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The National Electrostatics Corporation has built and tested a prototype low energy, open-air, single stage carbon accelerator mass spectrometry (AMS) system (patent pending). The configuration tested has a standard 40-sample, multi-cathode SNICS source on a 300-kV deck. The beam is mass analyzed before acceleration to a gas stripper located at ground. The 14C+ ions are separated from 13C+ and 12C+ arising from the molecular breakup by a 90° analyzing magnet immediately after the gas stripper which acts as a molecular dissociator. The 14C+ beam passes through an electrostatic spherical analyzer before entering the particle detector. The observed 14C/12C precision is better than 5% with a sensitivity of better than 0.05 dpm/gmC. A first single stage AMS system has been ordered. The configuration of this system will be discussed.
High precision for radiocarbon cannot be reached without profound insight into the various sources of uncertainty which only can be obtained from systematic investigations. In this paper, we present a whole series of investigations where in some cases 16O:17O:18O served as a substitute for 12C:13C:14C. This circumvents the disadvantages of event counting, providing more precise results in a much shorter time. As expected, not a single effect but a combination of many effects of similar importance were found to be limiting the precision.
We will discuss the influence of machine tuning and stability, isotope fractionation, beam current, space charge effects, sputter target geometry, and cratering. Refined measurement and data evaluation procedures allow one to overcome several of these limitations. Systematic measurements on FIRI-D wood show that a measurement precision of ±20 14C yr (1 σ) can be achieved for single-sputter targets.
Precision and accuracy in accelerator mass spectrometry (AMS) dating relies on the systematic reduction of errors at all stages of the dating process, from sampling to AMS measurement. With new AMS systems providing much better precision and accuracy for the final stage of the process, we need to review the process as a whole to test the accuracy of reported results. A new High Voltage Engineering Europa (HVEE) AMS system was accepted at Oxford in September 2002. Since then, the system has been in routine use for AMS dating and here we report on our experiences during the first year. The AMS system itself is known to be capable of making measurements on single targets to a precision of better than 0.2% for the 14C/13C ratio and better than 0.1% for the 13C/12C ratio. In routine operation, we measure known-age wood to a precision of just above 0.3%, including uncertainties in background and pretreatment. At these levels, the scatter in results is no higher than reported errors, suggesting that uncertainties of ±25 to ±30 14C yr can be reliably reported on single target measurements. This provides a test of all parts of the process for a particular material in a particular state of preservation. More generally, sample pretreatment should remove as much contamination as feasible from the sample while adding as little laboratory contamination as possible. For more complex materials, such as bone, there is clearly more work needed to prove good reproducibility and insignificant offsets in all circumstances. Strategies for testing accuracy and precision on unknown material are discussed here, as well as the possibilities of one day reaching precisions equivalent to errors of <±20 14C yr.
This paper reports on the performance of a new method of sample injection using the High Voltage Engineering Europa (HVEE) SO-110 ion source jointly developed between HVEE and Oxford. In order to use this source, we have developed a new gas handling system which works on the direct injection of carbon dioxide mixed into a continuous flow of helium. Preliminary work has also been carried out on online gas chromatography-accelerator mass spectrometry (GC-AMS). In this application, a GC is directly coupled to the AMS system using a GC-IRMS combustion interface and Nafion™ drier. We show here results for the measurement of natural abundance in separated compounds with good peak separation and precisions of about 10%. This type of system should be ideal for source apportionment studies, biomedical, and other similar work where high precision is not required but where sample sizes are very low.
The Keck Carbon Cycle accelerator mass spectrometry facility at the University of California, Irvine, operates a National Electronics Corporation 40-sample MC-SNICS ion source. We describe modifications that have increased beam current output, improved reliability, and made the source easier to service.
A new radiocarbon accelerator mass spectrometry (AMS) laboratory for carbon cycle studies has been established at the University of California, Irvine. The 0.5MV AMS system was installed in mid-2002 and has operated routinely since October of that year. This paper briefly describes the spectrometer and summarizes lessons learned during the first year of operation. In the process of setting up the system, we identified and largely suppressed a previously unreported 14C AMS background: charge exchange tails from 14N beams derived from nitrogen-containing molecular ions produced near the entrance of the accelerator.
