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.

Carbon isotopes are widely used as indicators in the study of atmospheric CO2 variability in space and time. Preliminary results are part of a project investigating 13C and 14C concentration changes during the last 150 yr in Poland, both in industrial and ecologically clean regions, using annual tree rings (Pinus sylvestris, Populus nigra). The results describe the local Suess effect recorded in the industrial Kraków and Upper Silesia regions compared to changes of background radiocarbon concentration caused by global human activity in a “clean region,” Augustów Wilderness. The δ13C record also shows the influence of the local Suess effect.

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.

Hawke's Bay is a region of New Zealand where earliest settlement of indigenous people may have occurred. A sedimentological and palynological study of lake sediments from a small catchment was undertaken to reconstruct erosion, vegetation, and fire histories to determine human environmental impact, and thus add to knowledge of the timing of initial settlement of New Zealand. Precise dating was an essential facet of the research because of the short time span of human occupation in New Zealand. A chronology is proposed based on accelerator mass spectrometry (AMS) radiocarbon dating of palynomorph concentrates. Known-age tephras were used as a check on the validity of the 14C ages obtained using this technique, which is being developed at Rafter Radiocarbon Laboratory. Two episodes of sustained erosion occurred between about 1500 and 1050 BC with a period of ~50 yr at about 1300 BC when no erosion occurred. Five episodes of erosion of very short duration occurred at about 625 BC, 450 BC, 100 BC, AD 950, and AD 1400. Erosion probably resulted from landslides induced by earthquakes or severe storms, with the exception of the last event which coincides with local burning and is probably a consequence of this. A conifer/broadleaved forest surrounded the lake until soon after AD 1075–1300, when a dramatic decline in pollen of forest plants and an increase in charcoal occurred. Forest was replaced by fire-induced scrub, interpreted as a result of anthropogenic burning by prehistoric Polynesians. A further decline in woody vegetation occurred when European-introduced plants appear in the pollen record and extensive pasture was established.

We report on a statistical analysis of a large set of radiocarbon dates for reconstruction of paleoclimate. Probability density functions were constructed by summing the probability distributions of individual 14C dates. Our analysis was based on 2 assumptions: 1) The amount of organic matter in sediments depends on paleogeographical conditions; 2) The number of 14C-dated samples is proportional to the amount of organic matter deposited in sediments in the examined time intervals. We quantified how many dates are required to give statistically reliable results. As an example, 785 peat dates from Poland were selected. The dates encompassed the Holocene and Late Glacial period. All dates came from the Gliwice Radiocarbon Laboratory. Results were compared with other paleoenvironmental records. Detailed analysis of the frequency distributions showed that preferential sampling plays an important part in the shape determination. The general rule to take samples from locations where visible changes of sedimentation are apparent (e.g. from the top and the bottom of the peat layer) results in narrow peaks in the probability density function near the limits of the Holocene subdivision.

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.

New radiocarbon dates obtained from Late Pleistocene and Holocene deposits of the southern, eastern, and northern shores of Lake Baikal in 1995–2001 are presented, and the most important results of paleoenvironmental studies based on C data are discussed. The following paleogeographic events were verified with the help of C dating: 1) first Late Pleistocene glaciation (Early Zyryan); 2) Middle Zyryan interstadial; 3) loess formation during the Late Zyryan (Sartan) deglaciation; 4) warm and cold events in the Late Glacial; and 5) vegetation changes and forest successions during the Late Glacial and Holocene.

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.

