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1. Thermal Decomposition of Lead White for Radiocarbon Dating of Paintings

Author

Jean-Pascal Dumoulin, Lucile Beck, Frédéric Miserque, Emmanuelle Delqué-Količ, Eddy Foy, Victor Gonzalez, Marion Perron, Céline Bonnot-Diconne, Solène Mussard, Cyrielle Messager, C Moreau, Ingrid Caffy, Stéphanie Coelho, Laboratoire de mesure du carbone 14 (LMC14 - UMS 2572), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Radioprotection et de Sûreté Nucléaire (IRSN)-Ministère de la Culture et de la Communication (MCC)-Centre National de la Recherche Scientifique (CNRS), Laboratoire des Sciences du Climat et de l'Environnement [Gif-sur-Yvette] (LSCE), Institut national des sciences de l'Univers (INSU - CNRS)-Université Paris-Saclay-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université de Versailles Saint-Quentin-en-Yvelines (UVSQ), Delft University of Technology, Delft University of Technology (TU Delft), Laboratoire Archéomatériaux et Prévision de l'Altération (LAPA - UMR 3685), Nanosciences et Innovation pour les Matériaux, la Biomédecine et l'Energie (ex SIS2M) (NIMBE UMR 3685), Institut Rayonnement Matière de Saclay (IRAMIS), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Institut Rayonnement Matière de Saclay (IRAMIS), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC), IRAMAT - Laboratoire Métallurgies et Cultures (IRAMAT - LMC), Institut de Recherches sur les Archéomatériaux (IRAMAT), Université d'Orléans (UO)-Centre National de la Recherche Scientifique (CNRS)-Université Bordeaux Montaigne-Université de Technologie de Belfort-Montbeliard (UTBM)-Université d'Orléans (UO)-Centre National de la Recherche Scientifique (CNRS)-Université Bordeaux Montaigne-Université de Technologie de Belfort-Montbeliard (UTBM), Laboratoire d'Etude de la Corrosion Aqueuse (LECA), Service de la Corrosion et du Comportement des Matériaux dans leur Environnement (SCCME), Département de Physico-Chimie (DPC), CEA-Direction des Energies (ex-Direction de l'Energie Nucléaire) (CEA-DES (ex-DEN)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-CEA-Direction des Energies (ex-Direction de l'Energie Nucléaire) (CEA-DES (ex-DEN)), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Département de Physico-Chimie (DPC), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay, Centre de Conservation et de Restauration du Cuir (2CRC), Université de Versailles Saint-Quentin-en-Yvelines (UVSQ)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut national des sciences de l'Univers (INSU - CNRS)-Université Paris-Saclay-Centre National de la Recherche Scientifique (CNRS), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Institut Rayonnement Matière de Saclay (IRAMIS), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université Paris-Saclay-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), and Université de Technologie de Belfort-Montbeliard (UTBM)-Université d'Orléans (UO)-Université Bordeaux Montaigne (UBM)-Centre National de la Recherche Scientifique (CNRS)-Université de Technologie de Belfort-Montbeliard (UTBM)-Université d'Orléans (UO)-Université Bordeaux Montaigne (UBM)-Centre National de la Recherche Scientifique (CNRS)

Subjects
010506 paleontology, Archeology, Materials science, Mineralogy, 02 engineering and technology, 01 natural sciences, law.invention, chemistry.chemical_compound, Lead (geology), law, Organic matter, Radiocarbon dating, thermal decomposition, 0105 earth and related environmental sciences, chemistry.chemical_classification, Calcite, White (horse), radiocarbon dating, Extender, Thermal decomposition, lead white painting, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, Decomposition, chemistry, cerussite, gilt leather, General Earth and Planetary Sciences, 0210 nano-technology
Abstract

Lead carbonates were used as cosmetic and pigment since Antiquity. The pigment, known as lead white, was generally composed of cerussite and hydrocerussite. Unlike most ancient pigments, lead white was obtained by a synthetic route involving metallic lead, vinegar and organic matter. Fermentation of organic matter produces heat and CO2 emission, leading to the formation of carbonates. As lead white is formed by trapping CO2, radiocarbon (14C) dating can thus be considered. We have developed a protocol to prepare lead white. We selected modern pigments for the experiment implementation and ancient cosmetic and paintings for dating. After characterization of the samples by XRD, thermal decomposition of cerussite at various temperatures was explored in order to select the appropriate conditions for painting samples. CO2 extraction yield, SEM and XPS were used to characterize the process. Thermal decomposition at 400°C was successfully applied to mixtures of lead white with other paint components (oil as binder, calcite as filler/extender) and to historical samples. We obtained radiocarbon measurements in agreement with the expected dates, demonstrating that thermal decomposition at 400°C is efficient for a selective decomposition of lead white and that paintings can be directly 14C-dated by dating lead white pigment.

