In a core off Pakistan, we obtained 38 14C analyses by accelerator mass spectrometry (AMS) from a 4.4-m-thick, expanded, annually-laminated Last Glacial Maximum (LGM) section, bracketed by bioturbated intervals ascribed to the Heinrich-1 (H1) and Heinrich-2 (H2) equivalent events (52 14C analyses between 24–15 kyr BP). A floating varve age scale, anchored to the oxygen isotope record of the layer-counted GISP2 ice core at the H2/LGM boundary, results in an annually dated record for the LGM from 23,450–17,900 cal BP. The floating varve scale of the LGM provides us with a tentative calibration of local marine AMS 14C age dates to calendar years.

Excavations since 1996 in the large El Mirón Cave in the Cantabrian Cordillera of northern Spain have revealed a cultural sequence of late Mousterian, early Upper Paleolithic, Solutrean, Magdalenian, Azilian, Mesolithic, Neolithic, Chalcolithic, Bronze Age, and Medieval occupations. These components have been dated by 51 generally coherent radiocarbon determinations, all run by the Geochron labs, in association with the Lawrence Livermore labs for AMS. This series is one of the largest for a single prehistoric site in Iberia or even Europe. The series is consistent with the record from Cantabrian Spain and provides new detail on the age of the Middle–Upper Paleolithic transition, on the various phases of the Magdalenian culture, on the appearance of the Neolithic in the Atlantic zone of Spain, and on the origins of the socioeconomic complexity in the metal ages. The stratigraphic relationship of 14C-dated levels to a roof-fall block and adjacent cave walls (both with engravings) provides rare terminus post and ante quem ages for execution of the rupestral art in El Mirón during the early to mid Magdalenian. The 14C record has also been instrumental in revealing the existence of depositional hiati during the early Holocene.

A simple method for preparing pollen concentrates for 14C AMS dating is applied to organic and inorganic deposits from a peat bog in south Westland, New Zealand, from which preliminary AMS dating indicated age inversions and severe younger carbon contamination problems. The AMS ages of the pollen concentrates provided consistently older age estimates for each sample than ages derived from their respective organic residue or combined pollen and organic residue fractions. It is likely that the younger age estimates of the organic residue fractions result from the incorporation of younger plant material into the sample and possible contamination from younger humic acids percolating through the site.

The design of FIRI included 3 pairs of duplicate samples: A and B (Kauri wood) near background, D and F (Belfast wood) around 50 pMC, and G and J (barley mash) at 111 pMC. Why include duplicates? Duplicates by their nature allow us to explore the within-lab variability and to assess whether the quoted errors are representative. We can also explore the differences as a function of the sample activity. In this section, we explore the differences between the duplicates. We also consider some different graphical presentations. First, we summarize the differences, then graphically explore the boxplot (to consider the distribution of differences), then a scatterplot of the duplicate pair (to show correlation and reproducibility), and finally, a measure of agreement plot (Bland and Altman 1999). The horizontal axis in this final plot is the mean of the duplicate pair and the vertical axis is the difference in the duplicate pair. Agreement between the pairs would result in the points being randomly scattered around the horizontal zero line.

The issue of comparability of measurements (and thus bias, accuracy, and precision of measurement) from diverse laboratories is one which has been the focus of some attention both within the radiocarbon community and the wider user communities. As a result, the 14C community has undertaken a widescale, far-reaching, and evolving program of intercomparisons, to the benefit of laboratories and users alike. The benefit to the users is, however, indirect, since the 14C intercomparisons have not been used to generate “league tables” of performance, but rather to allow individual laboratories to check procedures and modify them as required.

The historical progression of 14C laboratory intercomparisons from the Third (TIRI, completed in 1995, Gulliksen and Scott 1995) and Fourth (FIRI, completed in 2000, Scott 2003; Boaretto et al. 2000; Bryant et al. 2002) suggests that a Fifth (VIRI) should also be expected. We describe the plans for VIRI.

