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The relation of the X-ray small-angle scattering parameters to the results of transmission electron microscopy for spherical Guinier-Preston zones was investigated. Experimentally, the Guinier radius is found to equal (<R7>/<R5>1/2) and the Porod radius to equal <R3>/<R2>. These results were theoretically predicted by Baur and Gerold, A log normal distribution was found to be in close agreement with the experimental data. The use of this distribution allowed the size-distribution curve of spherical Guinier-Preston zones to be constructed from the X-ray parameters and from a knowledge of the metastable miscibility gap. This approach is used to follow the evolution of size distribution in both Al-Ag and Al-Zn alloys. The application of this approach to nncleation and growth as well as redistribution processes is discussed. Growth paths are established from the size distribution evolution curves through an Nv> construction. A brief discussion of the technique is included.
We compared accelerator mass spectrometry (AMS) 14C ages of large (>150 μm) pelagic foraminifera with radiometric bulk carbonate 14C ages in two northeastern Atlantic cores. The foraminiferal ages are consistently older than those of the bulk sediment (by + 0.76 ka in Core 11881 and by + 1.1 ka in Core 11886), whereas corresponding fine (<5 μm) fraction ages are similar to those of the bulk sediment carbonate. We calculated near-identical sediment accumulation rates from both the foraminiferal and bulk sediment age/depth relations (3.0 cm ka−1 in Core 11881 and 5.9 cm ka−1 in Core 11886). Consideration of various factors that might produce such offsets leads us to believe that they are not artifacts, but were most probably caused by differential bioturbation of the different size-fractions in the sediment surface mixed layer. The importance of this finding is that many paleoceanographic records, such as the oxygen isotope record, also derive from analyses of large foraminifera, so that these records must be offset in time from the bulk of the sediments that they characterize.
A third radiocarbon counting system has been established in the Chemistry Department, University of Glasgow, since April, 1968. Operating conditions for the previous systems have remained essentially as described by Baxter et al. (1969).
Patterns of 14C enrichment in the superficial plant debris and mineral soil horizons of an established woodland have been monitored at regular intervals during the past 15 years. These data are compared with a model evaluation of carbon turnover based on the recorded changes in atmospheric 14C concentration since AD 1900.
Leaf litter and decomposing plant debris are characterized by steady-state turnover values of ca 2 and ca 8 years, respectively. A two-component system of ‘fast’ (≤20 yr) and ‘slow’ (ca 350 yr) cycling carbon is indicated for the surface (0–5cm) soil humus; below 10cm, the “fast’ component is rare (<5%).
Selective microbal humification of leaf litter, branch, and root debris is proposed to explain a delay of several years in the peak transfer of ‘bomb’ 14C to the soil carbon pool.
In 1994, the Gliwice Radiocarbon Laboratory began operating a liquid scintillation spectrometry system, consisting of a Quantulus 1220™ spectrometer and two vacuum rigs for benzene production. This paper describes the procedures used for the benzene synthesis from samples containing < 1 g of carbon and in the range 1 to 10 g of carbon. We also present the Quantulus calibration procedures used in the Gliwice Radiocarbon Laboratory and NERC Radiocarbon Laboratory, and compare the calibration parameters.
The International Collaborative Study involved a wide range of sample materials and ages and, on completion, assessed each stage independently (Scott et al 1989; Aitchison et al 1990). We combine here the three stages of the study and provide an overview of the uncertainties in the dating procedure as a whole and in its component processes. Three key optimal performance indices, related to internal and external precision and to bias, have been defined to allow quantitative assessment of Internal Consistency and External Consistency (Aitchison et al 1990). We believe that these measures provide quantitative descriptions of a laboratory's reproducibility, accuracy and precision.
For the internal consistency, we have defined the Internal Error Multiplier of the quoted error and, for the external consistency of any laboratory relative to an appropriate baseline, we have defined two indices, the Systematic Bias and External Error Multiplier of the quoted error. We have evaluated the three indices over the three stages and have assessed the relative performances of gas counting, accelerator and liquid scintillation laboratories. The quoted errors describe adequately the variability in duplicate results, but there is evidence of systematic biases and underestimation of interlaboratory variability. We have considered the contribution of pretreatment, synthesis counting to the overall variability for each laboratory type. We found that, for liquid scintillation (LS) and gas counting (GC) laboratories, ca 66% of the total variation is due to counting and sample synthesis whereas, for accelerator mass spectrometry (AMS) laboratories, the major sources of variability are the sampling and pretreatment processes.
Sample materials issued to participants in the interlaboratory calibration exercise are defined and in context of their intended interpretational significance. Preparation of the benzene and calcium carbonate standards as issued for stage 1 is described in detail; likewise, the source and pretreatment/extraction of the environmental samples dispatched for stages 2 and 3.
The Radiocarbon Laboratory at the Scottish Universities Research and Reactor Centre was established in August 1971. The laboratory is funded by the Natural Environment Research Council and its main function is geochemical investigations in collaboration with the component bodies of the Council and with grant-aided associations. A dating service is also provided to others.
