scholarly journals Revisiting radiocarbon dating of lime mortar and lime plaster from Jerash in Jordan: Sample preparation by stepwise injection of diluted phosphoric acid

2022 ◽  
Vol 41 ◽  
pp. 103244
Author(s):  
Thomas Schrøder Daugbjerg ◽  
Achim Lichtenberger ◽  
Alf Lindroos ◽  
Rubina Raja ◽  
Jesper Olsen
2020 ◽  
Vol 47 (1) ◽  
pp. 187-195
Author(s):  
Alf Lindroos ◽  
Jan Heinemeier ◽  
Åsa Ringbom ◽  
Thomas Schrøder Daugbjerg ◽  
Irka Hajdas

AbstractFour lime mortar samples from the Mérida amphitheatre in Spain were dated in 2001 and re-dated in 2019 with refined dating methods and focus on carbon dioxide that was released in late CO2 fractions when dissolved in phosphoric acid. The samples were difficult to date because they contained highly soluble, young carbonate contamination that dominated the carbon dioxide from the early stages of the reaction with the acid in the hydrolysis process. They were also rather hydraulic and rich in magnesium, which could have caused delayed hardening. However, there was very little dead carbon contamination so that late carbon dioxide fraction gave uniform 14C ages, pointing to a late 1st c. AD Flavian, or later age of the amphitheatre.


Radiocarbon ◽  
2012 ◽  
Vol 54 (3-4) ◽  
pp. 905-914 ◽  
Author(s):  
Khaled Al-Bashaireh ◽  
Gregory W Hodgins

This research aims at radiocarbon dating 2 structures of archaeological interest from Petra, south Jordan, using lime plaster and mortar. Initially, the samples' content of calcareous contamination was examined by petrography and cathodoluminescence. In order to date clean lime binders, the samples were gently crushed and 63–45 μm powders were collected by dry sieving, then the CO2 gases, collected by a hydrochloric acid hydrolysis of the powders, were dated. The interpreted 14C dates clarify the chronology of the studied structures, show an agreement with the archaeological and historical data, and may indicate the efficiency of the cleaning and hydrolysis procedures.


Radiocarbon ◽  
2021 ◽  
pp. 1-23
Author(s):  
Thomas Schrøder Daugbjerg ◽  
Alf Lindroos ◽  
Irka Hajdas ◽  
Åsa Ringbom ◽  
Jesper Olsen

ABSTRACT Dating lime mortar samples using the radiocarbon (14C) method can be difficult. This is because the contamination is similar to the primary dating material (CaCO3) and consequently difficult to remove. Mortar can also have late-in-formation pyrogenic carbonate from interactions with the environment after the initial hardening phase, such as recrystallization, fire damage or delayed hardening. When 14C dating a system of primary dating material, contamination and late-in-formation pyrogenic carbonate, one approach is multi-fraction dating with conclusiveness criteria. If a sample has sufficient contamination or late-in-formation pyrogenic carbonate, the criteria evaluate the result inconclusive. To improve inconclusive results from such samples, this study investigates sample preparation by thermal decomposition. Here samples that were inconclusively dated by the authors’ traditional method, sequential dissolution with 85% phosphoric acid, are investigated further. This study finds that CO2 thermally decomposed at low temperatures contains some late-in-formation pyrogenic carbonate. By rejecting CO2 decomposed at low temperatures, Kastelholm castle and Kimito church in Finland are conclusively and accurately dated. Furthermore, a preheating method removes some late-in-formation carbonate, but not enough for a conclusive result. Finally, thermal decomposition finds difficulty in discerning binder carbonate from limestone and marble contamination.


