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    Over the last 40 years, there has been a discernible increase in the number of scholars who have focused their research on early industrial organizations, a field of study that has come to be known as Archaeotechnology. Archaeologists have conducted fieldwork geared to the study of ancient technologies in a cultural context and have drawn on the laboratory analyses developed by materials scientists as one portion of their interpretive program.

    Corroded iron from the Java Sea Wreck. Chinese Warring States arrowhead dating to about — B. A wrought-iron Roman cleaver. Large spear from Burkino Faso, Africa. Paperweight made by reworking iron from the Himeji Castle in Japan. In this article, an overview is presented of the status of the radiocarbon dating of iron-based materials. Recent advances include simplification in sample preparation and reduction in sample size for accelerator mass spectrometry measurements, and the potential use of rust as a viable source of material for radiocarbon dating.

    Additionally, a summary is presented of all 63 previously published results for iron-based materials and 29 new results that have not been published previously. These materials range from low-carbon wrought irons to medium to very high-carbon steels and cast irons. Artifact dates range from several hundred years ago to several thousand years ago.

    Brief descriptions are given of some of these examined samples to illustrate issues and complexities that can arise in determining the age of iron-based carbon materials using radiocarbon dating. A recent summary has been published 1 of techniques for dating that range from astronomical methods to cover time scales from the age of the universe e. One well-known method for dating is based on the use of isotopic techniques.

    Included are reactions such as the uranium-to-lead transformation utilized for dates that range from 1 billion years to 4. Perhaps the best-known isotopic technique, however, is that of radiocarbon [e. The present paper deals with an issue of great interest to materials scientists and archeologists—the dating of iron-based materials that contain carbon.

    In addition, however, the corrosion products or rust from these materials is included since they can also be used for dating in some cases. For the case of iron-based materials, the time span of interest is from the start of the Iron Age in the regions of interest about B. The most appropriate method for this time span and group of materials is 14C dating.

    It is key to point out that the usefulness of the method of dating carbon in iron-based materials relies on the source of the carbon found in the materials see sidebar.

    For the case of iron-based materials, van der Merwe and Stuiver 2 first demonstrated that it was feasible to extract the carbon from different iron-based materials and use it to establish their age using radiocarbon dating. A total of 15 samples of iron-based materials were dated by beta counting at Yale University 23 using a dependable method to extract carbon from iron utilizing flow-through combustion in oxygen with cryogenic trapping of CO2.

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    These studies showed that in a wide range of cases, the carbon in iron-based materials could be extracted and reliably radiocarbon dated. The Yale beta counter, however, required significant amounts of carbon compared to the amounts that were usually available from artifacts without consuming or damaging them.

    The amount of carbon required was 1g, equivalent to 50 g of a 2. In the late s, radiocarbon dating by accelerator mass spectrometry AMS became common.

    This new methodology required only 1 mg instead of 1 g of carbon. Inthe present authors published 9 a new carbon-extraction method for iron based on a sealed-tube combustion with CuO in quartz. This greatly simplified the previous technique and required only materials readily available in the standard AMS graphite-preparation laboratory: Unlike the previous techniques, no exotic gas-trapping equipment is required.

    Thus, over the years, the sample-size requirement has been greatly reduced and the carbon-extraction procedure has been simplified. However, as has been mentioned, for a radiocarbon date on iron to be meaningful, the carbon extracted from the iron-based material must be from biomass contemporaneous with original manufacture.

    In addition to fossil fuels such as coal and coke, other carbon sources such as geological carbonates e. Complications arising from the recycling of artifacts must also be considered. These limitations of the dating technique have been well summarized by van der Merwe 3 and Cresswell. If rust can be dated reliably, it opens up a large number of possibilities for dating iron artifacts.

    Investigators will not need to cut into valuable artifacts for clean metal, but will be able to use surface corrosion products.

    This potentially opens the way for dating precious samples such as the iron plate found in the Great Pyramid at Gizeh, 1011 now at the British Museum.

    It may also be possible to date completely rusted artifacts, commonly found in waterlogged early Iron-Age sites in Europe and in underwater shipwrecks.

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    Previous investigators had been careful to remove rust from iron prior to dating for fear that it adds contamination. A key issue though, is whether any of the original carbon remains within the matrix of rust and other corrosion products. If not, rust and similar materials are clearly of no interest for radiocarbon dating and should probably be removed since, at best, they can do no good.

    However, if original carbon is present, the corrosion products themselves may be appropriate targets for dating, subject to solving the potential contamination problems. Most of the carbon in iron-based materials is in the form of the orthorhombic, crystalline iron carbide Fe3C known as cementite.

    Morphologically, cementite appears either as spheroidized particles or as pearlite. For compositions exceeding the eutectoid level of about 0.

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    The thickness and sizes of all of these carbides can vary enormously, depending upon composition and heat-treatment history. For steels that have been quenched to form martensite body-centered tetragonal structurethe carbon is essentially in solid solution in the iron up to the eutectoid composition, beyond which it too will usually be in the form of carbides. Despite the complex range of possible amounts and morphologies of the cementite, the thermodynamic stability of iron carbide is significantly greater than that of iron.

    So, as iron rusts, the carbide phase will be more stable than the matrix and will remain behind. The question then becomes one of kinetics: How long will it take for the carbide to oxidize compared to the iron matrix? As long as the carbon remains in the rust, in whatever form, it will potentially be available for radiocarbon dating.

    Although little appears to have been published on this subject, Knox 12 reported the detection of iron carbide in the remaining oxide from a corroded 2,year-old Iranian steel dagger. The present authors and van der Merwe 14 have recently completed a study in this area.

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    This work provides some evidence for the reliability of dating corrosion products from artifacts that have rusted in the air, in the ground, and under water, although it does not prove that all such samples can be successfully dated.

    Nonetheless, iron samples that had completely rusted produced plausible radiocarbon dates, but issues of contamination and post-depositional carbon exchange must be thoroughly tested in a variety of field settings before rust dating can be considered a validated technique.

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    What the study does show, then, is that there is no a priori reason why the method should not work on rust.

    The work suggests that accurate radiocarbon dates may be obtainable with minimal material and with minimal risk to artifacts. Artifacts are designated as follows: Weight percent carbon vs. This table provides sample identification, radiocarbon years Before Present [B.

    This nomenclature is used in radiocarbon dating to avoid the variation introduced by calibration charts that convert radiocarbon years B. Sincea wide range of iron-based materials have been investigated Figures abcdand e. The determined ages range from relatively recent materials B. Sample sizes range from less than 0. Sample conditions range from clean metal to rusty metal to very corroded metal.

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    The nuances of radiocarbon dating of iron-based materials will be explained by way of example in this paper.

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