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Author |
Odin, G.P.; Belhadj, O.; Vanmeert, F.; Janssens, K.; Wattiaux, A.; Francois, A.; Rouchon, V. |
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Title |
Study of the influence of water and oxygen on the morphology and chemistry of pyritized lignite: Implications for the development of a preventive drying protocol |
Type |
A1 Journal article |
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Year  |
2020 |
Publication |
Journal Of Cultural Heritage |
Abbreviated Journal |
J Cult Herit |
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Volume |
42 |
Issue |
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Pages |
117-130 |
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Keywords |
A1 Journal article; Art; History; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation) |
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Abstract |
Lignite constitutes a unique testimony of past diversity and evolution of land plants. This material, usually waterlogged, is particularly difficult to dry because of its mechanical sensitivity to moisture changes. In addition, lignite may contain organic and inorganic sulfides, which are susceptible to oxidation once excavated. As a result, the conservation of lignite is particularly complicated and lignite remains scarce in paleobotanical collections. We experimentally test different drying protocols on waterlogged pyritized lignite, while documenting the respective role of water and oxygen on their morphology and chemistry. The results reveal that inorganic sulfides (pyrite) are more prone to oxidation than organic sulfides (thioethers). Critically, water is the main factor responsible for this oxidation, provoking sulfate efflorescence when samples are further exposed to oxygen. On the other hand, an abrupt removal of water provokes significant mechanical damage while sulfur remains mostly present as reduced compounds. The control of water and oxygen exchanges is thus critical for conserving lignite without physical damage and efflorescence. We successfully achieved this by storing the samples in hermetically sealed plastic bags made of semi-permeable films, which slowly release humidity while allowing a gradual influx of oxygen. We advise curators to quickly handle lignite once removed from its waterlogged environment because of the fast kinetics of oxidation, and to choose a drying protocol according to the purpose of the lignite treated. Finally, once dried, we advise to store the lignite in an anhydrous environment. (C) 2019 Elsevier Masson SAS. All rights reserved. |
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Wos |
000525864000013 |
Publication Date |
2019-09-07 |
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Abbreviated Series Title |
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Series Volume |
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Series Issue |
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Edition |
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ISSN |
1296-2074 |
ISBN |
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Additional Links |
UA library record; WoS full record |
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Impact Factor |
3.1 |
Times cited |
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Open Access |
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Notes |
; This research was funded by a doctoral school grant from the Museum National d'Histoire Naturelle (Paris, France) and a post-doctoral grant from SU (Paris, France; Convergence program, ACOPAL project). We thank SOLEIL for provision of synchrotron radiation facilities (proposals 20130462and 0110189). We are grateful to Ronan Allain, Renaud Vacant and Dario de Franceschi for access to excavation sites and fruitful discussions, to the LUCIA beamline staff (D.Vantelon, N.Trcera, P.Lagarde, A.-M.Flank) and the AGLAE team (Quentin Lemasson, Brice Moignard, Claire Pacheco and Laurent Pichon) for support during allocated beamtime. We acknowledge the ICMCB (Bordeaux, France) and the ISA (Villeurbanne, France) for elemental quantifications. Finally, we thank two anonymous reviewers who helped to improve a previous version of the manuscript. ; |
Approved |
Most recent IF: 3.1; 2020 IF: 1.838 |
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Call Number |
UA @ admin @ c:irua:168651 |
Serial |
6619 |
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Author |
Odin, G.P.; Vanmeert, F.; Farges, F.; Gand, G.; Janssens, K.; Romero-Sarmiento, M.-F.; Steyer, J.S.; Vantelon, D.; Rouchon, V. |
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Title |
Alteration of fossil-bearing shale (Autun, France; Permian), part II : monitoring artificial and natural ageing by combined use of S and Ca K-edge XANES analysis, Rock-Eval pyrolysis and FTIR analysis |
Type |
A1 Journal article |
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Year |
2015 |
Publication |
Annales de paléontologie |
Abbreviated Journal |
Ann Paleontol |
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Volume |
101 |
Issue |
3 |
Pages |
225-239 |
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Keywords |
A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation) |
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Abstract |