2009 ◽  
Vol 61 (4) ◽  
pp. 639-644 ◽  
Author(s):  
Gorica Vukovic ◽  
Snezana Pavlovic ◽  
M.S. Ristic

In preparation of samples for chromatographic determination of ochratoxin A, two types of columns were used for sample cleanup (SPE and immunoaffinity columns). The first method consisted of liquid-liquid extraction with a mixture of chloroform and phosphoric acid, followed by ion-exchange cleanup on Waters Oasis MAX columns. The sec?ond method consisted of extraction with a mixture of water and methanol, followed by LCTech OtaCLEAN immunoaf?finity column cleanup. Recoveries of the methods were determined at three levels in three repetitions for maize flour, and they were 84% (%RSD = 19.2) for the first method of sample preparation and 101% (%RSD = 2.2) for the second method. Values of LOQ for OTA were 0.25 and 1.00 ?g/kg for the IAC and SPE clean-up procedures, respectively. Both methods comply with present regulations, but the MAX sample clean-up procedure should be used as an alternative, since the immunoaffinity column clean-up procedure is characterized by better reproducibility, accuracy, and efficiency.


Radiocarbon ◽  
1972 ◽  
Vol 14 (1) ◽  
pp. 149-154 ◽  
Author(s):  
Dennis D. Coleman

The following date list includes all samples processed from December 1969 through November 1970 at the Illinois State Geological Survey Radiocarbon Dating Laboratory. The benzene liquid scintillation technique was used, following the method of Noakes, Kim, and Stipp (1965), and Noakes, Kim, and Akers (1967). Detailed sample preparation procedures used in this laboratory have been reported by Kim and Ruch (1969), and Kim, Ruch, and Kempton (1969).


Radiocarbon ◽  
2020 ◽  
Vol 62 (3) ◽  
pp. 565-577 ◽  
Author(s):  
Alf Lindroos ◽  
Åsa Ringbom ◽  
Jan Heinemeier ◽  
Irka Hajdas ◽  
Jesper Olsen

ABSTRACTWhen sampling mortars for radiocarbon (14C) dating it is crucial to ensure that the sample has hardened rapidly relative the resolution of the dating method. Soft and porous lime mortars usually fulfill this criterion if the samples are taken from an uncovered surface from less than a few centimeters deep. However, hard, concrete-like mortars may be impermeable for carbon dioxide and even the outermost centimeters may still contain uncarbonated calcium hydroxide. These mortars may harden very slowly and contain carbonate that formed centuries or even millennia after the original building phase, and they can still be alkaline and capture modern 14C, causing younger 14C ages than the actual construction age. Another problem is reactivation of the binder carbonate if it has been partly decarbonated during a fire later on in its history. It will be shown that these young carbonates dissolve rapidly in phosphoric acid and in many cases a reasonable 14C age can be read from 14C profiles in sequential dissolution if the measurements from initially formed carbon dioxide are disregarded. However, if a mortar was made waterproof deliberately by adding crushed or ground tile, as in Roman cocciopesto mortars, it may be very difficult to get a conclusive dating.


Radiocarbon ◽  
2020 ◽  
Vol 62 (3) ◽  
pp. 633-655 ◽  
Author(s):  
Michael B Toffolo ◽  
Lior Regev ◽  
Eugenia Mintz ◽  
Ifat Kaplan-Ashiri ◽  
Francesco Berna ◽  
...  

ABSTRACTRadiocarbon (14C) dating of anthropogenic carbonates (CaCO3) such as ash, lime plaster and lime mortar, has proven a difficult task due to the occurrence of a number of contaminants embedded within the CaCO3 pyrogenic binder. These include 14C-free geologic components and/or secondary phases bearing an unknown amount of 14C, and thus the alteration of the original pyrogenic isotopic signature of the material results in major age offsets when carbon recovery is performed through acid hydrolysis. Here we present a characterization/quantification approach to anthropogenic carbonates that includes Fourier transform infrared spectroscopy (FTIR), X-ray diffraction, thin section petrography, thermogravimetric analysis and scanning electron microscopy coupled with high-resolution cathodoluminescence, with which we identified the pyrogenic CaCO3 fraction in an aerial lime plaster and two hydraulic mortars. The preserved pyrogenic component was then isolated by density separation and its purity checked again using FTIR. Carbon was recovered through thermal decomposition in vacuum. The resulting 14C age matches the expected age of the lime plaster, whereas hydraulic mortars are slightly offset due to the carbonation of calcium hydroxide lumps. This approach highlights the importance of a dedicated characterization strategy prior to dating and may be applied to aerial lime plasters to obtain accurate ages.


