DARWIN Digitale Dissertationen German Version Strich

FU Berlin
Digitale Dissertation

Carsten Bloch :
The chromatomembrane-method as a sample preparation method for the gaschromatography
The combination of the chromatomembrane-method and the gaschromatography
Die Chromatomembran-Methode als Probenvorbereitung für die Gaschromatographie

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|Abstract| |Table of Contents| |More Information|

Abstract

The chromatomembrane-method is a new extraction technique. An aqueous phase flows through the macropores of a biporous material (PTFE). As a consequence of capillary phenomenons the liquid is not able to penetrate into the micropores, so that a nonpolar phase (a gas or a liquid organic phase) can flow through these micropores. At the interface boundary surface an analyt transfer can occur.

The combination of this chromatomembrane-method with the gaschromatography is described. Organic compounds in aqueous solutions was determinated after a liquid-gas-extraction or a liquid-liquid-extraction by using a chromatomembrane-cell.

The liquid-gas-extraction was preferred for the determination of volatile organic compounds (VOC´s). The VOC´s were extracted into a nitrogen stream and injected via a six-port-valve into the gaschromatographic system. By using a trap for accumulation the detection limits of the VOC´s were in the µg/l range. The influences of flow rates, temperature and salt concentration were investigated. A mathematical calculation for these effects in the chromatomembrane-method was developed.

For semivolatile or non-volatile organic compounds an extraction into a gas phase is not possible in an easy way. But these compounds can also be determinated with the CM-method, if a liquid-liquid-extraction will be taken. For this extraction it must be prevented that to large volumes of the organic solvent will be injected into the gaschromatographic system. This is the reason that another step must be carry out in the experimental system: After the organic compounds are accumulated in a trap, the solvent must be blow out of this trap with a nitrogen stream. Then the organic compounds were desorbed on a thermal way and injected into the GC. On this way semivolatile organic compounds could be detected in the µg/l range too.

The advantages of the CM-method are the easy possibility of automatisation, low detection limits, a better distribution of compounds in liquid-gas-systems and the possibility of working with very low volumes of solvents in a liquid-liquid-systems.


Table of Contents

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Inhalt


Inhalt
1
1. Einleitung und Problemstellung
3
2. Theoretischer Teil  
2.1 Methoden der Probenvorbereitung in der Wasseranalytik
7
2.1.1 Extraktions- und Anreicherungsverfahren
7
2.1.2 Membranen
24
2.2 Die Chromatomembran-Methode
27
2.2.1 Aufbau der Chromatomembran-Zelle
28
2.2.2 Prinzip der Chromatomembran-Zelle
29
2.2.3 Die Chromatomembran-Methode in der Analytik
34
3. Experimenteller Teil und Diskussion  
3.1 Ermittlung der Phasenkontaktfläche in der Chromatomembran-Zelle
38
3.1.1 Geräte und Chemikalien
40
3.1.2 Versuchsdurchführung
40
3.1.3 Ergebnisse
42
3.2 Flüssig-Gas-Extraktion mit der Chromatomembran-Methode
46
3.2.1 Geräte und Chemikalien
46
3.2.2 Leichtflüchtige organische Verbindungen
47
3.2.3 Versuchsaufbau
48
3.2.4 Der Einfluss äußerer Parameter auf die Extraktion
49
3.2.5 Vergleich mit der Purge-and-Trap-Technik
74
3.2.6 Überblick zur Diskussion der Flüssig-Gas-Extraktion
78
3.3 Flüssig-Flüssig-Extraktion mit der Chromatomembran-Methode
81
3.3.1 Versuchsdurchführung
81
3.3.2 Die Probenschleife
83
3.3.3 Die Flussraten durch die Chromatomembran-Zelle
87
3.3.4 Nachweisgrenzen der Flüssig-Flüssig-Extraktion
90
3.3.5 Vergleichende Messungen ohne Chromatomembran-Zelle
91
3.3.6 Vergleich von Flüssig-Flüssig-Extraktion und Flüssig-Gas-Extraktion mit der Chromatomembran-Methode  

93
4. Zusammenfassung und Ausblick
96
5. Literatur
100
6. Anhang
106
6.1 Verzeichnis der verwendeten Abkürzungen
106
6.2 Verzeichnis der Symbole
107
6.3 Tabellen
108


More Information:

Online available: http://www.diss.fu-berlin.de/1999/28/indexe.html
Language of PhDThesis: german
Keywords: Chromatomembrane-method; Gaschromatography; Extraction;VOC
DNB-Sachgruppe: 30 Chemie
Date of disputation: 30-Apr-1999
PhDThesis from: Fachbereich Biologie, Chemie, Pharmazie, Freie Universität Berlin
First Referee: Prof. Dr. Jürgen Simon
Second Referee: Prof. Dr.-Ing. Günter Marx
Contact (Author): bloch@chemie.fu-berlin.de
Contact (Advisor): behrens@chemie.fu-berlin.de
Date created:10-May-1999
Date available:02-Jun-1999

 


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