Cremated bones are a commonly preserved material and often found in burial environments where unburned bone may not be preserved. As such direct radiocarbon dating of cremated bone could be essential in determining the chronology of an event. Pretreatment of cremated bone exploits the structural carbonate component of the bone which survives cremation. However, due to the low abundance (ca. 0.1%) of this component, the extraction of an amount of endogenous carbon sufficient for radiocarbon dating may represent a challenge. Here we investigate two modifications to the phosphoric acid digestion protocol used during the preparation of cremated bones at the Oxford Radiocarbon Accelerator Unit (ORAU). The first of these was to use ultrasonication to release evolved CO2 from the viscous phosphoric acid and cremated bone mixture that is formed during digestion. The second was to double the amount of time during which evolved CO2 was removed from the reaction vessel by transfer into a cryogenically cooled ampoule. Ultrasonication of the digestion mixture failed to produce a significantly higher carbon yield, while double-time collection resulted in an average 21.5±13.8% increase of C yield without affecting the measured age. Extending the collection time can better enable reliable dating of small (less than 1 g) samples.

Experimental studies have shown that significant carbon exchange occurs between bone-apatite and the pyre atmosphere during cremation, which can cause a calendar date offset between the radiocarbon (14C) event and the date of cremation. There are limited empirical data available to assess the magnitude of such wood-age offsets, but the aim of this paper is to test if they can be modeled statistically. We present new 14C dates on modern bone cremated in realistic open-air experiments and on archaeological samples of cremated bone and associated organic material. Experimental results demonstrate a wide range of carbon exchange with a mean of 58.6 ± 14.8%. Archaeological results indicate that the wood-age offsets have an approximately exponential distribution. We test whether the default Charcoal Outlier_Model in OxCal v4.3, developed to reduce the impact of wood-age offsets in dates of charcoal, is appropriate for cremated bone, but find that it slightly underestimates apparent offsets. To counter the intrinsic age of both pyre fuel and unburned bio-apatite, we instead propose a bespoke Cremation Outlier_Model, which combines an exponential distribution of calendar age offsets with a minimum offset, and provides better estimates of the actual dates of cremations.

This study characterized cremated bone to better understand isotope exchanges during burial, using archeological samples. The cremated bones of Jokei, a Buddhist monk (AD 1155–1213), found in an urn from the Jisho-in Temple, Nara Prefecture, Japan, were used for the analysis. 14C dates were determined for eight of Jokei bone fragments of different colors (black, gray, and white). The white fragments had the highest x-ray diffractometry (XRD) crystallinity index (CI) values (0.89–1.05), Fourier-transform infrared spectroscopy (FTIR) splitting factor values (IRSF) of 5.3–7.1, and the lowest Ba concentrations. The calibrated date of the white bone fragments is 1152–1216 cal AD, consistent with Jokei’s lifespan, showing these fragments yield reliable 14C ages. Meanwhile, the black and gray fragments, which probably experienced lower temperatures during cremation, had lower CI and IRSF values of 0.25–0.46 and 4.2–4.9, respectively, and higher Ba concentrations. The black and gray fragments tended to show unreliable younger 14C dates and higher 87Sr/86Sr values close to the soil value due to soil contamination. The results in this study indicate that it is important to check crystallinity of apatite and soil contamination using chemical indexing methods such as Ba capture, to clarify the reliability of 14C dates for cremated bone samples.

Radiocarbon (14C) results on cremated bone are frequently published in high-ranking journals, but 14C laboratories employ different pretreatment methods as they have divergent perceptions of what sources of contaminants might be present. We found pretreatment protocols to vary significantly between three laboratories (Brussels [RICH], Kiel [KIA], and Groningen [CIO]), which all have a long history of dating cremated bone. We present a case study of 6 sets of replicate dates, to compare laboratory pretreatment protocols, and a further 16 sets of inter-laboratory replicate measurements, which compare specific steps of the conversion and measuring process. The 14C results showed dates to be reproducible between the laboratories and consistent with the expected archaeological chronology. We found that differences in pretreatment, conversion to CO2 and accelerator mass spectrometry (AMS) measurement to have no measurable influence on the majority of obtained results, suggesting that any possible diagenesis was probably restricted to the most soluble ≤5% of each sample, as this proportion of the sample mass was removed under all laboratory protocols.

A comparative study was undertaken to adopt and evaluate a radiocarbon (14C) preparation procedure for accelerator mass spectrometry (AMS) measurements of cremated bones at our laboratory, including different types of archaeological samples (cremated bone, bone, charcoal, charred grain). All 14C analyses were performed using the EnvironMICADAS AMS instrument at the Hertelendi Laboratory of Environmental Studies (HEKAL) and the ancillary analyses were also performed at the Institute for Nuclear Research (ATOMKI). After the physical and chemical cleaning of cremated bones, CO2 was extracted by acid hydrolysis followed by sealed-tube graphitization and 14C measurement. The supplementary δ13C measurements were also performed on CO2 gas while FTIR was measured on the powder fraction. Based on the FTIR and 14C analyses, our chemical pretreatment protocol was successful in removing contamination from the samples. Good reproducibility was obtained for the 0.2–0.3 mm fraction of blind-tested cremated samples and a maximum age difference of only 150 yr was found for the remaining case studies. This confirms the reliability of our procedure for 14C dating of cremated bones. However, in one case study, the age difference of 300 yr between two cremated fragments originating from the same urn shows that other processes affecting the cremated samples in the post-burial environment can substantially influence the 14C age, so caution must be exercised.

This article examines the evidence for fragmentation practices on Middle–Late Bronze Age (c. 1600–700 bc) settlement sites in Ireland by looking at two kinds of material: human remains, both burnt and non-burnt, and quern stones. It highlights evidence for the manipulation of non-burnt skulls through ‘de-facing’ and the potential retention of cranial and other fragments for ‘burial’ in settlements. It also explores the more difficult task of determining whether incomplete skeletal representation in cremated remains can be interpreted as deliberate fragmentation, and how the context of deposition must be considered. Human agency in relation to the fragmentation patterns of querns is also examined to understand whether the act of breaking these objects was intentional or unintended and if depositing them was symbolic or simply fortuitous. By discussing this evidence, I hope to contribute to the argument that the funerary and settlement spheres in later prehistoric Ireland were becoming increasingly intertwined.

In the late 1990s, it was demonstrated that reliable radiocarbon dates could be obtained directly from cremated bone. Many 14C laboratories have since used a protocol for pretreating cremated (calcined) bones that consists of consecutive treatments with bleach and acetic acid to remove organic matter and extraneous or diagenetic carbonate, respectively. In most instances, the bleach used is sodium hypochlorite, although in recent years the Oxford Radiocarbon Accelerator Unit (ORAU) has used acidified sodium chlorite instead. However, properly calcined (white) bones should not contain any organic material; hence, the bleach treatment is potentially unnecessary. This article describes studies investigating the effectiveness of bleach (and the specific bleach used) during pretreatment of calcined bone, and demonstrates that 14C dates on six cremated bone samples are statistically indistinguishable whether or not the initial bleach step is applied.