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Here we extend radiocarbon dating to lead carbonate, an inorganic material. We demonstrate that lead carbonates can be dated. We also show that natural and manufactured make-up powders can be discriminated by radiocarbon. We find that cerussite used for cosmetics was a natural mineral during the Egyptian Kingdom and then a synthesized compound manufactured by the ancient Greeks. Furthermore, we confirm that phosgenite was artificially produced by the Egyptians about years ago.
Our results confirm the expertize of ancient Egyptians and Greeks in the chemical synthesis of cosmetics. The detection of radiocarbon in lead carbonate holds great promise for art history and provides a new tool for the authentication of paintings by dating the lead white pigment. The development of the radiocarbon method has had a profound impact on archeology as it enables the dating of the remains of ancient civilizations.
The method is usually applied to organic materials – wood, charcoal, bone, etc. However, a few studies have shown that radiocarbon dating can also reveal the age of inorganic manufactured materials. As early as the s, 14 C dating was extended to building materials 1. In particular, mortar which incorporates atmospheric carbon dioxide as it hardens, has been extensively studied and used to date churches and Roman buildings 2 , 3.
More recently, the direct dating of iron was successfully achieved by combining chemical analysis and radiocarbon measurement. During the manufacture of the iron alloy, carbon from charcoal combustion is incorporated by diffusion into the metal and forms cementite Fe 3 C 4. This approach has shed new light on the technical skill and intentions of cathedral builders in Europe 5 and on the chronology of the Angkor temples in Cambodia 6.
Lead carbonates were used as ingredients in paint and cosmetics. Lead white, a mixture of cerussite PbCO 3 and hydrocerussite Pb 3 CO 3 2 OH 2 , was the most important of all white pigments until the nineteenth century 7. Lead carbonates were also employed as cosmetics from Antiquity to the eighteenth century 8 , 9. They were used by ancient Egyptians, Greeks, and Romans 10 , 11 , 12 , 13 , 14 , Understanding the synthetic process of cosmetics production in Antiquity is of great interest for human history and for our knowledge of the development of chemical techniques.
Here we demonstrate the ability of radiocarbon to date archeological and historical lead carbonates and to discriminate natural and synthesized cosmetics. Based on a purposely designed protocol Methods , radiocarbon measurements are performed on ancient Egyptian and Greek make-up held at the Louvre museum. As they are considered as the earliest synthesized cosmetics, the application of the radiocarbon method is highly meaningful not only to date the compound but also to determine its natural or artificial origin.
We show that atmospheric carbon dioxide was incorporated in some lead carbonates during their synthesis. In this way, the radioactive isotope 14 C was fixed in the mineral matrix through the carbonate ion and decayed in time after its incorporation, making radiocarbon dating possible. To our knowledge, this study presents the first absolute dating of lead carbonate. We provide a tool to directly date lead carbonate-based materials such as ancient cosmetics and paintings.
Recrystallization of lead carbonate in cosmetics or paintings is unlikely to be problematic for radiocarbon dating as for other carbonates such as shells and some mortar due to lack of exposure to water. We also show that the quantity of radiocarbon 14 C is the criterion of choice to discriminate natural and synthesized lead carbonates. The results give new insight into the production of white make-up powders in Antiquity and confirm the expertize of ancient Egyptians and Greeks in chemically synthesizing lead carbonate make-up.
To highlight the novelty of our approach we report here results obtained on well-preserved Egyptian and Greek ancient cosmetics. They are held at the Louvre museum in their original containers in wood, reed or alabaster Fig. The cosmetics were selected on the basis of their known archeological context and chemical composition.
These two compounds were pure or mixed together or associated to other lead minerals: Galena is an abundant natural mineral, widely distributed in various environments. On the contrary, laurionite and phosgenite are very rare in nature and are considered as the earliest synthesized cosmetics Cerussite exists as a natural mineral, but has also been manufactured. Natural cerussite is found in the oxidation zone of lead deposits.
Egyptian and Greek make-up from the Louvre museum collection. It was preserved in a small box found in a tomb discovered in Eretria Greece. This tomb was dated on a numismatic basis from ca to ca BC The other four powders are mainly composed of phosgenite and were placed in four distinct channels of a wooden cylinder E , Fig. This date is consistent with the numismatic result and in agreement with two previous radiocarbon dates measured on an almond seed AGER-CA from the same tomb 21 Fig.
Radiocarbon dating of a Greek cerussite make-up powder. The radiocarbon dates of the four phosgenite Egyptian powders E are between and calBC Fig. The powders are preserved in four distinct channels of the container and do not have exactly the same composition The relative scatter on the dating results may suggest different production periods.
However, we have to keep in mind that the date obtained on the wood might not accurately reflect the period of use due to the inbuilt effect as well as a possible material reuse due to the scarcity of wood in Ancient Egypt The container may have been carved from reclaimed wood that had previously been used for other purposes. Calibrated radiocarbon dates of Egyptian make-up. Four phosgenite powders and their wooden container are dated from to calBC. This large range can be due to the fact that the four powder samples may not have been manufactured from the same batch since they are preserved in four distinct channels of the container.