Pachacamac, covering an area of about 600 hectares (ha) near the Pacific shore, is one of the largest and most important archaeological sites in Peru. Most of the monumental adobe-made buildings of the later pre-Inca period (or Late Intermediate Period, about 10th–15th century AD) are so-called pyramids with ramps (the role of the ramps has been interpreted in different ways). Precise dating of the pyramids appears as a crucial step in defining the functions of Pachacamac in pre-Inca times. In this paper, we present the results obtained from 3 field campaigns at Pyramid III, one of the biggest buildings of the site. A total of 24 radiocarbon datasets from 4 different laboratories will help us to place the various steps of development of Pyramid III on a timescale, defined on the basis of the excavations. More absolute dates are available from another pyramid with ramps, which allow us to make comparisons and propose a new model of interpretation for the Pachacamac site during the Late Intermediate Period (LIP).

Kauri wood, a sub-fossil wood from New Zealand (which had previously been used in an IAEA exercise, IAEA-C4, in 1990), was considered to be an important sample to include in FIRI because it provided a link to previous exercises, was available in sufficient quantity, and was a “close to background” organic sample. IAEA-C4 had previously been criticized since it was believed that in its milling, some contamination had been introduced, so that a replacement sample would prove useful. The Kauri wood has a very low 14C activity and, as such, is very sensitive to even small amounts of contaminant carbon. Such low-activity samples give a true test for the laboratory procedures since pretreatment and laboratory background definition become critical.

Carmi (2002) is a response to our study published in Radiocarbon 43(1) by Rasmussen et al. (2001). We noted widespread possible exposure to castor oil of the Dead Sea Scrolls (DSS) in the Rockefeller Museum in the 1950s and reported experiments showing that the AAA pretreatment used in the first 2 series of radiocarbon datings of the DSS (Bonani et al. [1992] and Jull et al. [1995]), “cannot be guaranteed to have removed all of the modern carbon in any samples if they had been contaminated with castor oil and hence could have produced some 14C dates that were younger than the texts' true ages.” Carmi, a coauthor of the Bonani et al. (1992) study, criticizes our analysis on 4 grounds:

Unleached aliquots of TIRI/FIRI turbidite were analyzed by accelerator mass spectronomy (AMS) over a timespan of 18 months. Individual analyses ranged from 18,090–18,245 yr BP with reported errors between 30–50 yr. The weighted average fraction modern (FM) of these 28 measurements is 0.10378 ± 0.00008 (which equates to 18,199 ± 8 yr BP) and the measurements show a 1 standard deviation scatter of 0.00044 (±35 yr). The fractional error of these results indicates reproducibility of individual measurements at the 4 (1σ) level, which is consistent with the quoted counting-statistics-based errors. Laboratories engaged in the determination of 14C results at reasonably high precision should consider taking advantage of the TIRI and FIRI sample materials in the role of process standards. Additional suites of high-precision data are necessary to refine the accuracy of these sample materials.

Each material needs to be characterized by estimating its activity, which creates a reference value for each material. This value then can be considered as the “known” activity of the material and future analyses can be compared to this to quantify the accuracy of the measurement. In this way, the materials remain useful for laboratory quality assurance.

It is common practice to estimate the age of undated material extracted from a sediment core from radiocarbon or other radiometric dates of samples taken above and below the extracted material. This paper presents a simple expression for the variance of this estimated age. This variance accounts for both 14C dating error and error due to bioturbation.

The radiocarbon content of Japanese cedars was measured by accelerator mass spectrometry for decadal tree-ring samples from the period of 240 BC to AD 900. Conventional gas counting was also used for part of the samples. The data were compared with the INTCAL98 calibration curve (Stuiver et al. 1998). The results indicate that the difference in atmospheric 14C between Japan and North America or Europe is negligible at this period, less than 18 14C yr using an average of 50 yr. However, in the period of about AD 100 to about AD 200, we cannot exclude the possibility of a deviation of the order of 30 to 40 14C yr to the older ages.

