For several decades, many efforts have been dedicated to enhancing the accuracy of mortar radiocarbon dating and evaluating the reliability of the results concerning the typology of the examined specimens. Several assumptions that are fundamental for the application of the method may be in many cases not fulfilled, such as (a) complete primary limestone dissociation during calcination, (b) efficient separation of geogenic carbon contained in calcareous aggregates, (c) short carbonation time, and (d) absence of secondary calcite. Many laboratories all over the world have proposed different methods to select suitable fractions of mortar.

The first intercomparison attempt, involving eight international laboratories, was organized in 2016 aiming at comparing and statistically treating the results obtained on the same materials by different laboratories with their own characterization and pre-treatment methods (Hajdas et al. 2017; Hayen et al. 2017). Following this first step, a new intercomparison experiment was proposed and set up in 2018 during the Mortar Dating International Meeting (Bordeaux, FR). A new set of three mortar samples was chosen, taking care of the selection of standardized materials (homogeneity, known mineralogical composition, absence of exogenous inclusions, known expected age).

This work describes the results of two research teams involved in the intercomparison. The samples were characterized, selected, and dated depending on each laboratory strategy. The results stress the importance of the characterization of the raw material is to better understand the mineralogical and petrographical composition of the samples. Such information can support the choice of the most appropriate strategy for the extraction of CO2 and then for data interpretation.

Horizontal watermills in the southern Levant have proved difficult to date. This study investigates the use of radiocarbon (14C) dating of various organic carbon fractions in structural mortars and carbonate deposits to identify terminus post quem (TPQ) construction dates for seven arubah watermills and two chute watermills in northern Jordan. Dating results from the various organic fractions are discussed in the contexts of carbon fraction integrity and mortar type. The arubah watermill construction dates fall into two chronological groups. Four arubah watermills have Middle Islamic (late 12th to early 14th century AD) construction dates based on macrocharcoal and bulk organic fraction ages, whereas the bulk organic fraction ages of two earlier arubah watermills straddle the Byzantine-Early Islamic transition. Their possible fifth to seventh-century construction dates are among the earliest in the southern Levant. Limited 14C data from the chute water mills suggests that the earliest may date to the sixth–seventh century period, concurrent with the older arubah watermills. The study supports the viability of the AMS 14C method to provide estimated TPQ construction dates for watermills, providing caution is exercised. Short-lived macrocharcoals have the highest integrity but are subject to severe sample loss during pretreatment. 14C ages from humic and humin fractions in earthen mortars are influenced by “old carbon” contamination, possibly a soil reservoir effect, and are centuries older than the probable construction date. Attention is drawn to the potential use of arubah carbonate deposits as proxy records of water flow, watermill use, and hydroclimate.

The research aims to reconstruct the chronology of building the Southwest Church, Umm el-Jimal, Jordan by AMS radiocarbon dating organic inclusions uncovered from the mortars collected from the floor of the church, seat of the apse and the base of the north wall. It sheds light on the major aspects of mortar recipes at the time of their production. Samples were examined macroscopically with magnifying lenses and characterized using archaeometric techniques of optical microscopy and X-ray diffraction. The radiocarbon dates showed that 594–643 AD is the most probable age for flooring and plastering the church and 995–1154 AD is the earliest possible date for its final collapse. The preparatory layers of the church floor were laid on an older one, probably of a yard, and its north wall was raised on an older base, both most probably date to the late fifth–early sixth century AD. The production recipe of the mortars is made from a lime binder and inclusions mainly of organic (charcoal) and inorganic (quartz, grog, volcanics). The mortars have the same recipe regardless their bedding and jointing functions which remained unchanged during the building stages of church complex.

To obtain scientific data regarding the chronology of archaeological structures, lime mortar radiocarbon dating has often demonstrated to be a decisive method. However, knowing the specific chemical-mineralogical characteristics of mortars can help when preparing samples or interpreting results. Among other issues, the dating of magnesian mortars can be particularly difficult because of the combined slaking, setting and hardening reactions of the calcium and magnesium phases, typical of these mortars. The formation of numerous mineralogical phases depending on reaction conditions adds further complexity to the dating method, which deserves to be studied with further detail. During the project “Mortar technology and construction history at Müstair Monastery” the first experiments in this regard had yielded encouraging results. An additional 4 samples from buildings with controversial chronology, thought to belong approximately to the 9th, 12th, and 15th centuries, were selected, prepared and radiocarbon dated. The data obtained were discussed by integrating preliminary petrographic characterization analyses of the mortars with archaeological information and excavation records. The results opened up new questions about the chronology of the Monastery, clarified the dating of some buildings and provided a better understanding of the potential and limitations of dating dolomitic mortars coming from archaeological context.

