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UBC Theses and Dissertations

An automated sample line for the preparation of O¹⁸ /O¹⁶ isotope analyses from water samples Whaite, Peter

Abstract

An automated sample preparation line has been developed to equilibrate water samples for determination of their oxygen isotope ratio. Preliminary estimates put the repeatability of the sample preparation methods at approximately 0.04°/oof a figure that compares very favourably with the present state of the art. A noteworthy feature of our sample line, is that temperature control is unnecessary during sample equilibration. Errors arising from non-constant temperature conditions are prevented by simultaneously saving all of the equilibrated gas samples in separate reservoirs when the equilibration reaction is complete. Several other innovations in sample rack design are also described. These are: a circular rack geometry; an improved, inexpensive, magnetic stirrer design to agitate water samples; a Peltier cooling device to trap water vapour; and the use of standard Pyrex test tubes as equilibration flasks. The preparation line is highly modular. Up to sixteen racks, each capable of preparing sixteen samples, can be included in the system. Racks may be removed, repaired or modified, and replaced, without disturbing the operation of any other racks in the system. The current configuration is a minimum system with only one rack. The programming concepts used to control operation of the system are new to this application, and hence are a significant contribution. A multi-tasking executive allocates resources amongst the racks on a priority basis. By using linked list structures, the operating system maximises resource and processor utilisation, but does not compromise flexibility and modularity. The operator can submit any rack for preparation at any time, and the system could, with sixteen racks, prepare a full load of 256 samples in a day. A simple handshaking interface has been provided to control the release of samples for analysis. This should make it possible to connect the sample line to any mass spectrometer capable of the automated analysis of carbon dioxide. The user controls sample line operation by commands entered on a teletype keyboard. The command language is deliberately unstructured, and users can type in "natural" English sentences if they wish. All system operations and user sentences are printed on the teletype to provide a permanent record for later scrutiny. Finally a manual command repertoire has been provided. It allows the operator complete control over any rack. All solenoids, registers, and control lines, can be manipulated on an individual basis from the teletype keyboard.

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