Preparation and Dating of Mortar Samples—Mortar Dating Inter-Comparison Study (MODIS)

Hajdas, Irka; Lindroos, Alf; Heinemeier, Jan; Ringbom, Åsa; Marzaioli, Fabio; Terrasi, F.; Passariello, Isabella; Capano, Manuela; Artioli, Gilberto; Addis, Anna; Secco, Michele; Michalska, Danuta; Czernik, Justyna; Goslar, Tomasz; Hayen, Roald; Strydonck, Mark Van; Fontaine, Laurent; Boudin, Mathieu; Maspero, Francesco; Panzeri, Laura; Gallí, Anna; Urbanová, Petra; Guibert, Pierre

doi:10.1017/rdc.2017.112

Cited by 47 publications

(60 citation statements)

References 39 publications

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“…Mineralogical quantitative phase analyses (QPAs) were performed by XRPD on fine sample powders obtained by micronization. The quantitative measurements are expressed in wt% ± (Rietveld error), which is the most quoted value used as the error related to phase abundance and represents the uncertainty in the mathematical fit between the observed and calculated patterns (Madsen and Scarlett 2008;Gualtieri et al 2019). XRPD analyses were performed using a Malvern PANalytical X'Pert PRO diffractometer in Bragg-Brentano geometry, Co-Kα radiation, 40 kV and 40 mA, equipped with a real-time multiple strip (RTMS) detector (X'Celerator by Malvern Panalytical).…”

Section: Mortar Characterizationmentioning

confidence: 99%

“…The principle of the radiocarbon ( 14 C) dating method of lime mortars has been discussed and applied since the 1960s, and in the case of lime-based mortars with a one-step carbonation history, new and modified protocols are applied in order to provide plausible dates relative to the time of setting and hardening of the binder (Delibrias and Labeyrie 1964;Heinemeier et al 2010;Van Strydonck 2016;Hajdas et al 2017). However, such an ideal situation is hardly encountered in practical cases, where 14 C dating of the carbonated binder is variously affected mainly by: (i) geologic or fossil carbonate, which could affect the dating incorporating dead carbon and overestimating the age; (ii) secondary alteration processes, lime lumps, delayed hydraulic reactions and formation of new phases containing carbonate occurring over a relatively long period, could be responsible of an underestimation of the age (Lindroos et al 2007;Artioli 2010;Miriello et al 2010;Michalska and Czernik 2015;Ponce-Antón et al 2018).…”

Section: Introductionmentioning

confidence: 99%

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The Cannero Castle (Italy): Development of Radiocarbon Dating Methodologies in the Framework of the Layered Double Hydroxide Mortars

et al. 2020

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The mortar samples of the Castle of Cannero (Lake Maggiore, Italy) have been characterized and radiocarbon (14C) dated. The presence of LDH phases was identified. The hydraulic reaction was evaluated by a multi-analytical approach. Careful extraction, preparation and purification of the binder fraction have been performed. Contaminations due to LDH phases have been removed allowing reliable absolute dating of the structures. Non-hydraulic lime-based mortars represent only part of the binding materials found in archaeological and historical structures, and a new challenge is the application of 14C dating techniques on mortars that feature hydraulic reactions. This research work aims at 14C dating a series of Mg-rich hydraulic mortars from the Castle of Cannero (Lake Maggiore, Italy), from which both charcoals and mortar samples were collected. A multi-analytical approach employing X-ray powder diffraction (XRPD), optical microscopy (OM), and scanning electron microscopy/energy-dispersive microanalysis (SEM-EDS) was adopted in order to carefully characterize the samples. A wet gravimetric separation for the extraction of the fine fraction mainly composed by the mortar binder was carried out and the binder fraction was characterized by XRPD in order to investigate the presence of contaminants. The binding fractions are characterized by the widespread occurrence of hydrotalcite-type minerals, considered contaminants in 14C dating of mortars because of their capability to exchange carbonate anions even after the hardening process. A further purification treatment by thermal decomposition was performed before 14C dating by AMS. The obtained dates were consistent with archaeological expectations, confirming the potential of the developed purification methodology for hydraulic mortars dating.

