title: DATINK pilot study: an effective methodology for ballpoint pen ink dating in questioned documents.
abstract: Establishing the approximate age of an ink entry from a questioned document is often a complicated task and a controversial issue in forensic sciences. Among the existing approaches, the analysis of solvents in ballpoint inks may be a useful parameter for determining the age of ink on paper. In recent years, several ink dating methods have been proposed. These methods have been based on the analysis of common ink solvents using gas chromatography/mass spectrometry (GC/MS) as the analytical platform. Despite these recent methods, several questions remain. The aim of this work was to develop an ink dating methodology (DATINK) for documents written by ballpoint pens based on the disappearance of volatile solvents from the ink entry. Multiple solid-phase microextraction (MHS-SPME) coupled to GC/MS was used to measure the solvents from ink entries made with four BIC(®) ballpoint pens. The β parameter, the remaining fraction of the analyte in the system after one equilibration, corresponding to the successive extractions was considered for modelling a mathematical equation for later ink age dating. Preliminary tests of DATINK method showed that it was possible to detect the presence of ink solvents on documents up to the studied five years. The analyses of different real samples of known age were analyzed in terms of β values, which provided a mean relative error of 21%. The proposed use of β parameter for estimating the absolute age of ballpoint ink entries has shown promising results with a standard deviation of β ranging from 0.002 to 0.004.
authors.affiliation: Analytical Chemistry Department, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), Box 644, 48080 Bilbao, Spain. Electronic address: itxasosanroman@hotmail.com.
authors.forename: I
authors.initials: I
authors.lastname: San Román
authors.affiliation: Central Analysis Service (SGIker), Faculty of Science and Technology, University of the Basque Country (UPV/EHU), Box 644, 48080 Bilbao, Spain.
authors.forename: L
authors.initials: L
authors.lastname: Bartolomé
authors.affiliation: Analytical Chemistry Department, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), Box 644, 48080 Bilbao, Spain.
authors.forename: M L
authors.initials: ML
authors.lastname: Alonso
authors.affiliation: Analytical Chemistry Department, Faculty of Science and Technology, University of the Basque Country (UPV/EHU), Box 644, 48080 Bilbao, Spain.
authors.forename: R M
authors.initials: RM
authors.lastname: Alonso
authors.affiliation: LEYAS Investigaciones Forenses Documentales S.L., 31011 Pamplona, Spain.
authors.forename: M
authors.initials: M
authors.lastname: Ezcurra
keywords: Ballpoint pen ink; Forensic science; Multiple headspace solid-phase microextraction; Questioned documents; Volatile ink compound dating