Published
2019

2. ARTEMIS, te 14C AMS facility of the LMC14 national laboratory: A status report on quality control and microsample procedures

Author

Cyrielle Messager, Bernard Berthier, B Thellier, Valérie Setti, Jean-Pascal Dumoulin, Marc Sieudat, Emmanuelle Delqué-Količ, Lucile Beck, Stéphane Hain, Marion Perron, Ingrid Caffy, Solène Mussard, C Moreau, Laboratoire de mesure du carbone 14 (LMC14 - UMS 2572), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Radioprotection et de Sûreté Nucléaire (IRSN)-Ministère de la Culture et de la Communication (MCC)-Centre National de la Recherche Scientifique (CNRS), Laboratoire des Sciences du Climat et de l'Environnement [Gif-sur-Yvette] (LSCE), Institut national des sciences de l'Univers (INSU - CNRS)-Université Paris-Saclay-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université de Versailles Saint-Quentin-en-Yvelines (UVSQ), and Université de Versailles Saint-Quentin-en-Yvelines (UVSQ)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut national des sciences de l'Univers (INSU - CNRS)-Université Paris-Saclay-Centre National de la Recherche Scientifique (CNRS)

Subjects
[SDU.OCEAN]Sciences of the Universe [physics]/Ocean, Atmosphere, 010506 paleontology, Archeology, 060102 archaeology, Database, media_common.quotation_subject, Quality control, Sample (statistics), 06 humanities and the arts, computer.software_genre, Status report, 01 natural sciences, General Earth and Planetary Sciences, Environmental science, 0601 history and archaeology, Quality (business), National laboratory, Routine analysis, [SDU.ENVI]Sciences of the Universe [physics]/Continental interfaces, environment, computer, 0105 earth and related environmental sciences, media_common
Abstract

Quality control procedures have been developed at the Laboratoire de Mesure du Carbone 14 (LMC14) national laboratory throughout the years of operation. Routine procedures are applied to sample preparation depending on their composition and their size. The tuning of the ARTEMIS AMS facility, hosted by the LMC14 laboratory, uses an accurate procedure. A batch of unknown samples is measured with accompanying samples (primary and secondary standards and blanks), which give a powerful set of data to control the quality of each measurement. A homemade database has been created to store the sample information and study the evolution of the accompanying samples. The LMC14 laboratory participated in the Sixth International Radiocarbon Intercomparison, SIRI. The results are presented here, with statistical tests to assess the quality of the preparations and measurements done at the LMC14 national laboratory. To obtain a reliable radiocarbon (14C) age by AMS, 1 mg of sample is required in routine analysis. Recently, the LMC14 developed a new procedure dedicated to microsamples, allowing the size of samples to be reduced and contributing to opening 14C dating to materials that were previously unreachable. This new procedure has been successfully tested on valuable Cultural Heritage samples: lead white mural paintings.

Published
2020

3. Thermal analysis of carbonate pigments and linseed oil to optimize CO2 extraction for radiocarbon dating of lead white paintings

