A new purge and trap headspace technique to analyze low volatile compounds from fluid inclusions of rocks and minerals

Research output: Contribution to journalArticleResearchpeer review

Authors

  • Ines Mulder
  • Stefan G. Huber
  • Torsten Krause
  • Cornelius Zetzsch
  • Karsten Kotte
  • Stefan Dultz
  • Heinz F. Schöler

External Research Organisations

  • Heidelberg University
  • Robert Bosch GmbH
  • University of Bayreuth
View graph of relations

Details

Original languageEnglish
Pages (from-to)148-155
Number of pages8
JournalChemical geology
Volume358
Publication statusPublished - 4 Nov 2013

Abstract

A new method for the analysis of trace gases from fluid inclusions of minerals has been developed. The purge and trap GC-MS system is based on the system described by Nolting et al. (1988) and was optimized for the analyses of halogenated volatile organic compounds (VOCs) having boiling points as low as -128. °C (carbon tetrafluoride).The sample preconcentration cold trap consists of a U-shaped glass lined steel tube (GLT™), that is immersed into a small liquid nitrogen Dewar vessel for cooling. A rapid desorption step heats up the preconcentration tube in <30s from -196°C to 200°C. The process is carried out by using a pressurized air stream to dissipate the liquid nitrogen followed by resistive heating of the trap. The design of the cold trap and the direct transfer of desorbed analytes onto the GC column via a deactivated capillary column retention gap made sample refocusing within the GC oven unnecessary. Furthermore, a special air-tight grinding device was developed in which samples ranging from soft halite (hardness 2, Mohs scale) to hard quartz (hardness 7) are effectively ground to average diameters of 1000nm or below, thereby releasing gases from fluid inclusions of minerals. The gases are then purged from the grinding chamber with a He carrier gas flow. The detection and quantitative determination of gases, such as SF6 and CF4 released from fluorites and CH3Cl from halite samples is demonstrated.

Keywords

    Carbon tetrafluoride, Dynamic headspace purge and trap technique, Fluid inclusions, Methyl chloride, Mineral grinding, Sulfur hexafluoride

ASJC Scopus subject areas

Cite this

A new purge and trap headspace technique to analyze low volatile compounds from fluid inclusions of rocks and minerals. / Mulder, Ines; Huber, Stefan G.; Krause, Torsten et al.
In: Chemical geology, Vol. 358, 04.11.2013, p. 148-155.

Research output: Contribution to journalArticleResearchpeer review

Mulder I, Huber SG, Krause T, Zetzsch C, Kotte K, Dultz S et al. A new purge and trap headspace technique to analyze low volatile compounds from fluid inclusions of rocks and minerals. Chemical geology. 2013 Nov 4;358:148-155. doi: 10.1016/j.chemgeo.2013.09.003
Mulder, Ines ; Huber, Stefan G. ; Krause, Torsten et al. / A new purge and trap headspace technique to analyze low volatile compounds from fluid inclusions of rocks and minerals. In: Chemical geology. 2013 ; Vol. 358. pp. 148-155.
Download
@article{7f21fefc9c4542b1b0c12be1e71e48a9,
title = "A new purge and trap headspace technique to analyze low volatile compounds from fluid inclusions of rocks and minerals",
abstract = "A new method for the analysis of trace gases from fluid inclusions of minerals has been developed. The purge and trap GC-MS system is based on the system described by Nolting et al. (1988) and was optimized for the analyses of halogenated volatile organic compounds (VOCs) having boiling points as low as -128. °C (carbon tetrafluoride).The sample preconcentration cold trap consists of a U-shaped glass lined steel tube (GLT{\texttrademark}), that is immersed into a small liquid nitrogen Dewar vessel for cooling. A rapid desorption step heats up the preconcentration tube in <30s from -196°C to 200°C. The process is carried out by using a pressurized air stream to dissipate the liquid nitrogen followed by resistive heating of the trap. The design of the cold trap and the direct transfer of desorbed analytes onto the GC column via a deactivated capillary column retention gap made sample refocusing within the GC oven unnecessary. Furthermore, a special air-tight grinding device was developed in which samples ranging from soft halite (hardness 2, Mohs scale) to hard quartz (hardness 7) are effectively ground to average diameters of 1000nm or below, thereby releasing gases from fluid inclusions of minerals. The gases are then purged from the grinding chamber with a He carrier gas flow. The detection and quantitative determination of gases, such as SF6 and CF4 released from fluorites and CH3Cl from halite samples is demonstrated.",
keywords = "Carbon tetrafluoride, Dynamic headspace purge and trap technique, Fluid inclusions, Methyl chloride, Mineral grinding, Sulfur hexafluoride",
author = "Ines Mulder and Huber, {Stefan G.} and Torsten Krause and Cornelius Zetzsch and Karsten Kotte and Stefan Dultz and Sch{\"o}ler, {Heinz F.}",
note = "Funding information: Thanks to G{\"u}nther Sch{\"o}nlein, a private mineral collector from Bamberg, Germany, for generously providing us with minerals for testing and to Ronald Bakker at the University in Leoben for his fluid inclusion workshop. This work was supported by the DFG Research Unit 763 .",
year = "2013",
month = nov,
day = "4",
doi = "10.1016/j.chemgeo.2013.09.003",
language = "English",
volume = "358",
pages = "148--155",
journal = "Chemical geology",
issn = "0009-2541",
publisher = "Elsevier",

