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qNMR under pressure - applications on compressed and liquefied gases

  • During the last years quantitative NMR spectroscopy has become a general method for solving complex problems in science and industry. The opportunity of a calibration-free quantification, related to a simple counting of the nuclear spins in the active volume of the spectrometer represents a key advantage comparing to other analytical techniques. With modern NMR systems detection limits in the lower ppm range on a molar basis are accessible in a reasonable time period, which makes it a promising method for purity assessment, as well as applications in metrological research. First experiments showed that qNMR is suitable for gas analysis with respect to components used for production of primary reference gas mixtures. For this a laboratory setup for high-pressure NMR experiments up to 20 MPa (2900 psi) in fluid and gas phase was built and tested. In this work we show the determination of the composition of high precision mixtures, consisting of liquid and liquefied hydrocarbonsDuring the last years quantitative NMR spectroscopy has become a general method for solving complex problems in science and industry. The opportunity of a calibration-free quantification, related to a simple counting of the nuclear spins in the active volume of the spectrometer represents a key advantage comparing to other analytical techniques. With modern NMR systems detection limits in the lower ppm range on a molar basis are accessible in a reasonable time period, which makes it a promising method for purity assessment, as well as applications in metrological research. First experiments showed that qNMR is suitable for gas analysis with respect to components used for production of primary reference gas mixtures. For this a laboratory setup for high-pressure NMR experiments up to 20 MPa (2900 psi) in fluid and gas phase was built and tested. In this work we show the determination of the composition of high precision mixtures, consisting of liquid and liquefied hydrocarbons commonly supplied in floating piston cylinders. Therefore an experimental setup was developed allowing sampling, as well as circulation of the mixture within a high-pressure NMR tube by using a concentric tubing assembly. Additionally, a piston-cylinder pressure cell was designed and manufactured allowing wide-range volume displacement. Mainly intended for density variation within supercritical fluid experiments, it can also function as a compression element for further increasing of gas-pressure in the system. Equipped with liquid thermostat and a motor-powered screw drive unit it is designed to operate at pressure levels up to 60 MPa (8700 psi) and temperatures up to 130 °C.zeige mehrzeige weniger

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Metadaten
Autor*innen:Klas MeyerORCiD
Koautor*innen:K. Rademann, Michael Maiwald
Dokumenttyp:Posterpräsentation
Veröffentlichungsform:Präsentation
Sprache:Englisch
Jahr der Erstveröffentlichung:2016
DDC-Klassifikation:Naturwissenschaften und Mathematik / Chemie / Analytische Chemie
Freie Schlagwörter:Gas-phase NMR; High-pressure NMR; Liquefied gases
Veranstaltung:4th Annual practical applications of NMR in industry conference (PANIC)
Veranstaltungsort:Houston, TX, USA
Beginndatum der Veranstaltung:15.02.2016
Enddatum der Veranstaltung:18.02.2016
Verfügbarkeit des Dokuments:Datei im Netzwerk der BAM verfügbar ("Closed Access")
Datum der Freischaltung:11.03.2016
Referierte Publikation:Nein
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