A vacuum sample processing line was set up and methods were developed for the determination of radiocarbon in small-volume seawater and biota samples. Seawater samples (500 mL per borosilicate glass bottle and poisoned with HgCl2) were acidified with 5 mL concentrated hydrochloric acid. Pure N2 was used as a carrier gas to strip CO2 from the samples for 10 min in a circulation mode. After purification through several water traps, the CO2 was isolated cryogenically. Using Na2CO3 standard solutions, recovery yields were calculated superior to 95 ± 5%. Freeze-dried marine biota samples were thoroughly mixed with Cu(II)O and combusted at 900°. The CO2 was purified by passing through Ag wool and Cu granules at 450° before reduction to graphite. Finally, graphite was synthesized using Zn dust heated to 450° in the presence of an Fe catalyst at 550°. Although this method takes about 8 hr (synthesis done overnight), the advantage is that no water vapor by-product is formed to hinder the reaction. The graphite yields, measured both by gravimetric methods and by pressure readings, were 95 ± 5%. Accelerator mass spectrometry (AMS) measurements were carried out at the NSF-Arizona AMS Facility. Results for water samples from the northwest Pacific Ocean are reported which are in agreement with data reported elsewhere.

While it is customary to use solid samples for measuring the 14C/12C ratio, it is sometimes necessary to handle liquid or gas samples. Motivated by a scientific purpose to count radiocarbon yields in deuterated acetone irradiated with energetic neutrons, we developed a new combustion system to treat liquid or gas samples. In contrast with the typical combustion system using CuO for solid samples, the new combustion system uses high-purity O2 (99.999%) gas. As an initial investigation, we combusted deuterated acetone (acetone-d6, certified 100.0 atm % D) to make CO2 under the ambient O2 pressure. The resulting CO2 gas then went through the reduction process to form graphite for further accelerator mass spectrometry (AMS) measurement.

Two pretreatment methods for accelerator mass spectrometry (AMS) dating of insect remains were explored. One method involves a simple acid wash that removes carbonate, while the other is based on the industrial purification of chitin and results in isolation of polymeric chitosan. No contamination is observed from Maillard reactions during the deacetylation reaction used to isolate the chitosan. The methods were tested on Coleoptera samples from two Roman Britain sites. Our results demonstrate that both methods produce acceptable AMS dates that correspond well to the expected age of the deposits from which they came.

Bone is one of the most widely used materials for dating archaeological activity. It is also relatively difficult to pretreat effectively and new methods are an area of active research. The purpose of the chemical pretreatment of bone is to remove contaminants present from burial and to do so in a way which does not add any additional laboratory contaminant. To some extent, these two aims must be balanced since, on the whole, the more complex the procedure and the more steps included, the greater the chance for contamination. At the Oxford Radiocarbon Accelerator Unit (ORAU), the method used is a continuous-flow or manual acid/base/acid (ABA) treatment followed by gelatinization and ultrafiltration (based on Brown et al. [1988]; documented in Bronk Ramsey et al. [2000]). We find this overall method is very effective at removing more recent contamination in old bones. However, two aspects of the method have recently been improved and are reported here: the redesign of ORAU's continuous flow pretreatment and a new protocol in our pretreatment ultrafiltration stage.

We present a brief discussion of sample preparation procedures at the Keck Carbon Cycle Accelerator Mass Spectrometer (KCCAMS), University of California, Irvine, and a systematic investigation of the use of Mg(ClO4)2 as an absorptive water trap, replacing the standard dry ice/ethanol cold finger in graphite sample preparation. We compare high-precision AMS measurement results from oxalic acid I and USGS coal samples using Mg(ClO4)2 under different conditions. The results obtained were also compared with those achieved using the conventional water removal technique. Final results demonstrate that the use of Mg(ClO4)2 as an alternative water trap seems very convenient and reliable, provided the Mg(ClO4)2 is replaced frequently.