}

Download

TY - JOUR

T1 - A new purge and trap headspace technique to analyze low volatile compounds from fluid inclusions of rocks and minerals

AU - Mulder, Ines

AU - Huber, Stefan G.

AU - Krause, Torsten

AU - Zetzsch, Cornelius

AU - Kotte, Karsten

AU - Dultz, Stefan

AU - Schöler, Heinz F.

N1 - Funding information: Thanks to Günther Schönlein, a private mineral collector from Bamberg, Germany, for generously providing us with minerals for testing and to Ronald Bakker at the University in Leoben for his fluid inclusion workshop. This work was supported by the DFG Research Unit 763 .

PY - 2013/11/4

Y1 - 2013/11/4

N2 - A new method for the analysis of trace gases from fluid inclusions of minerals has been developed. The purge and trap GC-MS system is based on the system described by Nolting et al. (1988) and was optimized for the analyses of halogenated volatile organic compounds (VOCs) having boiling points as low as -128. °C (carbon tetrafluoride).The sample preconcentration cold trap consists of a U-shaped glass lined steel tube (GLT™), that is immersed into a small liquid nitrogen Dewar vessel for cooling. A rapid desorption step heats up the preconcentration tube in <30s from -196°C to 200°C. The process is carried out by using a pressurized air stream to dissipate the liquid nitrogen followed by resistive heating of the trap. The design of the cold trap and the direct transfer of desorbed analytes onto the GC column via a deactivated capillary column retention gap made sample refocusing within the GC oven unnecessary. Furthermore, a special air-tight grinding device was developed in which samples ranging from soft halite (hardness 2, Mohs scale) to hard quartz (hardness 7) are effectively ground to average diameters of 1000nm or below, thereby releasing gases from fluid inclusions of minerals. The gases are then purged from the grinding chamber with a He carrier gas flow. The detection and quantitative determination of gases, such as SF6 and CF4 released from fluorites and CH3Cl from halite samples is demonstrated.

AB - A new method for the analysis of trace gases from fluid inclusions of minerals has been developed. The purge and trap GC-MS system is based on the system described by Nolting et al. (1988) and was optimized for the analyses of halogenated volatile organic compounds (VOCs) having boiling points as low as -128. °C (carbon tetrafluoride).The sample preconcentration cold trap consists of a U-shaped glass lined steel tube (GLT™), that is immersed into a small liquid nitrogen Dewar vessel for cooling. A rapid desorption step heats up the preconcentration tube in <30s from -196°C to 200°C. The process is carried out by using a pressurized air stream to dissipate the liquid nitrogen followed by resistive heating of the trap. The design of the cold trap and the direct transfer of desorbed analytes onto the GC column via a deactivated capillary column retention gap made sample refocusing within the GC oven unnecessary. Furthermore, a special air-tight grinding device was developed in which samples ranging from soft halite (hardness 2, Mohs scale) to hard quartz (hardness 7) are effectively ground to average diameters of 1000nm or below, thereby releasing gases from fluid inclusions of minerals. The gases are then purged from the grinding chamber with a He carrier gas flow. The detection and quantitative determination of gases, such as SF6 and CF4 released from fluorites and CH3Cl from halite samples is demonstrated.

KW - Carbon tetrafluoride

KW - Dynamic headspace purge and trap technique

KW - Fluid inclusions

KW - Methyl chloride

KW - Mineral grinding

KW - Sulfur hexafluoride

UR - http://www.scopus.com/inward/record.url?scp=84884924318&partnerID=8YFLogxK

U2 - 10.1016/j.chemgeo.2013.09.003

DO - 10.1016/j.chemgeo.2013.09.003

M3 - Article

AN - SCOPUS:84884924318

VL - 358

SP - 148

EP - 155

JO - Chemical geology

JF - Chemical geology

SN - 0009-2541

ER -