Interlaboratory comparisons have been widely used in analytical chemistry and radiochemistry as an important part of ongoing quality assurance programs. The 14C community has been no exception in this respect, and in just under 20 years, there have been a number of significant and very extensive interlaboratory trials organized by individual laboratories and the International Atomic Energy Agency (IAEA) to the benefit of the 14C community (both labs and users) (Otlet et al. 1980; ISG 1982; Scott et al. 1990; Rozanski et al. 1992; Scott et al. 1992; Gulliksen and Scott 1995). The comparisons have varied widely in terms of sample type and preparation, but all have had as their primary goal the investigation of the comparability of results produced under possibly quite different laboratory protocols. As techniques have been developed and new labs formed, the reference materials created as a result of the intercomparisons have presented an opportunity for checking procedures and results. Users have been reassured by the existence of regular comparisons as one sign of the concern that laboratories have to ensure highest quality results, but also confused about how to make use of the results from past exercises in the interpretation of sets of dates from many laboratories. The laboratories have also learned valuable lessons from participation in such studies. These have included identification of systematic offsets and additional sources of variation and in studies which have used realistic samples requiring pretreatment, chemical synthesis and counting, it has been possible to identify the stage at which such problems have arisen and to quantify the relative contributions to the overall variation. In this paper, we will briefly review the comparisons so far, draw some conclusions from their findings, and make proposals for the future organization of intercomparisons.
For more than 15 years, the radiocarbon community has participated in a series of laboratory intercomparisons in response to the issue of comparability of measurements as perceived within the wider user communities (Scott et al. 1990; Rozanski et al. 1992; Gulliksen and Scott 1995; Scott et al. 1997). In this report, we provide an update on the current 14C laboratory intercomparison and reflect on future issues linked to the laboratory intercomparison program, not least those resulting from a significant growth in the number of accelerator mass spectrometry (AMS) facilities providing routine dating of small samples (milligram size).
This paper outlines a dating program designed to test the reproducibility of radiocarbon dates on different materials of Late-Glacial age (plant macrofossils, fossil beetle remains, and the “humic” and “humin” chemical fractions of limnic sediments) using a combination of radiometric (beta counting) and accelerator mass spectrometry (AMS) techniques. The results have implications for the design of sampling strategies and for the development of improved dating protocols, both of which are important if a high-precision 14C chronology for the Late-Glacial is to be achieved.
We present δ13C data from both bulk organic sediment samples and terrestrial plant macrofossils from five high-resolution sedimentary sequences from the United Kingdom from which extensive multiproxy data sets have been obtained. These span the last glacial-interglacial transition. Chronological control has been provided by radiocarbon dating and/or tephrochronology. The results demonstrate that significant shifts in bulk organic δ13C can be identified at key climatic transitions in most of the sites. The data are affected by site-specific influences that restrict their use as chronological markers. However, terrestrial plant macrofossil records are more consistent and reveal shifts that appear to be synchronous and which therefore offer a basis for interregional correlation as well as significant paleoenvironmental information.
We present a proposal for a further intercomparison exercise following discussions at the 16th International Radiocarbon Conference in Groningen in 1997. This new intercomparison will build on previous exercises by making use of both reference materials already characterized and additional known-age material. For this comparison, we describe two separate but essentially related protocols that are meant to satisfy the different priorities of radiometric and AMS laboratories. The new intercomparison is planned to begin in mid-1998.
A series of soil samples were collected in November 1984 from five stands of Sitka spruce planted at recorded times between 1951 and 1968. Within a comprehensive program of ecologic and biogeochemical analyses, natural 14C measurements on selected organic components of the 0 to 5cm soil horizons serve to quantify progressive changes induced in the organic carbon inventory and relative to that of the original grassland. Points of particular interest are: 1) an enhanced input of fresh organic matter in the years immediately following planting; this, in parallel with a net decrease in the total carbon content of the topsoil; 2) this freshly introduced carbon predominates in the soil profile even after 30 years of afforestation; 3) during the 15- to 30-year growth period, the soil carbon content remains constant but progressive changes occur in its biogeochemical composition and rate of turnover.
We describe a simple method for trapping low concentrations of CO2 present in gas mixtures, such as air and soil respiration, using a zeolite molecular sieve (type 13x) for environmental carbon isotope studies. We employ reusable molecular-sieve cartridges and a lightweight battery-driven pumping system, developed to enable CO2 collection in difficult and dangerous terrain or under extreme climatic conditions. The results of a small field experiment suggest that CO2 could be quantitatively trapped on and recovered from the 13x molecular sieve, without any fractionation of the stable carbon isotope. The δ13C of CO2 was also independent of the amount of air ≤18 liters and rate at which it was collected, i.e. ≤ 1 liter of air/min.
In this short article, we summarize some milestones in the 50-yr-long development of natural 14C measurement. In the light of this appraisal we presume to hazard some personal opinions and forecasts as to where best opportunities might lie for future gains from the continued investment in applied 14C science. The technique and the journal are one and the same in this regard.
We describe a new compilation of radiocarbon age measurements performed by the NERC Radiocarbon Laboratory that is freely available to access over the World Wide Web. The database contains 1000 14C measurements performed using the liquid scintillation counting method between 1996 and 2005, and further results will be added as the information is compiled. Contextual information including sampling location and the nature of sample material is provided, alongside 14C age results and publications codes. Hypertext links provide access to the original 14C age report associated with the samples, providing additional details. The 14C measurements were originally performed for earth and environmental science NERC projects and are therefore likely to be most relevant to the Quaternary research community.