As part of the FIRI program, it was recognized that providing samples in sufficient quantity for laboratory procedures is close to ideal and does not represent “typical” conditions. Therefore, laboratories were asked to consider 2 optional studies: investigating the effects of sample size on results and achieving high precision. The sample size study was focused on Sample E, humic acid, which had been chosen because of the rigorous pretreatment it had undergone in the solution stage, and which would ensure sample homogeneity. The precision study was focused on Sample D, the Belfast dendro-dated wood sample, given its importance in the master calibration.

After the first and main phase of FIRI, which focused on routinely measured materials, an optional series of samples were also made available to participating laboratories. This second list included archaeological samples, mammoth tusks, and modern cellulose. Not all samples were available in sufficient quantity for radiometric measurement (in particular, the mammoth tusks). The samples are briefly described in Table 9.1 below.

Coral skeletal radiocarbon records reflect seawater ∆14C and are useful for reconstructing the history of water mass movement and ventilation in the tropical oceans. Here, we reconstructed the inter-annual variability in central equatorial Pacific surface water ∆14C from 1922–1956 using near-monthly 14C measurements in a Porites sp. coral skeleton (FI5A) from the windward side of Fanning Island (3°54′32′′N, 159°18'88′′W). The most pronounced feature in this record is a large, positive shift in the ∆14C between 1947 and 1956 that coincides with the switch of the Pacific Decadal Oscillation (PDO) from a positive to a negative phase in the mid-1940s. Although the absolute ∆14C values from 1950–1955 in FI5A differ from the ∆14C values of another coral core collected from the opposite side of the island, both records show a large, positive shift in their ∆14C records at that time. The relative increase in the ∆14C of each record is consistent with the premise that a common mechanism is controlling the ∆14C records within each coral record. Overall, the Fanning ∆14C data support the notion that a significant amount of subtropical seawater is arriving at the Equator, but does not allow us to determine the mechanism for its transport.

Dating of prehistoric anthropogenic earthworks requires either excavation for archaeological artifacts or macroscopic organic matter suitable for 14C analysis. Yet, the former, in many cases, is undesirable and the latter is difficult to obtain. Here we present a soil science procedure, which has the potential to overcome these problems. It includes careful sampling of buried former soil surfaces, acid-alkali-acid fractionation of soil organic matter (SOM), and subsequent 14C AMS dating. To test the procedure, soil from one of the largest known burial mounds in Scandinavia, Hohøj, and 9 other Danish burial mounds were sampled. The 14C dates from extracted SOM fractions were compared to reference ages obtained by other methods. We show that humic acid fractions in 7 of the 10 mounds had the same age as the reference, or were, at maximum, 280 yr older than the reference ages. The best age estimates were derived from an organic-rich layer from the upper cm of buried soil or sod. Differences among SOM fraction ages probably indicate the reliability of the dating. Hohøj dated to approximately 1400 BC and, thus, was up to 500 yr older than other dated Scandinavian mounds of comparable size. The remaining investigated burial mounds were dated to between 1700 and 1250 BC. We conclude that combined sampling of buried soil surfaces, SOM fractionation, and 14C analysis allows for dating of archaeological earthworks when minimal disturbance is required, or if no macroscopic organic remains are found.

A significant and substantial effort has been made by the 14C community in quality assurance (QA) procedures, of which participation in FIRI is only one part but one that provides an independent and blind check on laboratory performance. The overwhelming willingness to participate is a testament to the importance which laboratories place on quality.

TIRI was officially launched at the 14th International Radiocarbon Conference in Arizona in 1991. Prior to the conference, 150 laboratories received a letter describing the general intention to organize an intercomparison and over 90 laboratories from around the world responded positively to the invitation to participate. Simply stated, the aims of this intercomparison were:

1. 1. To function as the third arm of the quality assurance (QA) procedure.

2. 2. To provide an objective measure of the maintenance and improvement in analytical quality.

3. 3. To assist in the development of a “self-help” scheme for participating laboratories.