Method optimisation for the analysis of ancient glass using laser ablation inductively couple plasma mass spectrometry
RICHARDS L. 1, CHARLTON M. 1
1 UCL Institute of Archaeology, London, United Kingdom
Compositional analysis of ancient glasses can be used to identify their provenance, the raw materials used in their production and the technologies employed to manufacture them. Laser ablation inductively couple plasma mass spectrometry (LA-ICP-MS) is a technique that has become popular because of its ability to detect elements in low concentrations (ppb levels), enabling higher resolution provenance investigations. However, LA-ICP-MS is still new to the field of archaeology compared with other techniques, and its continued development is important to further our knowledge of ancient glass production and trade. There are many different operating parameters for LA-ICP-MS reported in the literature and this study explores the optimal repetition rate and laser power to maximise sensitivity while minimising elemental fractionation for the LA-ICP-MS at the Wolfson Archaeological Science Laboratories at the UCL Institute of Archaeology. Analysis was carried out using a Nd:YAG laser operating at a wavelength of 213 nm on an Applied Spectra J200 Tandem LA/LIBS system combined with an Agilent 7900 quadrupole ICP-MS. Repetition rates used were 8 Hz, 10 Hz, 12 Hz, and 15 Hz, and the laser was run at 40% and 60% power for each repetition rate. NIST 610 and NIST 614 were used as standards for calibration, and NIST 612 and Corning B were chosen as reference materials. An experiment consisted of analysing the NIST glasses three times sequentially and the Corning glass twice, one between each set of NIST analyses. The criteria used to determine the optimal settings included: the stability of the raw and Si29-normalised signal using the relative standard deviation (RSD), the fit of the calibration lines, the accuracy (percent error) and precision (RSD) of the reference glasses, and the limits of detection on NIST 612. 40% laser power was chosen because it showed more stable signals for volatile oxides across all repetition rates. 12 Hz was chosen to maximise sensitivity but minimise potential damage to the sample.