Author

Cyrielle Messager, Laurence de Viguerie, Lucile Beck, Maguy Jaber, Laboratoire des Sciences du Climat et de l'Environnement [Gif-sur-Yvette] (LSCE), Institut national des sciences de l'Univers (INSU - CNRS)-Université Paris-Saclay-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université de Versailles Saint-Quentin-en-Yvelines (UVSQ), Laboratoire de mesure du carbone 14 (LMC14 - UMS 2572), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Radioprotection et de Sûreté Nucléaire (IRSN)-Ministère de la Culture et de la Communication (MCC)-Centre National de la Recherche Scientifique (CNRS), Laboratoire d'Archéologie Moléculaire et Structurale (LAMS), Institut de Chimie du CNRS (INC)-Sorbonne Université (SU)-Centre National de la Recherche Scientifique (CNRS), Université de Versailles Saint-Quentin-en-Yvelines (UVSQ)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut national des sciences de l'Univers (INSU - CNRS)-Université Paris-Saclay-Centre National de la Recherche Scientifique (CNRS), and Université Pierre et Marie Curie - Paris 6 (UPMC)-Institut de Chimie du CNRS (INC)-Sorbonne Université (SU)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Thermogravimetric analysis, food.ingredient, chemistry.chemical_element, Mineralogy, 02 engineering and technology, 01 natural sciences, Analytical Chemistry, law.invention, chemistry.chemical_compound, food, Linseed oil, law, Radiocarbon dating, [SDU.ENVI]Sciences of the Universe [physics]/Continental interfaces, environment, Spectroscopy, [SDU.OCEAN]Sciences of the Universe [physics]/Ocean, Atmosphere, 010401 analytical chemistry, Lead carbonate, Extraction (chemistry), 021001 nanoscience & nanotechnology, humanities, 0104 chemical sciences, Calcium carbonate, chemistry, Carbonate, Environmental science, 0210 nano-technology, Carbon
Abstract

International audience; Lead white was a white pigment extensively used in paintings from Antiquity until the beginning of the 20th century. It is composed of hydrocerussite (Pb3(CO3)2(OH)2) and cerussite (PbCO3). Historical recipes report metallic lead, vinegar and horse manure as ingredients to produce the two lead carbonates. The incorporation of organic CO2 carrying 14C representative of the time of manufacture of lead white allows radiocarbon dating of this pigment. One possible protocol for lead white paint preparation for dating is based on the extraction of carbon from lead carbonates by thermal decomposition. Since lead white paints are mixed with a binder and other pigments, a thermogravimetric study was implemented to study CO2 extraction from each component. The measurements were carried out on samples of modern paints prepared with lead white (lead carbonate), Meudon white (calcium carbonate) and linseed oil. The results show that it is possible to separate the carbon of interest (carrying the 14C signature: lead white and linseed oil) from the dead carbon coming from geological carbonates (containing no radiocarbon: Meudon white) by heating the paint sample at 400 °C. This study provides a better understanding of the thermal behavior of these three paint constituents and confirms the validity of the thermal protocol for the preparation of lead white paints for radiocarbon dating.

Published
2020

4. Unexpected presence of 14C in inorganic pigment for an absolute dating of paintings

Author

Jean-Pascal Dumoulin, Cyrielle Messager, Emmanuelle Delqué-Količ, C Moreau, Marion Perron, Christian Degrigny, Lucile Beck, Vincent Serneels, Ingrid Caffy, Laboratoire des Sciences du Climat et de l'Environnement [Gif-sur-Yvette] (LSCE), Institut national des sciences de l'Univers (INSU - CNRS)-Université Paris-Saclay-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université de Versailles Saint-Quentin-en-Yvelines (UVSQ), Laboratoire de mesure du carbone 14 (LMC14 - UMS 2572), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Radioprotection et de Sûreté Nucléaire (IRSN)-Ministère de la Culture et de la Communication (MCC)-Centre National de la Recherche Scientifique (CNRS), Haute Ecole Spécialisée de Suisse Occidentale (HES-SO), Department of Geosciences - Earth Sciences [Fribourg], University of Fribourg, Université de Versailles Saint-Quentin-en-Yvelines (UVSQ)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut national des sciences de l'Univers (INSU - CNRS)-Université Paris-Saclay-Centre National de la Recherche Scientifique (CNRS), and Université de Fribourg = University of Fribourg (UNIFR)

Subjects
0301 basic medicine, 010506 paleontology, media_common.quotation_subject, [SDV]Life Sciences [q-bio], lcsh:Medicine, Art history, Mural, 01 natural sciences, Natural (archaeology), law.invention, 03 medical and health sciences, Absolute dating, law, Inorganic pigments, Radiocarbon dating, lcsh:Science, 0105 earth and related environmental sciences, media_common, Painting, Multidisciplinary, White (horse), lcsh:R, Art, Scientific technique, 030104 developmental biology, lcsh:Q
Abstract

The absolute dating of paintings is crucial for tackling the problem of fake art. Investigations to authenticate paintings rely on an advanced knowledge of art history and a collection of scientific techniques. Radiocarbon dating is the only technique that gives access to an absolute time scale, but its application is limited to organic materials such as wood, canvas or natural binder. Extending absolute dating to inorganic pigments would make it possible to overcome the lack of available materials for dating easel and mural paintings. Here, we present a novel technique permitting paintings that contain inorganic pigment to be radiocarbon dated. We report results obtained on lead white that was the major white pigment used from Antiquity to the 20th century. We demonstrate that its manufacture is the key point for an absolute and reliable dating. We report an unprecedented use of 14C to date 14th to 16th century wall paintings. Since lead white was extensively used by the greatest artists, we anticipate that this study will open new avenues for detecting forgeries on the art market and for museums.