Sediment cores were collected from 2 sites in the forested fringe of an oxbow lake surrounded by land that was converted from forest to agricultural use in the late 19th century. The 2 sampling areas were selected to represent areas of high (West site) and low (East site) current sediment accumulation rates, based on distance from a perennially discharging stream. Modern (post settlement and land clearing) sediment accumulation rates were calculated using 210Pb and 137Cs on bulk sediment samples from 2 cores from each site. Two additional cores were collected from each site for radiocarbon analysis of twig cellulose with the assumption that most twigs in the sediment within the forested fringe fell from overhead and are contemporaneous with the sediment. Only the West site, however, yielded sufficient identifiable twig material for analysis. Modern sediment accumulation rates based on 210Pb and 137Cs fall between 0.2–0.4 cm/yr at the East site, and 0.7–1.3 cm/yr at the West site (nearest the stream inlet), with approximate agreement between the 210Pb and 137Cs methods. Modern sediment accumulation rate based on bomb-pulse 14C activity of twigs from cores from the West site is approximately 1.0 cm/yr, in agreement with the 210Pb and 137Cs results. Historic sediment accumulation rates were estimated at the West site using twigs from deeper intervals with pre-bomb 14C activity. Sediment covering approximately 1000 yr of pre-settlement sediment accumulation exhibited evidence of minor bioturbation or in-washing of reworked material, but with a clearly lower accumulation rate of less than 0.1 cm/yr.

Two sediment cores collected from the saline lagoon St. Michiel on Curaçao (Dutch Antilles) preserve a ~5000-yr record of environmental change. Investigation of radiocarbon-dated sections by accelerator mass spectrometry (AMS) is based on faunal assemblage analyses, sediment mineralogy, and the interpretation of sedimentary facies. The cores recovered from different parts of the lagoon demonstrate different development. Initially, in the proximal part of the lagoon (core STM-2), the sediment accumulated in a coastal, semi-protected bay with strong marine influence, whereas the distal part (STM-1) was dominated by chemical precipitation (gypsum, aragonite). By about 3500–3400 BP, connection with the open sea became very limited due to the gradual formation of a coral rubble barrier at the coastline. Subsequently, the record reveals undisturbed sedimentation in the highly restricted shallow lagoon. Around 1100–1000 BP, biological and sedimentological records indicate a change to less evaporitic conditions. Stages of increased salinity are intercalated with intervals of episodic freshening due to increased runoff and precipitation. The authors demonstrate that since permanent human settlements were established on the island about 1100 BP, the watershed has undergone intensive deforestation, especially during the European colonization at the beginning of the 16th century. Deforestation resulting from agriculture and construction caused increased erosion, which was translated to increased sediment accumulation rates and a shift in lagoon sedimentation from almost entirely endogenic to mostly detrital.

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.

This paper examines if an erosive hiatus found in the peat stratigraphy and marsh-accumulation record from northwest Hammock River Marsh (HRM), Connecticut (CT) can be attributed to a 14th or a 15th century hurricane, each documented by a radiocarbon-dated overwash fan in Succotash Marsh (SM) (Rhode Island) about 90 km to the east. Given that (i) the best estimate age range for the 15th century overwash deposit in SM (1400–1440 cal AD, 2 σ) overlaps entirely with that for first plant growth after erosion at HRM (1390–1450 cal AD, 2 σ), while the best estimate age range for the 14th century overwash deposit (1290–1410 cal AD, 2 σ) overlaps just 10 yr, and (ii) interpretation of the available stratigraphic and sedimentary evidence from HRM suggests that a high-energy event offers the simplest explanation for the observed marsh erosion, we conclude that a plausible link exists between the 15th century hurricane and the marsh erosion in HRM. The best estimate age range for the 14th century hurricane appears to overlap for 91% with the age range for the first plant growth (1290–1400 cal AD, 2 σ) following marsh erosion in East River Marsh (CT), located about 12 km west of HRM. These results imply that erosive boundaries in salt-marsh peat deposits have potential as markers of past hurricane activity.

A high-resolution atmospheric radiocarbon record has been obtained for the interval of 17–36 kyr from U/Th-dated aragonite sediment of Lake Lisan. Reservoir age corrections were applied with reservoir ages of 200, 1250, and 2000 yr, which correlate with the different water levels of the lake. The present 14C record for Lake Lisan shows near resemblance with that of Lake Suigetsu: both converge to the value of Δ14C ∼0‰ at 32 kyr cal BP. Both also show significant differences compared to other reported high-resolution 14C records (e.g. Iceland Sea, Cariaco basin, and Bahamas speleothem). This inconsistency should be addressed by re-assessment of the basic assumptions behind the determination of calendar ages of the various records.

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.