The article, which was prepared by three of the most prestigious AMS laboratories, is available to the general public on the web www. Together with public television [ 39 ], it is helping to create a broad awareness and understanding of the nature and importance of the AMS measurement capability. Secondly, because of controversy surrounding the meaning of the radiocarbon result, measurement aspects of artifact dating have been given intense scrutiny. Such scrutiny is quite positive, for it gives the possibility of added insight into unsuspected phenomena and sources of measurement uncertainty.
The Turin Shroud is believed by many to be the burial cloth of Christ. The documented record, however, goes back only to the Middle Ages, to Lirey, France ca. The Shroud image, considered by some to be the skilled work of a mediaeval artist, shows a full length image of a crucified man; but as a negative image [ Fig. The unique herringbone twill [ Fig. Shown in the montage are: Apart from sampling, 10 the AMS measurements were performed taking the strictest quality control measures. Three highly competent laboratories were selected: Samples of the Shroud, plus three control samples of known age, were distributed blind to the three laboratories.
Control of this operation distribution of samples, collection of results was the responsibility of Michael Tite of the British Museum. The accuracy and precision of the interlaboratory data for the control samples were outstanding, leaving no doubt as to the quality of the AMS measurement technique Fig. Sample-1 Shroud results, however, were just marginally consistent among the three laboratories, prompting the authors of Ref. The transformation is shown in Fig. In addition, an interesting link exists between this figure and Fig. A comparison of the two figures shows that the radiocarbon date BP , near the end of a significant calibration curve protrusion Fig.
As indicated in the figure, the projected calendar age ranges are: Consistency of the AMS results with the existing Lirey documentation seems compelling, but a wave of questioning has followed—not of the AMS method, but of possible artifacts that could have affected the linen and invalidated the 14 C result Ref. A sampling of the creative hypotheses put forward is given in Table 2.
The first, for example, is based on the premise that nuclear reactions involving the substantial amount of deuterium contained in a human body could produce neutrons, which might then produce excess 14 C through the n,p reaction, making the age too young. The proposed deuteron reactions, however, are either qualitatively or quantitatively inaccurate—barring an unnatural burst of high energy photons photofission. Apart from the effects of such factors on the Shroud, the issue of organic reactions and non-contemporaneous contamination of ancient materials can be a very serious and complex matter, deserving quantitative investigation of the possible impacts on measurement accuracy.
The Story of Carbon Dating
Radiocarbon metrology is at the very moment in the midst of still another revolution, involving the dating or isotopic speciation of pure chemical fractions: In order to understand the nature of the challenge it is interesting to consider the limiting factors. Thus, the ultimate limiting factor for very small sample AMS is the overall isotopic-chemical blank.
This is in sharp contrast with small sample, low-level counting where the Poisson modern carbon limit ca. Microgram level 14 C soot studies have already been successful in Greenland snow; and pollen studies hold great promise for ice core dating, and perhaps even for dating the pollen found by Max Frei on the Turin Shroud. To give a rough estimate: Ongoing multidisciplinary, multi-institutional research on soot particles in remote and paleo-atmospheres, which is absolutely dependent on the small sample dating capability, is indicated in Fig.
The upper portion of the figure relates to climate oriented research on the sources and transport of fossil and biomass aerosol to the remote Arctic [ 49 ]; the lower portion relates to atmospheric and paleoatmospheric research at Alpine high altitude stations and ice cores [ 50 , 51 ]. In the remainder of this section we present some of the highlights and measurement challenges of the first project, on the long-range transport of carbonaceous particles to Summit, Greenland. Submicromolar 14 C apportionment of anthropogenic and natural carbonaceous aerosols at remote sites in Europe and Greenland provides knowledge of their impacts on present and paleoclimate [ 49 — 51 ].