The fact that the measured radiocarbon dates of these cosmetics match with the expected dates is strong evidence that atmospheric carbon dioxide was incorporated at the time of formation of the lead carbonates and that the carbonate formation occurred in a period close to that of the use of the cosmetics. Through the absorption of CO 2 , the radioactive isotope 14 C was fixed in the carbonate ion, and decayed over time. The present radiocarbon content of the phosgenite samples ranges from The mean value of the four samples The radiocarbon measurements thus provide two key results: As galena, laurionite, and anglesite do not contain carbon, the radiocarbon measurements concern phosgenite and cerussite exclusively.
The two samples containing galena and cerussite give dates from to calBC. As they are much older than the expected age — BC , these results evidence a natural origin of the Egyptian cerussite. Cerussite is abundant in nature as a secondary mineral formed by the natural weathering of galena exposed to air or water The measured radiocarbon dates thus correspond to its in situ formation about 10 kyears ago and indicate that these cosmetics are composed of a natural association of galena and cerussite.
The radiocarbon dates of the five samples containing galena, cerussite and phosgenite are also older than expected, but to a significantly lesser extent — calBC. We interpret this result to mean an intentional combination of natural cerussite associated to galena with synthetic phosgenite. Radiocarbon measurements on ancient cosmetics provide two key results: Our results show two distinctive cases: In the first case, for the cosmetics composed of a mixture of cerussite and galena, radiocarbon dates give ages that are too old.
This result is the fingerprint of a natural cerussite since geological carbonates contain very low amounts of 14 C. Cerussite is a common alteration product of galena, associated to secondary minerals and other carbonates in oxidized zones of deposits. The weathering of galena exposed to air and water involves the formation of anglesite. In presence of calcareous soil or carbonated water, cerussite is also found.
Galena deposits in Egypt occur mainly along the Red Sea coast The site of Gebel el-Zeit was one of the main mines exploited in Antiquity The mines are located on the calcareous slope of the wadi and in the superficial zones, galena is partially transformed into cerussite Minerals containing galena and secondary minerals were collected at this period and used as cosmetics without chemical transformation.
The color, from black to light gray, was probably adjusted by selecting various mineral blends, depending on the proportion of black galena and grayish natural cerussite and anglesite. White powder was thus difficult to obtain and it became necessary to search for pure white compounds. Phosgenite is a solid white powder. Its presence is observed in the cosmetics as pure or mixed with galena and cerussite.
Very few occurrences of natural phosgenite are reported. Contrary to lead carbonates and lead sulfates, phosgenite is, like all minerals of lead and chlorine, soluble and does not accumulate in the oxidized zones of lead deposits To obtain large quantities of pale powder, the production of an artificial white was thus required.
The first evidence that phosgenite was chemically synthesized by ancient Egyptians was reported twenty years ago This statement was based on the small abundance of these minerals in nature, on ancient recipes and on their replication in modern laboratories. Here, by using radiocarbon, we provide an absolute method to directly identify a synthetic process for phosgenite.
Dioscorides in the second half of the first century AD reported a recipe involving lead oxide, salt, and white soda to produce a white compound 19 , 32 the corresponding chemical compounds are indicated in brackets:. Successful replication of this recipe showed that phosgenite is obtained after many repetitive operations 15 , The first step in the recipe is to form laurionite by stirring PbO litharge with NaCl salt: When carbon dioxide is added in the solution, the chemistry of lead oxychloride is altered and phosgenite forms The CO 2 g provides the radioactive isotope 14 C used for dating the cosmetics.
According to our results, the carbon dioxide used to manufacture phosgenite is of atmospheric origin. In the recipe, CO 2 g is produced by the dissolution of natron in water.
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Thanks to thermoluminescence, it is possible to differentiate authentic excavated items from recently manufactured fakes with reasonable accuracy. How do you know when a work of art was painted? Unfortunately there are no affordable direct methods for dating pigments, except in some cases as we will see later. For instance, it is possible to date the wood support of a panel as well as canvas. The three most important dating techniques which are useful for the analysis of works of art are: Thermoluminescence dating is used for pottery. It dates items between the years , BP before present. Thermoluminescence dating is generally not very accurate. One way to pass a fake through a TL test is to expose the newly-made pottery to a high dose of artificial radiation sources, thus fooling the measurement instruments.
Resources for the post were mainly Wikipedia, ColourLex. These minerals were crushed, ground into powder, and then mixed with a quick-drying binding agent, such as egg yolk tempera painting.
The initial chronological hypotheses Henri Breuil and Denis Peyrony established an association with the Gravettian. For Breuil, the chronology of Palaeolithic parietal art depended on the existence of two cycles: He drew parallels between Lascaux and the painted figures found in stratigraphy — and thus reliably dated — at the Labattut Perigordian and Blanchard Aurignacian shelters.
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