Szopa C, Freguglia G, Sternberg R, Nguyen M J, Coll P, Raulin F, Pietrogrande C, Niemann H
Service d'Aéronomie, SA, IPSL, UMR CNRS 7620, BP3, Réduit de Verrières, 91371 Verrières le Buisson Cedex, France.
J Chromatogr A. 2006 Oct 27;1131(1-2):215-26. doi: 10.1016/j.chroma.2006.07.064. Epub 2006 Aug 21.
In the frame of the calibration of the aerosol collector and pyrolyser, and gas chromatography-mass spectrometry experiments of the Huygens probe arrived at Titan, systematic experimental studies were led to estimate the influence of the operating conditions on the analyses that should have been achieved in the Titan's atmosphere. The primary objective of this study was to estimate the influence of operating conditions variations induced by (i) instrumental modifications made shortly before the probe launch which can have changed the operating pressures; (ii) the change of the probe environmental conditions (pressure, temperature) during its descent in the atmosphere; (iii) a possible deviation of pressure and temperature regulations from their nominal values because of the long journey of the instrument in space, or of other external events. The secondary objective of this work was to create an analytical database that can be used as a reference to treat the chromatograms obtained in situ, and help to identify chromatographically the analyzed species, complementary to mass spectrometry. Beyond the application to a specific instrument, this work was also useful to experimentally estimate the fundamental evolution of the separation as a function of the changes of operating conditions with time. The obtained results show (i) the significant influence of inlet and outlet pressure variation on the time of analysis, but not on the separation power. It thus enables to significantly shorten the analysis duration, and thus to analyze more compounds within the fixed time of analysis of the instrument; (ii) the significant influence of temperature on the retention. In this frame, the enthalpies of exchange between the gas phase and the stationary phase of the species were determined to be used to retrieve the analyzed species in case of deviation of the operating temperature; (iii) that the possible aging of the columns does not have influence on the columns efficiency and separation power; (iv) the analytical capabilities of the gas chromatography-mass spectrometry experiment within operating conditions representative of those encountered in situ. Finally, in spite of possible operating condition changes, it is shown that results coming from the gas chromatograph-mass spectrometer experiment, which are currently under analysis, could bring important information on the Titan's atmosphere and its history.
在对气溶胶收集器和热解器进行校准以及对抵达土卫六的惠更斯探测器进行气相色谱 - 质谱实验的框架内,开展了系统的实验研究,以评估操作条件对本应在土卫六大气中进行的分析的影响。本研究的主要目标是评估由以下因素引起的操作条件变化的影响:(i) 在探测器发射前不久进行的仪器改装,这可能改变了操作压力;(ii) 探测器在大气中下降过程中环境条件(压力、温度)的变化;(iii) 由于仪器在太空中的长途飞行或其他外部事件,压力和温度调节可能偏离其标称值。这项工作的次要目标是创建一个分析数据库,可作为处理现场获得的色谱图的参考,并有助于通过色谱法识别所分析的物种,作为质谱分析的补充。除了应用于特定仪器外,这项工作对于通过实验评估分离随操作条件随时间变化的基本演变也很有用。获得的结果表明:(i) 进样口和出口压力变化对分析时间有显著影响,但对分离能力没有影响。因此,它能够显著缩短分析持续时间,从而在仪器固定的分析时间内分析更多化合物;(ii) 温度对保留有显著影响。在此框架内,确定了物种在气相和固定相之间的交换焓,以便在操作温度出现偏差时用于检索所分析的物种;(iii) 色谱柱可能的老化对柱效和分离能力没有影响;(iv) 气相色谱 - 质谱实验在代表现场遇到的操作条件下的分析能力。最后,尽管可能存在操作条件变化,但目前正在分析的气相色谱 - 质谱实验结果表明,这些结果可能会带来有关土卫六大气及其历史的重要信息。