Bret C. Windom

Novel reduced pressure-balance syringe for chromatographic analysis.

When withdrawing a fluid sample (for additional chromatographic analyses) from an apparatus operated at a reduced pressure, a typical syringe proves to be ineffective (even if it is equipped with a gas tight plunger). It simply does not create enough pressure differential to remove a fluid sample from a reduced pressure environment. We encountered such a situation as part of efforts to extend the operation of the advanced distillation curve protocol to reduced pressures. The problem was solved by the development of a pressure balance syringe that allows reliable and precise sampling from an apparatus operating at sub-ambient pressures. This new device uses an external vacuum source to evacuate a syringe barrel, allowing a user to withdraw fluid samples from environments with pressures as low as 0.5kPa. To demonstrate the operation of the newly developed device, distillate analyses were performed on two fluids at low pressure: a predefined validation mixture, and a commercial soy based biodiesel fuel. The pressure balance syringe was used successfully for sampling in both cases. The use of the pressure balance syringe is not limited to reduced pressure distillations; indeed it can be used for a variety of applications in which chemical/compositional analyses are desired on a fluid contained in a reduced pressure environment.

Chromatographic sample collection from two-phase (gas+liquid) flows.

A particularly challenging sample presentation in analytical chemistry is a flowing stream that consists of both a gas and liquid phase, combined with the common situation in which a reliable analysis is needed for both phases, separately. In these cases, the vapor and liquid must be physically separated (without change to either), before the individual phases can be collected and analyzed. It is not possible to analyze two-phase flows otherwise. Although the two phases are at equilibrium, it is imperative that no liquid contaminate the vapor, and no vapor be entrained in the liquid at a given temperature and pressure. In this paper, we describe a simple on-line device that can individually separate and collect the vapor and liquid phases of a two-phase flow. The apparatus, which we call P(2)SC, uses an adaptation of the branch point separator, with vapor collection done downstream in a metal bellows. The liquid collection is done in a length of Teflon tube. The separated vapor and liquid phases are then easily transferred into any desired analytical instrument with a syringe, although any sample introduction method, such as a valve, could be used as well. We discuss the application of this device with a stream of thermally stressed rocket kerosene.