Fossil-bearing shale specimens that include sulfides in their compositions are chemically reactive and sometimes also mechanically fragile. This decay is often related to iron sulfate efflorescence resulting from the oxidation of sulfide compounds. The processes underlying these degradations are poorly known, thus impeding the elaboration of curative or preventive treatments. The present contribution aims to identify the origin of museum specimen alterations. It focuses on the Flouest collection housed at the Museum National d'Histoire Naturelle (MNHN, Paris, France) and originating from the Autun Basin (Saone-et-Loire, France, Permian). To evaluate the alteration of MNHN specimens, it appeared necessary to compare their composition with that of unaltered shale so as to identify chemical changes occurring during ageing. Therefore, new material was collected in the Autun Basin, among others on the locality of Muse that corresponds to the same lithostratigraphic unit as that of the MNHN specimens. This material was, if necessary, artificially aged. The first part of this work, presented elsewhere, deals with the use of Xray diffraction and Mossbauer spectroscopy for characterizing iron reactivity and speciation. It leads to the conclusion that the reactivity of iron in the shale matrix was limited and could not account for the large efflorescence of iron (II) sulfate occurring nearby the fossil. The second part presented here focuses on the use of S K-edge X-ray Absorption Near Edge Structure (XANES) spectroscopy for characterizing sulfur speciation and reactivity. Measurements were performed on the shale matrix and on thin layers of maceral found in the proximity of damaged areas. As sulfur may be found in association with calcium or organic matter, complementary techniques were implemented, such as FTIR spectroscopy, Rock-Eval pyrolysis (characterization of organic matter content) and Ca K-edge XANES (analysis of calcium speciation) spectroscopy. It was shown that sulfur is mainly related to thioether, sulfoxide, iron sulfide, and sulfates whereas calcium is mainly bound to carboxylate, carbonate and/or sulfate groups. FTIR analysis of the macerals confirmed the presence of vitrinite on damaged MNHN specimens. The low oxygen content of new shale samples determined by Rock-Eval pyrolysis indicates that the organic matter is well preserved, despite the fact that samples come from outcrop surface. In the newly collected material, sulfur is mainly related to organic sulfides (thioether) with a minor occurrence of iron sulfide. In the shale fraction of damaged MNHN specimens, sulfur is mostly oxidized into a mixture of iron and calcium sulfate. However, in the vitrinite layers of the same specimens, a large proportion of sulfur corresponds to organic sulfides. Also the oxidation of sulfur does not occur homogeneously but preferentially in the shale fraction, probably because this latter is porous whereas vitrinite is not. Artificial ageing of new shale material showed that the oxidation of organic sulfides could be reproduced at 90 degrees C, 80% of relative humidity. However, the obtained efflorescence almost exclusively corresponds to calcium sulfate whereas iron (II) sulfates are mostly observed on MNHN specimens. The new material collected on site is probably to be questioned, and future studies will have to select new samples with fossil remains. This will be the object of the third part of this work. (C) 2015 Elsevier Masson SAS. All rights reserved. |
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Wos |
000363821700009 |
Publication Date |
2015-05-09 |
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Series Title |
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Abbreviated Series Title |
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Series Volume |
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Series Issue |
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Edition |
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ISSN |
0753-3969 |
ISBN |
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Additional Links |
UA library record; WoS full record; WoS citing articles |
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Impact Factor |
1.113 |
Times cited |
6 |
Open Access |
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Notes |
; This work was conducted within a PhD work that was supported by a doctoral school grant of the Museum national d'Histoire naturelle, Paris, France. We acknowledge SOLEIL for provision of synchrotron radiation facilities (Proposals ID “20130462” and “20110189”) and we would like to thank Nicolas Trcera, Pierre Lagarde and Anne Marie Flanck for assistance in using beamline LUCIA. ; |
Approved |
Most recent IF: 1.113; 2015 IF: 0.970 |
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Call Number |
UA @ admin @ c:irua:129523 |
Serial |
5462 |
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Author |
Odin, G.P.; Vanmeert, F.; Janssens, K.; Lelièvre, H.; Mertz, J.-D.; Rouchon, V. |
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Title |
Accelerated ageing of shales of palaeontological interest : impact of temperature conditions |
Type |
A1 Journal article |
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Year |
2014 |
Publication |
Annales de paléontologie |
Abbreviated Journal |
Ann Paleontol |
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Volume |
100 |
Issue |
2 |
Pages |
137-149 |
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Keywords |