One problem in preparing iron for radiocarbon dating is the low carbon content which makes the sample size needed too large for some sample combustion systems. Also, the metallic character of the samples complicates sample combustion or oxidation. The Erlangen accelerator mass spectrometry group uses an elemental analyzer for the sample combustion, directly followed by a reduction facility. As the carbon content and sample size for iron samples are unsuitable for combustion in an elemental analyzer, 2 alternative approaches are to (a) avoid oxidation and reduction, or (b) extract the carbon from the iron, prior to combustion. Therefore, 2 different pathways were explored. One is direct sputtering of the unprocessed iron sample in the ion source. The other is the complete chemical extraction of carbon from the iron sample and dating of the carbonaceous residue. Also, different methods for cleaning samples and removing contamination were tested. In Erlangen, a Soxhlet extraction is employed for this purpose. Also, the sampling of the iron sample by drilling or cutting can be a source of contamination. Thus, the measurement of iron drill shavings yielded ages that were far too high. The first results for iron samples of known age from 2 archaeological sites in Germany are presented and discussed.

This work focuses on the preparation and dating of sporomorph (pollen and spores) concentrates of high purity. Three sediment cores recovered from Lake Baikal within the EU-Project CONTINENT were subjected to palynological analyses and accelerator mass spectrometry (AMS) radiocarbon dating. Laboratory processing of concentrates was aimed at the removal of non-sporomorph organic matter by means of chemical treatment, micro-sieving, and heavy liquid separation. The obtained concentrates were checked under the microscope and sample purity was estimated on the basis of particle counts. The results of AMS 14C dating show differences in the sedimentation rate among 3 sites of Lake Baikal.

Progressive dissolution experiments were performed on samples of ostracode shells from lacustrine sediments from the western Great Basin to remove contamination of the surface by secondary calcite. The observed age differences between the external and residual fractions were as great as 2000 to 6000 yr. A “plateau” in ages of the last fractions was obtained only for 1 sample; however, results of repeated experiments resulted in very good agreement of the final ages. A comparison with previously published chronologies based on bulk radiocarbon ages of ostracodes from Wilson Creek (Benson et al. 1990) shows that leaching is imperative for dating samples older than 20 ka B P. This study focuses on the problem of contamination and its removal. However, the final chronology of the Wilson Creek Formation (and other late Pleistocene lacustrine sediments) will require additional dating of other sections as well as establishment of a reservoir effect correction.

Radiocarbon is produced within minerals at the earth's surface (in situ production) by a number of spallation reactions. Its relatively short half-life of 5730 yr provides us with a unique cosmogenic nuclide tool for the measurement of rapid erosion rates (>10−3 cm yr−1) and events occurring over the past 25 kyr. At SUERC, we have designed and built a vacuum system to extract 14C from quartz which is based on a system developed at the University of Arizona. This system uses resistance heating of samples to a temperature of approximately 1100° in the presence of lithium metaborate (LiBO2) to dissolve the quartz and liberate any carbon present. During extraction, the carbon is oxidized to CO2 in an O2 atmosphere so that it may be collected cryogenically. The CO2 is subsequently purified and converted to graphite for accelerator mass spectrometry (AMS) measurement. One of the biggest problems in measuring in situ 14C is establishing a low and reproducible system blank and efficient extraction of the in situ 14C component. Here, we present initial data for 14C-free CO2, derived from geological carbonate and added to the vacuum system to determine the system blank. Shielded quartz samples (which should be 14C free) and a surface quartz sample routinely analyzed at the University of Arizona were also analyzed at SUERC, and the data compared with values derived from the University of Arizona system.

We have AMS dated samples of Pacific rat (Rattus exulans) bone “collagen” and filtered gelatin samples from the prehistoric site of Shag River Mouth, New Zealand. The age of occupation of this site has previously been determined based on 50 radiocarbon measurements. The site dates to the late Archaic phase of southern New Zealand prehistory (about 650–500 BP; 14th–15th century AD). The results of rat bones which we have dated produce a range in ages, from about 980–480 BP, a difference we attribute to a combination of effects. Pretreatment appears to be an important variable, with results showing differences in 14C age between the progressive “collagen” and filtered gelatin chemical treatment stages. Amino acid profiles suggest there is a proteinaceous but non-collagenous contaminant which is removed by the more rigorous pretreatment. Stable isotopes vary between pretreatments, supporting the removal of a contaminant, or contaminants. Variation in δ15N values imply a range in uptake of dietary protein, and might suggest a potential influence from the local aquatic environment or the consumption of marine-derived protein. Rats are opportunistic, omnivorous mammals, and, therefore, obtain carbon from a variety of reservoirs and so we ought to expect that in environments where there is a variety of reservoirs, these will be exploited. Taken together, the results show that rat bone AMS 14C determinations vary in comparison with the established age of the site, but are in notably better agreement with non-collagenous data than in previously published determinations (Anderson 1996).