Published
2020

5. Unexpected presence of

Author

Lucile, Beck, Cyrielle, Messager, Ingrid, Caffy, Emmanuelle, Delqué-Količ, Marion, Perron, Jean-Pascal, Dumoulin, Christophe, Moreau, Christian, Degrigny, and Vincent, Serneels

Subjects
Chemistry, Mass spectrometry, Archaeology, Article
Abstract

The absolute dating of paintings is crucial for tackling the problem of fake art. Investigations to authenticate paintings rely on an advanced knowledge of art history and a collection of scientific techniques. Radiocarbon dating is the only technique that gives access to an absolute time scale, but its application is limited to organic materials such as wood, canvas or natural binder. Extending absolute dating to inorganic pigments would make it possible to overcome the lack of available materials for dating easel and mural paintings. Here, we present a novel technique permitting paintings that contain inorganic pigment to be radiocarbon dated. We report results obtained on lead white that was the major white pigment used from Antiquity to the 20th century. We demonstrate that its manufacture is the key point for an absolute and reliable dating. We report an unprecedented use of 14C to date 14th to 16th century wall paintings. Since lead white was extensively used by the greatest artists, we anticipate that this study will open new avenues for detecting forgeries on the art market and for museums.

Published
2019

6. Comparison of Two Bone-Preparation Methods for Radiocarbon Dating: Modified Longin and Ninhydrin

Author

Ingrid Caffy, Emmanuelle Delqué-Količ, C Moreau, Lucile Beck, J. P. Dumoulin, Matthieu Lebon, Hélène Valladas, Cyrielle Messager, Laboratoire de mesure du carbone 14 (LMC14 - UMS 2572), Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut de Radioprotection et de Sûreté Nucléaire (IRSN)-Ministère de la Culture et de la Communication (MCC)-Centre National de la Recherche Scientifique (CNRS), Laboratoire des Sciences du Climat et de l'Environnement [Gif-sur-Yvette] (LSCE), Institut national des sciences de l'Univers (INSU - CNRS)-Université Paris-Saclay-Centre National de la Recherche Scientifique (CNRS)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Université de Versailles Saint-Quentin-en-Yvelines (UVSQ), and Université de Versailles Saint-Quentin-en-Yvelines (UVSQ)-Commissariat à l'énergie atomique et aux énergies alternatives (CEA)-Institut national des sciences de l'Univers (INSU - CNRS)-Université Paris-Saclay-Centre National de la Recherche Scientifique (CNRS)

Subjects
[SDU.OCEAN]Sciences of the Universe [physics]/Ocean, Atmosphere, 010506 paleontology, Archeology, Chromatography, 060102 archaeology, Chemistry, 06 humanities and the arts, 01 natural sciences, Preparation method, chemistry.chemical_compound, Elemental analysis, Ninhydrin, General Earth and Planetary Sciences, 0601 history and archaeology, [SDU.ENVI]Sciences of the Universe [physics]/Continental interfaces, environment, 0105 earth and related environmental sciences
Abstract

In this paper, first results comparing modified Longin and ninhydrin collagen extraction methodologies are presented. The goal of this study is to investigate the bones of several species with different ages, preservation conditions, and collagen contents to determine the most suitable preparation method. Different types of samples are used such as VIRI samples, previously dated bones, and background samples. Each bone has undergone elemental analysis, infrared analysis, and 14C measurement. The results are presented and the advantages and disadvantages of each preparation method are discussed. In general, results obtained by the two methods are in accordance with the consensus value for 2σ uncertainty. For VIRI I and a mammoth bone, the ninhydrin preparation gives, respectively, 8450±70 BP and 14,870±60 BP whereas the modified Longin process gives 8365±45 BP and 14,750±100 BP in agreement with the expected values. From the experimental point of view, the modified Longin process is easier to implement than the ninhydrin protocol. From this approach, we can conclude that the modified Longin process could be preferred in most cases and particularly when the amount of bone is small and the sample is not too contaminated.

Published
2017

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