 3 Quantitative X-ray fluorescence analysis A complex matter… “Physics unveils possibilities, Sample technology harnesses potentials, Limits of Preparation Detection while the synergy between the sample and the analytical query
Slide 8: Understanding your sample from the XRF point of view
BRU KE R N AN O AN ALYTICS ' CU LTU RAL H ERITAG E W EBIN AR SERIES 2 0 2 3 Quantitative X-ray fluorescence analysis Understanding your sample… from the XRF point of view Each material has its own intrinsic structure and composition that impacts not only the analysis itself but also its outcomes. Li
Slide 9: Quantification: With standards or without?
BRU KE R N AN O AN ALYTICS ' CU LTU RAL H ERITAG E W EBIN AR SERIES 2 0 2 3 Quantification …With standards or without? Ideally, for a Quantification the samples are: ? Homogeneous If this IS the case, standard-less or reference material-free (FP) methods are well suitable with possibilities to inc
Slide 10: Quantification: With standards or without?
BRU KE R N AN O AN ALYTICS ' CU LTU RAL H ERITAG E W EBIN AR SERIES 2 0 2 3 Quantification …With standards or without? Ideally, for a Quantification the samples are: ? Homogeneous If this IS the case, standard-less or reference material-free (FP methods) are well suitable with possibilities to inc
Slide 11: Non-infinite samples in Cultural Heritage: An overview
BRU KE R N AN O AN ALYTICS ' CU LTU RAL H ERITAG E W EBIN AR SERIES 2 0 2 3 Non-infinite samples in Cultural Heritage An overview What types of materials Which research questions are we talking about? can be answered using XRF? Gildings Provenance (origin and dating) Alloys Composition Cor
Slide 12: Measuring gildings
BRUKER NANO ANALYTICS' CULTURAL HERITAGE WEBINAR SERIES 2023 Measuring gildings
Slide 13: Studying gildings: An introduction to the art-technology
BRU KE R N AN O AN ALYTICS ' CU LTU RAL H ERITAG E W EBIN AR SERIES 2 0 2 3 Studying gildings An introduction to… the art-technology Historically, different gilding techniques have been used: Water/ poliment gilding: gold leaf applied on a layer of bole that covers a gesso ground and afterwards bu
Slide 14: Studying gildings: ongoing research
BRU KE R N AN O AN ALYTICS ' CU LTU RAL H ERITAG E W EBIN AR SERIES 2 0 2 3 Studying gildings An introduction to… ongoing research What can we learn from spatial resolved micro-XRF analysis? Information Research question Application technique Attribution Application quality Skill level Size of gold
Slide 15: Studying gildings: ongoing research
BRU KE R N AN O AN ALYTICS ' CU LTU RAL H ERITAG E W EBIN AR SERIES 2 0 2 3 Studying gildings An introduction to… ongoing research A historical overview about analytical approaches to determine the leave thickness Invasive approaches SEM/EDX on cross-section samples. doi.org/10.1111/arcm.12287 Non
Slide 16: Studying gildings: Non-infinity of gold leaves
BRU KE R N AN O AN ALYTICS ' CU LTU RAL H ERITAG E W EBIN AR SERIES 2 0 2 3 Studying gildings Non-infinity of gold leaves Looking at the Au-Lα distribution of a gilded surface, intensity differences are clearly notable between areas covered with a single gold layer or overlapping leaves. The common
Slide 17: Non-infinity of gold leaves: Using reference materials
BRU KE R N AN O AN ALYTICS ' CU LTU RAL H ERITAG E W EBIN AR SERIES 2 0 2 3 Studying gildings Non-infinity of gold leaves: Using reference materials Thin gold foils were measured on top of the prepared priming and bole to simulate the same background: The plot of net intensity (cps) vs. gold layer
Slide 18: Non-infinity of gold leaves: Using reference materials
BRU KE R N AN O AN ALYTICS ' CU LTU RAL H ERITAG E W EBIN AR SERIES 2 0 2 3 Studying gildings Non-infinity of gold leaves: Using reference materials Thin gold foils were measured on top of the prepared priming and bole to simulate the same background: The plot of net intensity (cps) vs. gold layer
