preparation of microgram samples on iron wool for radiocarbon analysis via accelerator mass spectrometry: A closed-system approach

A technique has been developed at NBS for the production of high quality targets for radiocarbon analysis by accelerator mass spectrometry (AMS). Our process optimizes chemical yields, ion currents and characterizes the chemical blank. The approach encompasses sample combustion to CO₂, catalytic reduction of CO₂ by Zn to CO, reduction to graphitic carbon on high-purity iron wool and in situ formation of a homogeneous iron-carbon bead; all steps are performed in a closed system. The total measurement system blank and variability are considered in the light of contributions from combustion, iron wool, reduction, bead formation and instrument blank. Additionally, use of this approach provides an increase in throughput, i.e. the effective management of large numbers of samples. Chemical yields for 50-800 μg C samples deposited on 15 mg iron wool were greater than 90%. Integrated ¹²C^- ion currents observed were significant, being 4-64% of those observed in pure graphite. These currents are about an order of magnitude greater than those expected from dilution of graphite with an inert substrate. Isotopic accuracy, precision and blank were assessed by measuring the ¹⁴C ¹³C ratios of a series of targets prepared from dead carbon and oxalic acid (SRM 4990C). Each target was typically measured for one hour; bead consumption was estimated at 5% to 10%. System blank subsequent to combustion was equivalent to (2.2 ± 0.5) μg modern carbon (chemistry + instrument); combustion blank currently stands at (0.4 ± 0.1) (SE, n = 6) μg C.