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Section: Mortar Characterizationmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

The Cannero Castle (Italy): Development of Radiocarbon Dating Methodologies in the Framework of the Layered Double Hydroxide Mortars

et al. 2020

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“…Indeed, pyrogenic calcite has been targeted since the 1960s to date lime mortars (Labeyrie & Delibrias, 1964). However, the accuracy of the method is significantly limited by several carbonate contaminants, such as secondary calcite, to the point that presently a single approach to date any type of mortar is not available (Hajdas et al, 2017). Similar problems affect calcite in wood ash (e.g., Koumouzelis et al, 2001), although promising results have been obtained from well‐preserved crystals (Regev, Eckmeier, Mintz, Weiner, & Boaretto, 2011).…”

Section: Archaeological Significancementioning

confidence: 99%

The significance of aragonite in the interpretation of the microscopic archaeological record

Toffolo

2020

Geoarchaeology

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Aragonite is one of the metastable polymorphs of calcium carbonate and is commonly found at archaeological sites in the form of mollusk shells and speleothems. Other occurrences include corals, fish otoliths, seed endocarps, wood ash, and lime plaster. These materials contain microscopic embedded information of fundamental importance for the assessment of the state of preservation of the archaeological record, the reconstruction of paleoenvironments, the identification of pyrotechnological processes, and the establishment of absolute chronologies. However, this information can be used only if the aragonite found at archaeological sites preserves its pristine structure and chemistry. Aragonite is metastable at ambient conditions and tends to dissolve and recrystallize into secondary aragonite or calcite, a process that entails the loss of its original elemental and isotopic signature. Therefore, well‐grounded archaeological interpretations depend on the correct identification of aragonite and the careful characterization of its basic properties. This article reviews the dissolution processes of different types of aragonite, the methods used for their identification, and the archaeological information that can be extracted. Particular emphasis is given to the discussion of key issues regarding absolute dating and postdepositional processes of archaeological sediments, and to a detailed overview of the recently observed pyrogenic aragonite.

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“…The preparation procedure of bulk mortars is described by Hajdas et al (2017). The mortars are carefully crushed and sieved into decreasing grain-size fractions (see e.g.…”

Section: Sample Preparationmentioning

confidence: 99%

Radiocarbon Dating Historical Mortars: Lime Lumps and/or Binder Carbonate?

et al. 2018

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Lime lumps and bulk mortars show different 14C contamination when analyzed in several CO2 fractions isolated from the effervescence of an ongoing hydrolysis reaction. Age profiles of both materials are therefore highly complementary and together they can provide a reliable date. Furthermore, they can also reveal the complexity of the radiocarbon (14C) distribution within the mortar and thus prevent over-interpretation of the data. The lime lump versus bulk mortar dating data presented here has been collected over 22 years, with only a small fraction of the results so far published internationally. Since there has been an increasing interest in mortar dating over recent years with a special focus on lime lumps, and since many laboratories have just begun mortar dating experiments, we wish to present some of the extensive data that already exist. Previously published data from 15 lime lumps (including 34 14C measurements from sequential dissolution) and 43 new 14C measurements from 17 lime lumps are presented here. The samples are from medieval Finland and Sweden, classical Rome and medieval Italy, and the Roman Jerash (Gerasa), Jordan.

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Preparation and Dating of Mortar Samples—Mortar Dating Inter-Comparison Study (MODIS)

Abstract: ABSTRACT. Seven radiocarbon laboratories: Åbo/Aarhus, CIRCE, CIRCe, ETHZ, Poznań, RICH, and Milano-Bicocca performed separation of carbonaceous fractions suitable for

Cited by 47 publications

References 39 publications

The Cannero Castle (Italy): Development of Radiocarbon Dating Methodologies in the Framework of the Layered Double Hydroxide Mortars

The Cannero Castle (Italy): Development of Radiocarbon Dating Methodologies in the Framework of the Layered Double Hydroxide Mortars

The significance of aragonite in the interpretation of the microscopic archaeological record

Radiocarbon Dating Historical Mortars: Lime Lumps and/or Binder Carbonate?

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