The new accelerator mass spectrometry (AMS) Radiocarbon Analysis Laboratory in Jena is described. The laboratory developed a combustion system for solid samples and a CO2 extraction system for air samples. Thus far, sample preparation, including graphitization, was performed in the laboratory, and the samples were measured subsequently by other AMS facilities. Currently, the laboratory owns a 3MV AMS system from HVEE (Netherlands) that has passed the acceptance tests and will be used for routine 14C determinations in the near future. The AMS system is equipped with 2 ion sources, one suitable for graphite targets and the second for both graphite and CO2 targets.
A new National Electrostatic Corporation (NEC) 5MV accelerator mass spectrometer became operational at the Scottish Universities Environmental Research Centre (SUERC) in July 2002. It has 2 Cs sputter negative ion sources: a 134-sample source (S1) for the routine measurement of all species, and a hybrid source (S2) with 40 spaces for radiocarbon measurements with either graphite or CO2 samples. A number of performance tests on graphite samples have been carried out on both sources. A precison of better than 0.3% is feasible for modern samples on a routine basis. The 14C background of the machine and the graphite preparation process blank are 0.04 ± 0.01 and 0.16 ± 0.05 pMC, respectively, indicating that 14C dating back to ~50 kyr BP is possible. The normalized 14C values for a series of reference materials agree well with the IAEA, TIRI, and FIRI consensus values. Routine measurement of 14C has been underway since May 2003. Preliminary results of performance tests on the CO2 gas ion source are also reported.
The requests to measure many samples, and samples with very low carbon masses, make it necessary to develop new techniques in sample handling to accelerate sample preparation and to eliminate carbon contamination. Our 40 MC-SNICS was recently modified to a hybrid ion source. To run the hybrid ion source with a gas parameter, settings were studied and a gas handling system for the direct coupling of an elemental analyzer and a gas ion source was developed.
Sequential injection or bouncing has a number of properties which can lead to a reduction of the analysis accuracy if no appropriate measures are taken. A special injection system has been developed in order to eliminate these shortcomings. The influence of source glitches or instabilities on the measured isotopic ratio is substantially reduced by a high cycling frequency. A fast beam-blanking unit guarantees the needed accuracy of the injection periods. Background currents are avoided by synchronizing the current measurement for the stable isotopes with their injection periods. To achieve the required speed and precision of the gated measurement, new instrumentation was developed. The elimination of background contributions allows an efficiency for radiocarbon counting as high as 95% at a cycling frequency of 100 Hz.
The injection of 10BeF- instead of 10BeO- into a compact accelerator mass spectrometry system with a terminal voltage of 0.58 MV was investigated, because BF- molecules are unstable and isobaric interference of 10B with 10Be can thus be significantly reduced. We describe the method we developed to prepare BeF2 samples. 10Be was measured in a segmented gas ionization detector. Separation of 10Be from 10B could be achieved both for ions in the 1+ charge state with an energy of 0.8 MeV and in the 2+ charge state with an energy of 1.4 MeV. The 2+ ions are better separated, whereas the 1+ charge state has a higher transmission. 10Be/9Be ratios (~10-12) in a suite of rock samples were successfully determined for exposure dating in either charge state and compared with measurements made on the 6MV tandem.
A simulation study for the separation of rare isotopes such as beryllium and aluminum was performed for a new beam line to be attached to the 3MV Tandetron accelerator at the accelerator mass spectrometry (AMS) facility of Seoul National University in Korea. The new beam line will also be used for other scientific applications, namely, ion implantations, Rutherford backscattering, and nuclear astrophysics experiments. It mainly consists of 30° and 100° deflection dipole magnets and drift spaces. A transfer matrix for the beam line was determined by the TRANSPORT code. Simulation of the rare isotope separation was performed by a ray tracing method using the TURTLE code. The simulation results, including the effect of the energy degrader, provide feasibility for the separation of isobars with small mass differences in 10Be-10B and 26Al-26Mg.