2021 ◽  
Vol 8 ◽  
Author(s):  
Irka Hajdas ◽  
Ursula Sojc ◽  
Susan Ivy-Ochs ◽  
Naki Akçar ◽  
Philip Deline

The Arp Nouva peat bog located in the upper Ferret Valley in the Mont Blanc massif was critically evaluated since published radiocarbon dates have led to controversial conclusions on the formation of this swamp. Radiocarbon dating of woody fragments from three pits of up to 1 m depth was used to discuss the question of whether the historically documented rock avalanche occurring in 1717 CE overran the peat bog or settled prior to its formation. For the deepest samples in the pits, calibrated radiocarbon ages between 1,652 and 1950 CE (95.4%; confidence level) were obtained, which fit very well into the time frame of the historical documented 1717 CE rock avalanche event. It can, therefore, be concluded that the Arp Nouva peat bog was formed by blockage of the Bella Combe torrent by the rock avalanche deposits. Furthermore, careful sample preparation with consequent separation of woody fragments from the bulk peat sample has shown that the problem of too old 14C ages can be circumvented. This work demonstrates that a combined geomorphological and geochronological approach is the most reliable way to reconstruct landscape evolution. The key to successful 14C dating is careful sample selection and the identification of the material that might not be ideal for chronological reconstructions.


2017 ◽  
Vol 4 (2) ◽  
pp. 394-401 ◽  
Author(s):  
Rustam Musta ◽  
Aceng Haetami ◽  
Mimi Salmawati

Study of the transesterification of Calophyllum innophyllum seed oil from Kendari with methanol has been conducted. The purpose of the research to determine of the yield of ester produced in transesterification process with methanol, the viscosity of biodiesel produced, moisture content of biodiesel produced, density of biodiesel produced. The methods used in this study are sample preparation, transesterification process, biodiesel quality parameter test consisting of viscosity, moisture content and density. The results showed that good concentration of phosphoric acid was used to remove the gum is 85%, the yield of ester produced in the process of transesterification with methanol is 111,647%, parameter of biodiesel quality measured that viscosity = 0,315 mm2/ s not fulfill Indonesian National Standart (INS), water content is 0.02 meets the INS and the density = 0.8725 g / cm3 meets the INS standard


Heritage ◽  
2020 ◽  
Vol 3 (4) ◽  
pp. 1416-1432
Author(s):  
Michael B. Toffolo

Anthropogenic carbonates are pyrotechnological products composed of calcium carbonate, and include wood ash, lime plaster/mortar, and hydraulic mortar. These synthetic materials are among the first produced by humans, and greatly influenced their biological and cultural evolution. Therefore, they are an important component of the archeological record that can provide invaluable information about past lifeways. One major aspect that has been long investigated is the possibility of obtaining accurate radiocarbon dates from the pyrogenic calcium carbonate that makes up most of these materials. This is based on the fact that anthropogenic carbonates incorporate atmospheric carbon dioxide upon the carbonation of hydrated lime, and thus bear the radiocarbon signature of the atmosphere at a given point in time. Since plaster, mortar, and ash are highly heterogeneous materials comprising several carbon contaminants, and considering that calcium carbonate is prone to dissolution and recrystallization, accurate dating depends on the effectiveness of protocols aimed at removing contaminants and on the ability to correctly identify a mineral fraction that survived unaltered through time. This article reviews the formation and dissolution processes of pyrogenic calcium carbonate, and mineralogical approaches to the definition of a ‘dateable fraction’ based on its structural properties.


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