It was catalyzed by the discovery of an unusually heavy loading of soot on one of the air filters used for 7 Be sampling at Summit, Greenland by Jack Dibb of UNH [ 52 ]. Measurement of 14 C in the filter sample yielded definitive evidence for biomass burning as the source of the soot. On one day only 5 August , the biomass carbon increased by nearly an order of magnitude, with scarcely any change in the fossil carbon concentration on the filter. Supporting data for the origin of the biomass burning carbon came from backtrajectory analysis, AVHRR infrared satellite imagery of the source region, and TOMS ultraviolet satellite imagery that was able to chart the course of the soot particles from the source wildfires to Summit.
The several parts of this remarkable event are assembled in Figs. Massive 6 d, km transport of soot from boreal wildfires in Canada to Summit, Greenland. Left inset [ 1 ]: Consistent with the 14 C biomass carbon data, the cloud of smoke, indicated by the light turquoise circles, is present over central Greenland for 1 day only, 5 August This is illustrated in the upper right portion of Fig.
An organic tracer of conifer combustion, methyl dehydroabietate, was found also at the same depth [ 53 ]. For the first time, direct sampling of air and surface snow took place over the polar winter, extending from June to April The large spring peaks, in particular, consisted primarily of biomass carbon: Beyond the fossil-biomass apportionment, however, lay questions about the nature and origin of the carbonaceous aerosol.
Especially intriguing are contrasts between the samples showing summer [sample-4 WO4 ] and spring [sample-8 WO8 ] biomass-C maxima in Fig. Results for one of the microanalytical techniques employed, laser microprobe mass spectrometry LAMMS , are shown in Fig. First evidence of a seasonal pattern in biomass carbon aerosol in surface snow in central Greenland [ 55 , 56 ]. PCA biplot of laser microprobe mass spectral data; compositional contrast between particles from the summer biomass peak WO4, red: The weight of multi-spectroscopic evidence thus indicates that the summer WO4 and spring WO8 biomass particles do not represent the same type of biomass.
Rather, the WO4 particles appear to include a soot component from high temperature combustion motor vehicles, wildfires. The WO8 particles, whose carbon derives almost entirely from biomass, appear to have a major biopolymer component, such as cellulose and other bio-materials associated with soil and vegetative carbon. These findings are consistent with work by Puxbaum and colleagues, who have found by direct chemical analysis, significant amounts of cellulose, bacteria, and fungal spores in atmospheric particles [ 58 , 59 ].
The dating of ancient bones has been notably unreliable because of diagenesis and isotopic contamination that occur with millennia of environmental exposure. Molecular dating of individual amino acids in such bones has proven to be one of the most effective means to overcome this problem. Figure 23 shows dramatically how the apparent radiocarbon age of the Dent Mammoth changed from ca.
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The commonly dated organic fractions from bones weak acid insoluble collagen [COLL] and gelatin [GEL] gave ages that were at odds with the archaeological evidence—suggesting recent humate contamination. When the diagenesis-resistant molecular components were isolated individual amino acids and the collagen hydrolysates [XAD-HYD] , age concordance among the individual amino acids and with the archaeological evidence indicated reliability.
Had contamination from bio-intrusive material having a different chemical amino acid pattern occurred, amino acid age heterogeneity would have been expected [ 60 ]. Radiocarbon ages of commonly dated collagen, gelatin fractions were to years too young as a result of environmental degradation; pure molecular fractions amino acids were self-consistent and in agreement with the Clovis culture age [ 60 ].
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An historical footnote related to this work involves the question of the ancestors of the North American Clovis culture. The particle-based SRM, which has been characterized for nearly chemical species and properties, serves as an essential quality assurance material for a remarkably broad range of disciplines, from the monitoring of pesticides, PCBs, and particulate mutagenic activity to basic organic geochemistry to isotopic apportionment of carbonaceous particles. A dramatic illustration of the 14 C isotopic heterogeneity in this reference material is given in Fig.
Note that the Certificate of Analysis [ 63 ] provides 14 C data expressed in the proper reference units as fraction of modern carbon f M. To emphasize the more meaningful fossil-biomass carbon source dichotomy, however, we have chosen to present the information here in terms of the fraction of biomass carbon. Sampling for SRM a took place in —; the enrichment factor for biomass carbon at that time, indicated by the red arrow in the figure, was 1. SRM a potentially can serve as a key laboratory quality assurance reference material for EC measurement.