We have developed a prototype carbon extraction system for accelerator mass spectrometry (AMS) radiocarbon dating of archaeological iron remains by combusting them with a RF induction furnace. We have also successfully tested and used a method of carbon extraction from iron using a CuCl2 solution. Modifications to our carbon extraction systems and methods provide us acceptable performances; carbon yield is normally around 80% and the 14C background level is as low as 42–48 ka BP in 14C apparent age. We have also conducted an iron refining experiment to examine the sources for carbon 14C age derived from iron, using established AMS 14C dating and carbon extraction systems. Our refining experiment was conducted on iron slag, which are by-products formed during iron smelting methods in the 7th century AD, and using modern charcoal as fuel. The aim of the experiment was to determine whether original carbon characteristics in the original iron materials would be preserved, or if the carbon signature would be replaced to some degree by the modern charcoal. AMS 14C measurements on the refined iron yielded 14C ages equivalent to those of the modern charcoal fuel. The result indicates that the original carbon signatures in the iron slag from 7th century production was replaced completely by modern carbon used in our experiment. The experiment confirms the assumption that 14C ages on iron products are associated with the fuel source of the iron smelting or refining process. We also report on the dating of iron slag materials excavated from the Gennaitouge iron smelting site, where 14C dates were consistent with the age of the site estimated by archaeological evidence.

A representative selection of Roman and Coptic textiles is used to compare the radiocarbon dating results with the chronology proposed by art historians. In some cases, the comparison was made on individual objects, but in other cases, groups of stylistically and/or technologically related textiles were compared. In the case of the latter, the interquartile range was calculated. The results of this comparison show that some individual samples and groups are dated older than expected, while for another group the opposite is the case. One group was matching well with the presumed period as a whole, but not on the basis of the individual pieces. The analyses showed the necessity of 14C dating to obtain a more accurate dating of Coptic textiles.

The results of radiocarbon dating of several Late Neolithic archaeological sites in Slavonia, eastern Croatia, are presented. According to the archaeological findings, the sites belong to the Sopot culture. Stages I-B, II-A, II-B, and III were identified at the eponym site Sopot near Vinkovci, stages I-B and II at the site Dubovo-Košno near Županja, while findings for other investigated sites (Herrmann's Vineyard near Osijek, Mandek's Vineyard from Otok, Privlaka near Vinkovci, and Slavča near Nova Gradiška) were placed to phases II and III. 14C results place the I-B stage to the period 5480–5070 cal BC, stage II-A to 5030–4770 cal BC, stage II-B to 4800–4250 cal BC, and phase III to 4340–3790 cal BC. These dates were compared to those obtained for other Late Neolithic cultures in the Pannonian Valley. The results confirmed the Protolengyel character of Sopot culture.

We reconstructed climate change during the second half of the Holocene for the Minusinsk (southern Siberia) and the Uyuk (Central Asia) valleys in the Eurasian steppe zone. Sediment cores from 2 lakes and a soil profile from the Arzhan-2 burial mount were investigated. We combined pollen and geochemical analyses and radiocarbon dating with the archaeological record. A sharp increase of human population density occurred at the transition from the Bronze Age to Iron Age (about 2700 cal BP). The most representative Scythian culture started in the Uyuk and the Minusinsk valleys after increased humidity and occupation capacity of the steppe zone during the 9th century BC.

The first radiocarbon dates from the unique early Scythian monument Arzhan-2, discovered in 2001, are presented. The monument contained a royal burial (grave nr 5). Unfortunately, precise dating is hampered by the Hallstatt plateau in the calibration curve. However, using both accelerator mass spectrometry measurements from buried materials and conventional dates for floating tree rings from the burial chamber, we were able to date the construction of the monument to the 7th century BC. This is consistent with archaeological expectations. Other graves located inside the barrow were also dated. Grave nr 11, located on the edge of the barrow, is younger, showing that the monument was a place of burial ritual for many years for this ancient population.