Slide 19: Measuring gold leaf thickness: Standard addition method
BRU KE R N AN O AN ALYTICS ' CU LTU RAL H ERITAG E W EBIN AR SERIES 2 0 2 3 Measuring gold leaf thickness Standard addition method ? Standard addition method 62 52 y = 10x + 10 R² = 1 Parameter 1 (Intensity in cps) 42 32 22 Thickness of analyte 12 Sample intensity 2 -2 -1 0 1 2 3 4 5 Standard (Layer
Slide 20: Measuring gold leaf thickness: Standard addition method
BRU KE R N AN O AN ALYTICS ' CU LTU RAL H ERITAG E W EBIN AR SERIES 2 0 2 3 Measuring gold leaf thickness Standard addition method Gilding: Standard addition method 30000 154 nm 25000 Au net intensity (cps) 20000 53 nm Standard with two foils positioned on 15000 y = 95,55x + 12.706,98 R² = 1,00 top
Slide 21: Compositional analysis of iron gall inks
BRUKER NANO ANALYTICS' CULTURAL HERITAGE WEBINAR SERIES 2023 Compositional analysis of iron gall inks
Slide 22: Studying iron gall inks
BRU KE R N AN O AN ALYTICS ' CU LTU RAL H ERITAG E W EBIN AR SERIES 2 0 2 3 Studying iron gall inks An introduction to… the art-technology and ongoing research Iron gall inks have been used already in the antique and until late 20th century. It is one of, if not THE most important writing material
Slide 23: The need for reference materials
BRU KE R N AN O AN ALYTICS ' CU LTU RAL H ERITAG E W EBIN AR SERIES 2 0 2 3 The need for reference materials An introduction to the methodological approach Why do we need reference materials and what do they offer? Studying non-infinitely thick samples, the direct approach of FP quantification requi
Slide 24: Creating reference materials for inks: The Methodology
BRU KE R N AN O AN ALYTICS ' CU LTU RAL H ERITAG E W EBIN AR SERIES 2 0 2 3 Creating reference materials for inks Counting atoms: The Methodology Final specimen test single element Production process (for iron on glass substrate and filter paper) A defined amount of different chemical elements sol
Slide 25: Creating reference materials for inks: The specimen
BRU KE R N AN O AN ALYTICS ' CU LTU RAL H ERITAG E W EBIN AR SERIES 2 0 2 3 Creating reference materials for inks Counting atoms: The specimen The micro-XRF elemental distribution of Fe clearly indicates that the intensity increases with the amount of material present. However, also inhomogeneitie
Slide 26: Creating reference materials for inks: Ensuring accuracy
BRU KE R N AN O AN ALYTICS ' CU LTU RAL H ERITAG E W EBIN AR SERIES 2 0 2 3 Creating reference materials for inks Counting atoms: Ensuring accuracy The variation of material deposit over the specimen can be studied using line scans, that show the Fe accumulation on the edges of the paper. The more
Slide 27: Counting atoms: Calculating the mass deposit
BRU KE R N AN O AN ALYTICS ' CU LTU RAL H ERITAG E W EBIN AR SERIES 2 0 2 3 Creating reference materials for inks Counting atoms: Calculating the mass deposit Again, now the net counts of Fe are extracted but now Specimen ng/mm2 ± s% A2 63 1.4 2.3 only from the homogeneous center of the references
Slide 28: Counting atoms and improving the method
BRU KE R N AN O AN ALYTICS ' CU LTU RAL H ERITAG E W EBIN AR SERIES 2 0 2 3 Creating reference materials for inks Counting atoms and improving the method The reference material is in principle similar to the Alternatively, can we use again the previously one used for the gold leaves thickness desc
Slide 29: Counting atoms and improving the method
BRU KE R N AN O AN ALYTICS ' CU LTU RAL H ERITAG E W EBIN AR SERIES 2 0 2 3 Creating reference materials for inks Counting atoms and improving the method The samples were analyzed following the same Mn procedure, but this time located on a PE cap resting Fe on a mylar foil to reduce scattering.