Absolute dating of plasters and mortars clearly represents a key information to study important structures and buildings that may have undergone a difficult story starting from their construction. This is for instance the case of the architectures in the archaeological site of Hierapolis (Denizli, Turkey). However, when discussing about the possibility to apply radiocarbon (14C) dating, in this site the presence of different sources of contaminants, due to the geological and geochemical conditions and to the used raw materials, prevents the binder dating. As an alternative, we thus decided to focus on the small fragments of straw that had been used as additives in the mortar/plaster matrices. The fragments were identified, selected and dated using a 14C experimental set-up specifically optimized for microgram-sized samples. The obtained results were satisfying, even though the measured 14C ages also pointed out some possible criticalities in dating such small samples collected from a carbonaceous matrix.

An international consortium of radiocarbon (14C) laboratories was established to date the origin of the St. George’s Rotunda in Nitrianska Blatnica (Slovakia), because its age was not well established in previous investigations. Altogether, 20 samples of wood, charcoal, mortar and plaster were analyzed. The 14C results obtained from the different laboratories as well as between the different sample types were in good agreement, resulting in a 14C calibrated age of 783–880 AD (94.2% probability) for the Rotunda. Although the 14C results have very good precision, the specific plateau-shape of the calibration curve in this period caused the wide range of the calibrated age. The probability distribution from OxCal calibration shows, however, that about 86% of the probability distribution lies in the period before 863 AD, implying that the Rotunda could have been constructed before the arrival of Constantine (St. Cyril) and St. Methodius to Great Moravia. The Rotunda thus probably represents the oldest standing purpose-built Christian church in the eastern part of Central Europe.

The results of a short program of landscape, buildings and materials analysis undertaken at Achanduin Castle, Lismore, Scotland (NM 8043 3927) are presented from the pilot phase of the Scottish Medieval Castles & Chapels C14 Project (SMCCCP). The study presents the first independent chronological evidence relating to the construction of this important medieval building, by radiocarbon analysis of a limited assemblage of Mortar-Entrapped Relict Limekiln Fuel (MERLF) fragments. Informed by a wider investigation of structural phasing and sample taphonomy, these measurements are constrained within a series of different Bayesian models, to generate a range of comparative estimates for the building’s constructional chronology. The precision with which the construction of this building can now be dated, from other evidence associated with the site, makes the Achanduin Castle study a useful point of reference for wider materials research.

Electron paramagnetic resonance (EPR) spectroscopy is a well-established method of dating based on trapped charges, applied to various crystalline materials, including carbonates, bones, and teeth. It provides a detailed insight into the structure of radiation defects—paramagnetic centers generated by irradiation, without the need of a painstaking sample preparation, often challenging in other methods. Using EPR we studied the effect of γ radiation on lime mortars and plasters from ancient settlement Hippos in Israel, in order to analyze the process of defect generation. Analysis of the complex spectra revealed the presence of radiation-induced species, including CO2–, NO32– and organic radical. Using an artificial UV source, we generated relatively strong signals of paramagnetic centers, analogous to those created by γ irradiation, reaching their maximum intensity after 5–6 hr of UV exposure. Our results confirm the previous reports that radiation defects can also be generated, instead of bleached, in calcite by UV radiation, which is crucial for identifying the issues related to light exposition, affecting the accuracy of age determinations in trapped-charge dating methods.

The ages of mortars and plaster can help reveal the history of monuments, their construction, or restoration times. However, these anthropogenic carbonates pose a challenge when it comes to separation of the atmospheric radiocarbon (14C) signal of the CO2 fixed in the mortar at the time of consolidation, i.e., the time of binder formation. The variety and heterogeneity of mortars require individual assessments of each sample and 14C results. Here we present our current preparation method and summarize experience based on results collected during the last 20 years of mortar dating at the ETH laboratory.

