Organic Residue Analysis in Bronze Age/Iron Age pottery, soils, and adobes from the Southern Iberian Peninsula

Description

Technical info

Analysis

The analysis was performed by Gas Chromatography (GC) and GC-Mass Spectrometry (GC-MS) using an Agilent Technologies 7890B GC System series chromatograph including Agilent Technologies Capillary Flow-Technology Three-Way Splitter Kit coupled to an Agilent Technologies 5977A MSD and FID. The analyses were carried out using helium as a carrier gas, with a split/splitless injection system (Gerstel Multi-Purpose-Sampler and Gerstel Cold-Injection-System 4), operating in the splitless mode with a purge flow of 3.0ml min–1 and a constant pressure at the head of the column of 8.6667 psi. Samples were analysed using an Agilent J&W DB-5HT-column (15m × 0.32mm i.d.; 0.1μm film thickness) and divided in two equal parts using 0.18mm non-coated, deactivated silica capillary columns (0.66m splitter-column to FID/ 1.52m splitter-column to MSD) with the Three-Way Splitter Kit. The inlet temperature was ramped from 30°C to 240°C at 12°C s-1 (held isothermally for 5min) and then increased to 350°C at 12°C s-1 (held isothermally for 10min). The temperature of the oven was set at 50°C for 1min followed by an increase to 100°C at 15°C min–1, then to 240°C at 6°C min–1 and to 350°C at 10°C min–1 (held isothermally for 20min). Mass spectra were acquired using electron ionization at 70 eV and obtained by scanning between m/z 50–950 in 1.562s. The interface and the ion source temperatures were 300°C and 280°C, respectively. The temperature of the FID detector was fixed at 340°C. Mass spectra were matched against the National Institute of Standards and Technology (NIST) library, 2014 edition.