Radiocarbon measurements on a partially articulated female human skeleton, recovered from the foreshore of the river Thames in London, raised interesting questions of interpretation when the body did not produce the anticipated Neolithic date. A relatively recent 14C age and a strong marine component to the individual's diet, identified by stable isotope measurements, means that the date of death is difficult to estimate accurately, although the body probably does not constitute a forensic case.

A previous radiocarbon dating and stable isotope study of directly associated ungulate and human bone samples from Late Mesolithic burials at Schela Cladovei in Romania established that there is a freshwater reservoir effect of approximately 500 yr in the Iron Gates reach of the Danube River valley in southeast Europe. Using the δ15N values as an indicator of the percentage of freshwater protein in the human diet, the 14C data for 24 skeletons from the site of Lepenski Vir were corrected for this reservoir effect. The results of the paired 14C and stable isotope measurements provide evidence of substantial dietary change over the period from about 9000 BP to about 300 BP. The data from the Early Mesolithic to the Chalcolithic are consistent with a 2-component dietary system, where the linear plot of isotopic values reflects mixing between the 2 end-members to differing degrees. Typically, the individuals of Mesolithic age have much heavier δ15N signals and slightly heavier δ13C, while individuals of Early Neolithic and Chalcolithic age have lighter δ15N and δ13C values. Contrary to our earlier suggestion, there is no evidence of a substantial population that had a transitional diet midway between those that were characteristic of the Mesolithic and Neolithic. However, several individuals with “Final Mesolithic” 14C ages show δ15N and δ13C values that are similar to the Neolithic dietary pattern. Provisionally, these are interpreted either as incomers who originated in early farming communities outside the Iron Gates region or as indigenous individuals representing the earliest Neolithic of the Iron Gates. The results from Roman and Medieval age burials show a deviation from the linear function, suggesting the presence of a new major dietary component containing isotopically heavier carbon. This is interpreted as a consequence of the introduction of millet into the human food chain.

A review of the radiocarbon chronology of some late Upper Pleistocene mammals from Siberia is presented. Previously published data has been supplemented by new 14C dates for 5 species (woolly mammoth, woolly rhinoceros, bison, horse, and muskox) to reconstruct chronological extinction patterns. The final extinction of woolly rhinoceros and bison in Siberia can be dated to approximately 11,000–9700 BP, but some megafaunal species (woolly mammoth, horse, and muskox) survived into the Late Holocene, about 3700–2200 BP.

This article reports on 12 new accelerator mass spectrometry (AMS) dates from the latest phases of the Chalcolithic period occupation (late 5th millennium cal BC) at Teleilat Ghassul, type site for the south Levantine Ghassulian Chalcolithic culture. The new AMS dates from Teleilat Ghassul favor an amendment to a previous suggestion (Bourke et al. 2001), that all significant occupation at the site had ceased by 4000/3900 cal BC. This end-date should now be amended to 3900/3800 cal BC. Follow-up statistical modelling sourced to published 14C data drawn from a wide selection of south Levantine Chalcolithic period sites (Bourke 2001; Burton and Levy 2001) raises the possibility that Chalcolithic period occupation had ceased at virtually all major centers by 3800/3700 cal BC. This, in turn, suggests that the new data bearing on the end-date for occupation at Teleilat Ghassul may reflect a more widespread horizon of abandonment in the southern Levant.

The eruption of the volcano at Thera (Santorini) in the Aegean Sea undoubtedly had a profound influence on the civilizations of the surrounding region. The date of the eruption has been a subject of much controversy because it must be linked into the established and intricate archaeological phasings of both the prehistoric Aegean and the wider east Mediterranean. Radiocarbon dating of material from the volcanic destruction layer itself can provide some evidence for the date of the eruption, but because of the shape of the calibration curve for the relevant period, the value of such dates relies on there being no biases in the data sets. However, by dating the material from phases earlier and later than the eruption, some of the problems of the calibration data set can be circumvented and the chronology for the region can be resolved with more certainty.

In this paper, we draw together the evidence we have accumulated so far, including new data on the destruction layer itself and for the preceding cultural horizon at Thera, and from associated layers at Miletos in western Turkey. Using Bayesian models to synthesize the data and to identify outliers, we conclude from the most reliable 14C evidence (and using the INTCAL98 calibration data set) that the eruption of Thera occurred between 1663 and 1599 BC.