A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation) |
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Abstract |
The palaeontological collections of the Muséum national dHistoire naturelle (MNHN, Paris, France) and the Muséum dHistoire naturelle dAutun (MHNA, Autun, France) include many fossil specimens originating from the argillaceous shales of the Autun basin (Saône-et-Loire, France). These fossils are preserved within sedimentary rocks containing unstable sulphide compounds, such as pyrite, which may deteriorate in contact with water and oxygen. This alteration provokes crystalline efflorescence and cracks, thus compromising the preservations of the fossils. This work constitutes the first step of a project that aims to understand the mechanisms of alteration of these materials in order to define conservation guidelines for palaeontological collections. For this purpose, eight damaged specimens originating from the Permian Autun basin (Saône-et-Loire, France) were selected and analyzed by X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy coupled to energy dispersive X-ray spectrometry (SEM/EDS) and X-ray absorption spectroscopy at the threshold of the sulphur Kα-edge (XANES). This methodology enabled the characterization of the matrices composition and the chemical nature of the alterations. Subsequently, we have sought to reproduce by artificial ageing the alteration phenomena encountered in the collections. New shale samples were collected on seven outcrops of the same Autun basin. They were analyzed and subjected to artificial ageing at 50% relative humidity (RH) and at temperatures ranging between 40 °C and 90 °C. Our work shows that damaged specimens and newly collected shale have a similar mineralogical composition. Yet the crystalline efflorescence material formed on the surface of damaged specimens belongs to the iron sulphate group whereas gypsum predominates on artificially aged shale samples. Reproducing the alterations observed on specimens by artificial ageing remains therefore problematic. Additionally, it appears that the temperature of ageing controls the nature of the damage: at 40 °C, many samples are mechanically damaged whereas no or minor crystalline efflorescence occurs. At 90 °C, it is the opposite tendency that is observed. Finally, mechanical damages do not seem to be correlated with the development of the efflorescence: samples with efflorescent crystals generally do not show clearly visible cracks; those that seem most fragmented do not show any visible efflorescence. |
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Wos |
000338607500006 |
Publication Date |
2014-01-24 |
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Abbreviated Series Title |
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Edition |
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ISSN |
0753-3969 |
ISBN |
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Additional Links |
UA library record; WoS full record; WoS citing articles |
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Impact Factor |
1.113 |
Times cited |
5 |
Open Access |
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Notes |
; This work is part of a PhD that is funded by the Museum national d'Histoire naturelle, Paris, France and was additionally supported via the S2-ART project (SDD programme of BELSPO, Brussels). The research was realized in partnership with the Palaeontological Collection Management Unit, Collection Department and with the Centre de Recherche sur la Paleodiversite et les Paleoenvironnements (CR2P, CNRS, UMR7207) of the Museum national d'Histoire naturelle, Paris, France. We are grateful to our colleagues MM. Jean Dejax and Dominique Chabard who provided palaeontological specimens and gave us access to shale deposits and Mrs Marie-Madeleine Blanc-Valleron who was of great help for the interpretation of the XRD data. ; |
Approved |
Most recent IF: 1.113; 2014 IF: 0.970 |
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Call Number |
UA @ admin @ c:irua:116594 |
Serial |
5456 |
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Author |
Rouchon, V.; Pellizzi, E.; Duranton, M.; Vanmeert, F.; Janssens, K. |
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Title |
Combining XANES, ICP-AES, and SEM/EDS for the study of phytate chelating treatments used on iron gall ink damaged manuscripts |
Type |
A1 Journal article |
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Year |
2011 |
Publication |
Journal of analytical atomic spectrometry |
Abbreviated Journal |
J Anal Atom Spectrom |
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Volume |
26 |
Issue |
12 |
Pages |
2434-2441 |
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Keywords |
A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation) |
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Abstract |
