Dynamic headspace generation and quantitation of triacetone triperoxide vapor

• Published in: Journal of Chromatography A 2014-02, Vol.1331, p.38-43
• Main Authors: Giordano, Braden C., Lubrano, Adam L., Field, Christopher R., Collins, Greg E.
• Format: Article
• Language: English
• Subjects: Analytical chemistry; Applied sciences; Chemical industry and chemicals; Chemistry; Chromatographic methods and physical methods associated with chromatography; Dynamic headspace; Exact sciences and technology; Explosives; Gas chromatographic methods; GC/MS; Industrial chemicals; Inlets; Liners; Powders, propellants, explosives; Samples; Statistical analysis; Statistical methods; Streams; TATP; Triacetone triperoxide; Tubes; Vapor
• ISSN: 0021-9673
• DOI: 10.1016/j.chroma.2014.01.045

•An Online PTV inlet allows for direct sampling and quantitation of TATP vapor via GC/MS.•Estimates of vapor concentration determined from mass loss of a solid sample are in good agreement with GC/MS quantitation.•Vapor concentration varies from 50 to 5400ngL−1. Two methods for quantitation of triacetone triperoxide (TATP) vapor using a programmable temperature vaporization (PTV) inlet coupled to a gas chromatography/mass spectrometer (GC/MS) have been demonstrated. The dynamic headspace of bulk TATP was mixed with clean humid air to produce a TATP vapor stream. Sampling via a heated transfer line to a PTV inlet with a Tenax-TA™ filled liner allowed for direct injection of the vapor stream to a GC/MS for vapor quantitation. TATP was extracted from the vapor stream and subsequently desorbed from the PTV liner for splitless injection on the GC column. Calibration curves were prepared using solution standards with a standard split/splitless GC inlet for quantitation of the TATP vapor. Alternatively, vapor was sampled onto a Tenax-TA™ sample tube and placed into a thermal desorption system. In this instance, vapor was desorbed from the tube and subsequently trapped on a liquid nitrogen cooled PTV inlet. Calibration curves for this method were prepared from direct liquid injection of standards onto samples tube with the caveat that a vacuum is applied to the tube during deposition to ensure that the volatile TATP penetrates into the tube. Vapor concentration measurements, as determined by either GC/MS analysis or mass gravimetry of the bulk TATP, were statistically indistinguishable. Different approaches to broaden the TATP vapor dynamic range, including diluent air flow, sample chamber temperature, sample vial orifice size, and sample size are discussed. Vapor concentrations between 50 and 5400ngL−1 are reported, with stable vapor generation observed for as long as 60 consecutive hours.