Results of the largest intercomparison to date of EC in a uniform reference material, however, indicate a severe measurement problem: Three clusters of results for the mass fraction of EC relative to total-C , reported as information values on the Certificate of Analysis, are 0.
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For the 14 C data in Fig. Measurement of 14 C in multiple chemical fractions offers the possibility of two very interesting and important consistency tests: The first test is illustrated by comparison of the 14 C content of the EC fraction with that of the PAH fraction on average.
To the extent that both components originate from the same source, acetylenic free radicals that generate polyaromatic structures in the flaming stage of combustion, one would expect similar 14 C composition. The lack of isotopic consistency for cluster-3 EC is the stimulus for the different label, since this manifestation of EC necessarily reflects a different mix of fossil-biomass sources than the flaming stage EC, which derives primarily from fossil fuel carbon.
Regarding the second test, the 14 C data in Fig.
Cellulose is one excellent candidate [ 58 ]. The critical first step was the sequential isolation of tens of micrograms of the six PAHs in separate traps by automated preparative scale capillary gas chromatography [ 66 ]. In this case, as shown in Fig. This article represents an adaptation and extension of a recent publication in the Czechoslovak Journal of Physics: A A—A ]. Thanks go also to Cynthia Zeissler and Ed Mai for assistance in final preparation of the figures for publication. Figures are adapted, with permission, from the following sources.
California Press, Berkeley, ]. Chicago Press, Chicago, copyright 1st edition. Donahue, University of Arizona. Radiocarbon after Four Decades: Figures 15a reprint cover , 16, and 17, from Damon, P. The concept and scope of the article were crystallized in connection with luncheon talks at the Measurement Science Conference and the Radiochemical Measurement Conference , an invited NIST Sigma Xi lecture , and a plenary lecture at the Fourteenth Radiochemical Conference At the Conference in , Dr.
Currie was presented the I.
The UnMuseum - Radiocarbon Dating
These materials, designated IAEA C1 — C8, consist of wood, cellulose, sucrose, and carbonate; they cover a range of 0. Note that pMC percent modern carbon refers to f M expressed as a percentage. Meanwhile, the radiocarbon dating calibration function has undergone considerable refinement: The Calibration Issue of the journal Radiocarbon [ 13 ] has a compilation going back to ca.
By this means, calibration data have been given for periods beyond 20 BC [ 14 ]. The originally agreed upon sampling protocol was to have involved seven laboratories, two measurement techniques decay and atom [AMS] counting , and multiple samples representing different regions of the cloth. Shortly before the event, however, the scheme was changed to restrict the number of laboratories all AMS and the number of samples to three, all taken from the same location.
The sampling location, near a corner of the Shroud, and near an area damaged by the fire of AD, is considered an unfortunate choice, because of the possibility of exogenous carbon from the fire, repairs, and organic contamination from handling through the ages [ 40 , 41 ]. Organic contamination cannot be dismissed.
According to [ 42 ] Gove, et al. In a review article posted to the shroud website, www. Quantitatively, these authors suggest that the coating would contribute only a few percent to the sample carbon; qualitatively, they believe that it is a polysaccharide gum probably Gum Arabic that would be removed by the 14 C pretreatment chemistry.
1. Introduction
Nevertheless, Rogers and Arnoldi question the validity of the 14 C sample, partly because of the presence of cotton and other chemical differences between the adjacent Raes sample and the main shroud material. If the blank does not represent a homogeneous or stationary state as a reagent blank, well-mixed environmental or biological compartment, etc. Non-stationary blanks may exhibit geochemically meaningful structure, or they may be erratic, reflecting a transient source of contamination [ 46 ]. Such measurements are made feasible by the reduction of requisite sample sizes by a factor of ten or more, from what AMS 14 C dating required sixteen years ago.
The expected standard uncertainty would be equivalent to approximately radiocarbon years [ 43 ], Eq.
The back-trajectory model employed in Ref.