Many historical documents written with iron gall inks are endangered by the corrosive effects of these inks. In this work, a combination of complementary analytical methods was used for the first time in order to study the phytate process which is used in conservation studios to stabilize damaged manuscripts. This process consists of an antioxidant treatment performed by means of a calcium phytate (CP) solution, followed by a deacidification treatment performed with a calcium carbonate (CC) solution. The antioxidant treatment capitalizes on the properties of myo-inositol hexaphosphoric acid (phytic acid) that inhibits iron through chelation. In order to use relatively low acidic solutions, the pH of the CP solution is increased up to values between 5 and 6, which is in the range of the CP precipitation threshold. This study was performed on laboratory samples made of paper impregnated with iron gall ink and artificially aged in climatic chambers. It aims to investigate how the CP precipitate impacts the efficiency of the treatment. Side effects, such as elemental losses and deposits, were measured by means of several analytical techniques (FeK Edge XANES, SEM/EDS, and ICP-AES). These measurements were crosschecked with a ready to use colour spot test made of bathophenanthroline impregnated paper. It appeared that the CP treatment should necessarily be followed by the deacidification treatment in order to achieve long term stability. The precipitation of CP in the treating solution does finally not impact the efficiency of the treatment despite the fact that it should theoretically lower the availability of phytate to chelate iron. A scenario is proposed to explain this point. |
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Wos |
000297030400008 |
Publication Date |
2011-10-06 |
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Abbreviated Series Title |
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Series Volume |
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Series Issue |
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Edition |
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ISSN |
0267-9477 |
ISBN |
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Additional Links |
UA library record; WoS full record; WoS citing articles |
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Impact Factor |
3.379 |
Times cited |
10 |
Open Access |
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Notes |
; This research was funded by SOLEIL (proposals 20060396 and 20080761) and was supported by the Interuniversity Attraction Poles Programme-Belgian Science Policy (IUAP VI/16). The text also presents results of GOA “XANES meets ELNES” (Research Fund University of Antwerp, Belgium) and from FWO (Brussels, Belgium) projects no. G.0704.08 and G.01769.09. We are thankful to the paper conservator students of the Institut National du Patrimoine who were involved in some of the sample preparations, and to Dr Dominique Thiaudiere and Dr Solenn Reguer for their assistance and help during the experiments performed at SOLEIL beamline “DIFFABS”. ; |
Approved |
Most recent IF: 3.379; 2011 IF: 3.220 |
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Call Number |
UA @ admin @ c:irua:93845 |
Serial |
5527 |
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Author |
Rouchon, V.; Duranton, M.; Burgaud, C.; Pellizzi, E.; Lavédrine, B.; Janssens, K.; de Nolf, W.; Nuyts, G.; Vanmeert, F.; Hellemans, K. |
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Title |
Room-temperature study of iron gall ink impregnated paper degradation under various oxygen and humidity conditions : time-dependent monitoring by viscosity and X-ray absorption near-edge spectrometry measurements |
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A1 Journal article |
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Year |
2011 |
Publication |
Analytical chemistry |
Abbreviated Journal |
Anal Chem |
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Volume |
83 |
Issue |
7 |
Pages |
2589-2597 |
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Keywords |
A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation) |
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Abstract |
Many western manuscripts were written using iron gall inks. These inks can damage the paper via two major mechanisms: (a) acid hydrolysis, enhanced by humidity, and (b) oxidative depolymerization provoked by the presence of oxygen and free iron(II) ions. The degradation of unsized Whatman paper impregnated with different combinations of iron sulfate, gallic acid, and gum arabic was studied at room temperature in order to assess the relative importance of each mechanism. The samples were stored in various environments including a dry and/or an oxygen-free atmosphere. The cellulose depolymerization was monitored by viscometry and related to changes in the oxidation state of iron, determined by X-ray absorption near-edge spectrometry. The results indicate that residual amounts of oxygen (less than 0.1%) promote cellulose depolymerization, whereas the level of relative humidity has no impact. The cellulose depolymerization also appears closely correlated to oxidative mechanisms. Regarding the oxidation of iron, it only occurs in the simultaneous presence of oxygen and moisture, suggesting the occurrence of rustlike oxidative mechanisms. Finally, the presence of gallic acid has a strong influence, which is only partially explained by its capacity to reduce iron(III) to iron(II). |
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Wos |
000288887700028 |
Publication Date |
2011-03-04 |
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Abbreviated Series Title |
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Series Issue |
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Edition |
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ISSN |
0003-2700; 5206-882x |
ISBN |