The monastery of St. John in Müstair, a UNESCO world heritage site, preserves archaeological remains and stone structures dated from the 8th century to the present. It has been extensively studied archaeologically so that numerous samples of historical materials, including mortar, are available for study. In addition to that, some of the structures have been precisely dated with dendrochronology. The monastery is located in a region characterized by dolomite rocks and the mortars are therefore of dolomitic nature, being perfectly suited to test the possibility of being dated with 14C. Furthermore, the presence of embedded carbon fragments has provided additional independent data to support or deny the results of mortar dating. A comparison of the results obtained from radiocarbon (14C) dating of bulk mortars, sieved fractions enriched in binder, lime lumps and carbon fragments, for two samples is presented, in relation to the petrographic characterization and the mineralogical phase content. This preliminary study shows that the dating of 14C can potentially be applied to the mortar of Müstair, as results in accordance with the established chronologies have been obtained for one sample. However, if the dolomitic sand contamination is very high, further studies are needed to develop a specific sample preparation technique.

Dating lime mortar shows great potential for establishing the chronology of a construction. The basic premise of mortar dating by optically stimulated luminescence (OSL) is that quartz in the sand used for making mortar has been optically zeroed during the preparation process (optical bleaching). The moment to be dated is the last exposure of sand grains to light, before being embedded within the masonry and hidden from light. However, the main problem is the frequent partial and heterogeneous bleaching of grains, and this led us to use the single grain technique (SG-OSL) systematically. Some theoretical and experimental aspects of a new statistical treatment (the EED model, as exponential exposure distribution) are detailed and discussed. Our experience shows that SG-OSL dating of mortars is successful in a majority of situations. In a minority of cases (around 15%) difficulties originate when there is inappropriate OSL behavior of grains, and thus OSL dating is not possible. In the other cases, good agreement was obtained between OSL ages and the reference ones for a series of samples from a variety of ages and situations, even in the case of poorly bleached material. Anyway, the present situation of OSL dating methodology justifies the systematic use of SG-OSL in the dating of masonry today.

Accurate radiocarbon (14C) dating of lime mortars requires a thorough mineralogical characterization of binders in order to verify the presence of carbon-bearing contaminants. In the last 20 years, cathodoluminescence (CL) has been widely used for the identification of geologic calcium carbonate (CaCO3) aggregates and unreacted lime lumps within the particle size fraction selected for carbon recovery. These components are major sources of older and younger carbon, respectively, and should be removed to obtain accurate age determinations. More recently, laser-induced fluorescence (LIF) has provided another means of investigating the preservation state and composition of CaCO3 binders. Considered the growing interest of the mortar dating community in the latest advancements of these analytical methods, here we review the principles of CL and LIF of CaCO3, their instrument setup, and their application to the characterization of ancient lime mortars used for 14C dating. In addition, we provide examples of SEM-CL and LIF analyses using high-resolution instrumentation, we discuss current issues and propose future lines of research.

After the last damaging earthquake in 2012, an anti-seismic reinforcement project of the cathedral of Modena was designed giving us the opportunity to investigate and date the building materials. Radiocarbon (14C), optically stimulated luminescence (OSL), and thermoluminescence (TL) dating techniques were performed on the vaults with the aim to (1) clarify the construction timing, (2) define the history of the restorations, and (3) explore the possible correlation of the main restoration works to the earthquake chronology deduced from the historic catalog. Preliminary results show that medieval older bricks were reused for most of the original construction. Only lime and non-gypsum mortar was used for the original construction in the 15th century and for later repair of damage caused by earthquakes in the 16th and 17th centuries. Gypsum mortar was used for later repair in the 18th century. The results show much stronger damage due to earthquakes than previously thought.

The Aqueduct is one of the city landmarks of Skopje, Republic of North Macedonia. It was part of a water-supply system, with a total original length of about 10 km, while its surface remains are about 385 m long. The age of the Aqueduct is not known—several hypotheses place it to periods between the 6th and 16th centuries. Six mortar samples from different positions of the eastern façade were taken for radiocarbon (14C) dating. In order to extract only the carbon associated to the time of building, three strategies for sample preparation were used: (1) mechanical separation of lime lumps formed during mortar hardening (2) selection on the basis of particle size and the ability to suspend in water induced by ultrasonic shock, and (3) collection of two gas CO2 fractions produced from the same bulk in reaction with acid. Characterization of fractions was performed by isotopic carbon composition and FTIR-ATR analyses. The most plausible results were obtained from lime lump fractions that were dated in the timeframe of 15th to 17th century.