Slide 30: Counting atoms and improving the method
BRU KE R N AN O AN ALYTICS ' CU LTU RAL H ERITAG E W EBIN AR SERIES 2 0 2 3 Creating reference materials for inks Counting atoms and improving the method Reference location: Four points were measured on the The results allow to determine the mass of each object with and without the references and
Slide 31: Counting atoms and improving the method
BRU KE R N AN O AN ALYTICS ' CU LTU RAL H ERITAG E W EBIN AR SERIES 2 0 2 3 Creating reference materials for inks Counting atoms and improving the method Using the results from the correlation and knowing Conversion factor from arbitrary units to ng/mm² that the Blank is not 0 ng/mm², we can determi
Slide 32: Applying the method to a sample
BRU KE R N AN O AN ALYTICS ' CU LTU RAL H ERITAG E W EBIN AR SERIES 2 0 2 3 Finally, applying the method to a sample From counting atoms to determining mass deposition on paper Point measurements of the iron gall ink references. Point measurements of the blank paper. Iron gall ink mock-ups with vary
Slide 33: Iron gall ink mock-ups: Comparing the blank to the reference location
BRU KE R N AN O AN ALYTICS ' CU LTU RAL H ERITAG E W EBIN AR SERIES 2 0 2 3 Finally, applying the method to a sample From counting atoms to determining mass deposition on paper Chemical element Mn Fe Cu Zn Conversion factors 176 166 102 132 ng/mm2 Mn Fe Cu Zn Comparing the blank to the Blank_1 7.0 1
Slide 34: Applying the method to a sample: mass deposition
BRU KE R N AN O AN ALYTICS ' CU LTU RAL H ERITAG E W EBIN AR SERIES 2 0 2 3 Finally, applying the method to a sample From counting atoms to determining mass deposition on paper ng/mm2 Mn Fe Cu Zn VO_1 0 517 0 0 VO_2 0 434 58 0 VO_3 0 371 102 0 VO_4 0 367 148 0 VO_5 0 293 50 0 VO_6 0 240 39 24 VO_7 0
Slide 35: Conclusion
BRU KE R N AN O AN ALYTICS ' CU LTU RAL H ERITAG E W EBIN AR SERIES 2 0 2 3 Analysis of non-infinite samples in Cultural Heritage Conclusion Non-infinity does not prevent you from quantifying your sample! Standard-based XRF analysis offers a quick and reliable workflow to determine the coating thi
Slide 36: Questions and survey on upcoming webinar topics
BRU KE R N AN O AN ALYTICS ' CU LTU RAL H ERITAG E W EBIN AR SERIES 2 0 2 3 Art & Conservation Webinar Series Analysis of non-infinite samples in Cultural Heritage If you have questions during this webinar, please type your questions, thoughts, or comments in the Q&A box and press Send. We ask for y
Slide 37: Info.bna@bruker.com www.bruker.com/bna
Info.bna@bruker.com www.bruker.com/bna
Slide 38: Paper transmission
Paper transmission XRF Check - XRF Check (bruker.com) © 2023 Bruker | | - confidential -
Slide 39: Paper transmission
Paper transmission Minor effects for the filter Significant paper effects for Ca © 2023 Bruker | | - confidential -
Slide 40: Filter peak to background and secondary excitation from the glass
Filter Peak to background and secondary excitation from the glass Secondary excitation from Secondary bremsstrahlung excitation from scattering bremsstrahlung scattering With filter No filter © 2023 Bruker | | - confidential -
Slide 41: Secondary excitation from the glass
Secondary excitation from the glass Net intensity [cps] Spectrum Mn Fe Cu Zn ----------------------------------------------------------------------------- Paper on mylar no filter 1846.64 10908.62 2212.98 1908.02 Paper on glass no filter 1655.9 9873.29 2011.15 1789.18 live time Mn Fe Cu Zn 39 72019