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Additional Links |
UA library record; WoS full record; WoS citing articles |
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Impact Factor |
6.32 |
Times cited |
28 |
Open Access |
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Notes |
; This research was supported by the French Ministry of Culture within the National Program of Research (“La conservation des manuscrits: etude du vieillissement naturel de papiers impregnes d'encres ferrogalliques”). It was funded by grants from HASYLAB (experiments I-20090280 EC and II-20060245 EC) and SOLEIL (proposals 20060396 and 20080761) and was supported by the Interuniversity Attraction Poles Programme Belgian Science Policy (1UAP V1/16). The text also presents results of GOA “XANES meets ELNES” (Research Fund University of Antwerp, Belgium) and from FWO (Brussels, Belgium) projects nos. G.0689.06, G.0704.08 and G017909N. We are thankful to Dr. Dominique Thaudiere, Dr. Solenn Reguer, Dr. Andrea Somogyi, Dr. Karen Appel, Dr. Manuela Borchert, and Dr. Gerald Falkenberg for their assistance and help during the experiments performed at SOLEIL beamline “DIFFABS” and at HASYLAB Beam line “L” respectively. ; |
Approved |
Most recent IF: 6.32; 2011 IF: 5.856 |
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Call Number |
UA @ admin @ c:irua:89593 |
Serial |
5822 |
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Author |
Rouchon, V.; Pellizzi, E.; Janssens, K. |
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Title |
FTIR techniques applied to the detection of gelatine in paper artifacts: from macroscopic to microscopic approach |
Type |
A1 Journal article |
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Year |
2010 |
Publication |
Applied physics A : materials science & processing |
Abbreviated Journal |
Appl Phys A-Mater |
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Volume |
100 |
Issue |
3 |
Pages |
663-669 |
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Keywords |
A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation) |
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Abstract |
In order to render paper hydrophobic for ink and thus adequate for writing, gelatine has been largely used. To this day, it is still employed in conservation workshops as an adhesive or a sizing agent, for instance, during the treatment of iron gall ink manuscripts. Various types and concentrations of gelatine are recommended, depending on the desired effect, but little information is available regarding to the physical distribution of gelatine in the paper. This aspect is however determinant for a better control of conservation treatments. In this work, we investigate the possibilities offered by FTIR microscopy for the measurement of the gelatine distribution in paper. Laboratory papers were preliminary treated with different types of gelatine and then embedded in a resin and cut in thin slices. Mapping techniques enable to compare the penetration of different types of gelatine in a semiquantitative way. The performance of conventional laboratory equipment and synchrotron radiation experimental setup are discussed. |
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Wos |
000281317700011 |
Publication Date |
2010-04-01 |
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ISSN |
0947-8396 |
ISBN |
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Additional Links |
UA library record; WoS full record; WoS citing articles |
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Impact Factor |
1.455 |
Times cited |
12 |
Open Access |
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Notes |
; This work was performed with the support of the Fondazione Cassa di Risparmio di Torino, who founded the postgraduate internship of Eleonora Pellizzi at the CRCC (Master dei talenti). It received the technical support of the SMIS line of the SOLEIL synchrotron (Saint Aubin, France). We are thankful to all our colleagues who helped us during our experiments: Anne Laurence Dupont for providing gelatine samples, Chakib Djediat (Museum National d'Histoire Naturelle, Paris) for his advice regarding the samples preparation, Christophe Sandt (Synchrotron SOLEIL) for his help and availability during our Beam time allocation, and Paul Dumas (Synchrotron SOLEIL) for his warm reception on the SMIS line. ; |
Approved |
Most recent IF: 1.455; 2010 IF: 1.765 |
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Call Number |
UA @ admin @ c:irua:84579 |
Serial |
5627 |
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Author |
de Nolf, W.; Janssens, K.; Rouchon, V.; Falkenberg, G. |
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Title |
Study of the degradation on historical documents induced by iron gall ink by means of scanning μ-XRF/μ-XRD |
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H3 Book chapter |
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Year |
2007 |
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H3 Book chapter; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation) |
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Additional Links |
UA library record |
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Approved |
Most recent IF: NA |
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Call Number |
UA @ admin @ c:irua:64597 |
Serial |
5850 |
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