Cosmic background and its variation have been removed in the Gran Sasso National Laboratory (National Institute of Nuclear Physics) by its 1400-m rock overburden. Stable, high-performance liquid scintillation counting conditions are obtained when any remaining variable components of the environmental background, such as radon, are eliminated. The ultra low-level liquid scintillation spectrometer Quantulus™ has an anti-Compton guard detector (guard for short) that allows monitoring of gamma radiation in the background. The guard detector efficiency in radiocarbon background reduction is 8% in the Gran Sasso National Laboratory, while 80% is observed in surface laboratories. Thus, atmospheric pressure variations in surface laboratories cause variation in cosmic radiation flux. The Quantulus anti-Compton detector is highly efficient in detecting cosmic radiation, and the sample count rate remains stable in long-term counting. Also, correlation of sample backgrounds with environmental gamma radiation in various laboratories is examined.
Two methods of chemical preparation of radiocarbon samples are implemented in the Zagreb Radiocarbon Laboratory for measurement by a new liquid scintillation counter (LSC), Quantulus 1220™: a CO2 absorption method (LSC-A) and a benzene synthesis method (LSC-B). For samples prepared by both methods, the optimal counting windows for measurement in LSC were determined. The total efficiency of LSC-A is 65% and that of the LSC-B is 83%, while the corresponding 14C dating limits are 31,800 yr and 52,160 yr, respectively.
14C activities measured by the LSC-A and LSC-B methods were compared with those measured by the gas proportional counter (GPC) method (efficiency 75%, 14C dating limit 37,500 yr). The results obtained by the LSC-A method have larger errors than those measured by the GPC method, but LSC-A is quick, inexpensive, simple, and requires less carbon than the GPC method. Thus, LSC-A is suitable for 14C measurements of geological, hydrological, and environmental samples. On the other hand, the results obtained by the LSC-B method give smaller errors and a larger 14C dating range. Therefore, LSC-B is more suitable for 14C dating of archaeological samples.
Following the passing of Prof Cheikh Anta Diop in 1986, the radiocarbon laboratory (LC14) he created 20 yr earlier at the Institut Francophone d'Afrique Noire (IFAN), Dakar, Senegal, fell into a long hibernation. It took nearly 3 yr to renovate the laboratory and reinstall new equipment in order to return LC14 to full functionality and resume its activity. A new dating system has been implemented around a super low-level liquid scintillation spectrometer from Packard, the Tri-Carb 3170TR/LS, located in an underground room.
In this paper, we assess the performance of the dating setup (background level and figure of merit) using known samples from Paris 6 and international standards from the International Atomic Energy Agency (IAEA). After the calibration, the setup was used to study bolé seashells from the Khant area in the northern part of Senegal (West Africa). The aim is to present evidence of the correlation between the transgression of the Nouakchottan (5500 BP) and a few industries in the Khant area. The corresponding ages are difficult to assess and the dates available for this cultural site are randomly distributed, ranging from 4500 to 1500 BP, i.e., a chronological period spanning from the Neolithic to the Iron Age.
International radiocarbon intercalibration studies have revealed that radiometric laboratories using liquid scintillation (LS) spectrometry of benzene reported, on average, younger ages for near-background standards than either gas proportional counter (GPC) or accelerator mass spectrometry (AMS) laboratories. These studies suggested that the younger LS ages are probably related to the use of spectrophotometric benzene as a background standard. An analysis of successive 110-ka subfossil wood (Airedale Reef Ancient Wood: ARAW) standards shows that vacuum line memory effects occur in LS spectrometry and, consequently, must be corrected to obtain accurate 14C dates. ARAW standards, measured at monthly intervals in the Waikato laboratory, are used to provide blank corrections for both research and routine dating applications. The strong correlation between the ARAW δ14C data and the sample activities that preceded the standards may provide an opportunity to obtain sample-specific blank corrections. Lithium carbide synthesis is likely to prove a source of contamination. This work suggests that reproducible background levels for routine dating of less than 0.1 pMC (55 ka 14C yr) are achievable.