Bentonite is composed primarily of montmorillonite and is useful in a wide range of applications. This paper presents the results of an experimental investigation carried out to evaluate the possibility of using a Pakistani bentonite (from Jehangira, Swabi District) as a cement replacement material in mortar and concrete. The cement in mortar and concrete was replaced with the bentonite at 0%, 20%, 30%, 40% and 50% by cement mass. The strength activity index of bentonite was determined ‘as received’ (20ºC) and ‘heated’ (treatment at 500ºC and 900ºC). The test results indicated that the strength activity index of bentonite conformed to the ASTM Standard C618 specifications, except for the ‘900ºC heated’ bentonite. The water absorption decreased for mortar containing up to 30% bentonite and then steadily increased at higher bentonite loadings. When immersed in 5% Na2SO4 and 2% MgSO4 solution, the greatest compressive strength was observed for mortar containing 30% bentonite. The water demand of concrete increased with increasing bentonite content. Although the compressive strength of concrete decreased progressively as the substitution level of bentonite was increased, the compressive strength of concrete containing 30% ‘as received’ bentonite was found to be 70% of the control concrete, whereas for concrete containing 30% ‘500ºC heated’ bentonite, the strength was found to be 79% of the control concrete. It can be concluded that this Pakistani bentonite can be used to replace up to 30% of cement to produce concrete with sufficient compressive strength for low-cost construction resistant to sulphate attack.

Lime-based mortars with admixtures of metakaolin (10, 20 and 30 wt.%) and fine sepiolite (5 wt.%) were prepared with the aim of facilitating their use as repair mortars in low-humidity conditions. The mechanical properties and the dynamic modulus of elasticity were studied after 28, 90 and 180 days of curing. With an increasing amount of metakaolin in lime mortars, improved mechanical strength was observed mainly after 90 days. Addition of fine sepiolite, due to its adsorption properties for storing water for later supply to the mortar system and its microfibrous morphology, led to an improvement of compressive and flexural strength of blended air lime/air lime-metakaolin mortars, espec ially at later ages of curing. Incorporation of fine sepiolite into air lime-metakaolin mortars resulted in comprehensive densification of the core of the mortars. Air lime mortar containing 5 wt.% of fine sepiolite and 20 wt.% of metakaolin appears to be an optimal admixture.

Cement mortars and concretes incorporating clinoptilolite, silica fume and fly ash were investigated for changes in their physical and mechanical properties. It was found that additions of 10% clinoptilolite and 10% Pozzolite (1:1 mixture of silica fume and fly ash) were optimal for improvement of the quality of the hardened products, giving 8% and 13% increases in flexural and compressive strength respectively. The specific pore volume of the mortars incorporating zeolite decreased between the 28th and 180th day to levels below the values for the control composition due to the fact that clinoptilolite exhibits its pozzolanic activity later in the hydration. In these later stages, pores with radii below 500 nm increased at the expense of larger pores. The change in the pore-size distribution between the first and sixth months of hydration occurs mostly in the mortars with added zeolite.

To date, finding a technique able to effectively isolate the carbon signal from the binder of a mortar is still an open challenge. In this paper, the radiocarbon (14C) dating of one of the most challenging and diffuse types of mortar, the one with pozzolana aggregate, is investigated. Eight mortar samples from three archaeological sites near Rome (Italy) underwent a selection process called Cryo2SoniC. The selected fractions were analyzed by the accelerator mass spectrometry (AMS) 14C technique and compared to known historical references. Additional scanning electron microscopy analysis and petrographic investigations were done, respectively, to check the grain size of the fractions selected by Cryo2SoniC, and further, to characterize the original mortar samples. The masses of carbon yielded from the dated fractions were almost half of those released from some aerial mortars. The 14C dating results were accurate for pozzolana mortars, from buried and unburied structures, with calcination relics and small contamination of secondary calcite. A limitation in the purification protocol was observed on samples with a massive contamination of secondary calcite deposition of ground water origin, occluding porosity and substituting up to the 80% of the original binder matrix.

Seven radiocarbon laboratories: Åbo/Aarhus, CIRCE, CIRCe, ETHZ, Poznań, RICH, and Milano-Bicocca performed separation of carbonaceous fractions suitable for 14C dating of four mortar samples selected for the MOrtar Dating Inter-comparison Study (MODIS). In addition, optically stimulated luminescence (OSL) analyses were completed by Milano-Bicocca and IRAMAT-CRP2A Bordeaux. Each laboratory performed separation according to laboratory protocol. Results of this first intercomparison show that even though consistent 14C ages were obtained by different laboratories, two mortars yielded ages different than expected from the archaeological context.

The authors demonstrate the potential for dating structures in Near Eastern archaeology by applying AMS radiocarbon to organic inclusions found in mortar and plaster. The method was successfully applied to date and sequence excavated walls and floors, and to spot-date structures exposed in surveys.