DE3900799A1 - Measuring apparatus for determining volatile constituents in a liquid by the headspace method - Google Patents

Measuring apparatus for determining volatile constituents in a liquid by the headspace method

Info

Publication number
DE3900799A1
DE3900799A1 DE19893900799 DE3900799A DE3900799A1 DE 3900799 A1 DE3900799 A1 DE 3900799A1 DE 19893900799 DE19893900799 DE 19893900799 DE 3900799 A DE3900799 A DE 3900799A DE 3900799 A1 DE3900799 A1 DE 3900799A1
Authority
DE
Germany
Prior art keywords
headspace
autoclave
fed
liquid sample
measuring apparatus
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
DE19893900799
Other languages
German (de)
Inventor
Alfred Kelder
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
META MESSTECHNISCHE SYSTEME GM
Original Assignee
META MESSTECHNISCHE SYSTEME GM
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by META MESSTECHNISCHE SYSTEME GM filed Critical META MESSTECHNISCHE SYSTEME GM
Priority to DE19893900799 priority Critical patent/DE3900799A1/en
Publication of DE3900799A1 publication Critical patent/DE3900799A1/en
Withdrawn legal-status Critical Current

Links

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G01N30/12—Preparation by evaporation
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/18—Water
    • G01N33/1826—Water organic contamination in water
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/02—Devices for withdrawing samples
    • G01N1/22—Devices for withdrawing samples in the gaseous state
    • G01N1/2226—Sampling from a closed space, e.g. food package, head space
    • G01N2001/2229—Headspace sampling, i.e. vapour over liquid
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/24—Automatic injection systems

Abstract

Measuring apparatus for determining volatile constituents in a liquid sample by the headspace method. The measuring apparatus comprises the following individual parts: a) a heatable autoclave (7) having a headspace (9), into which a metered liquid sample (8) can be introduced, b) a gas chromatograph (16) which is connected to the headspace of the autoclave (7) via a line, c) and a data processing circuit connected to the gas chromatograph for evaluating the measured analytical values. For programmable, fully automatic control of the analysis, a series of controllable valves is present, namely: - a first valve (V1) by means of which a liquid sample (8) can be fed into the autoclave chambers (7), - a further valve (V4) by means of which a carrier gas can be fed into the headspace (9), - a further valve (V5) via which gaseous samples can be taken from the headspace, which samples can be fed via a pipe (13) to the GC (16), - and a further valve (V3) by means of which the processed sample can be drained from the autoclave (7). <IMAGE>

Description

Die Neuerung betrifft eine Meßvorrichtung zur Bestimmung flüchtiger Bestandteile in einer Flüssigkeitsprobe nach dem Headspace-Verfah­ ren, wie sie in der Zeichnung dargestellt ist.The innovation relates to a measuring device for determining volatile Components in a liquid sample according to the headspace procedure ren, as shown in the drawing.

Aus einer Flüssigkeitsleitung, hier Wasserleitung, wird über einen Pufferbehälter und über das steuerbare Ventil V 1 jeweils eine Flüssigkeitsprobe in einen Autoklaven eingegeben. Der Autoklav ist beheizbar. Üblicherweise werden 60 C eingestellt. Der sich oberhalb des Wasserspiegels befindende Headspace, d. h. Kopfraum, wird über ein steuerbares Ventil und eine Vakuumpumpe weitgehend von Luft befreit. Nach Erwärmung der Probe bildet sich demnach im Headspace ein Gasgemisch, das aus Wasserdampf und aus Gasen besteht, die im Wasser enthalten sind und die durch die Erwärmung ausgebracht werden. Nachdem eine festgelegte Meßzeit vergangen ist, wird über ein zweites steuerbares Ventil V 4 ein Trägergas mit einem Druck von 0,5-1 bar eingespeist. Bei dem Trägergas handelt es sich beispielsweise um Stickstoff oder Argon. Nachdem eine Durchmischung des Trägergases mit dem Gas im Headspace stattgefunden hat, wird über ein drittes steuerbares Ventil V 5 und eine Probenleitung, die ebenfalls beheizt ist, eine Gasprobe entnommen. In einer Probeschleife, d. h. Wartestation, die durch ein weiteres Ventil V 6 betätigbar ist, wartet die Probe auf die eigentliche Messung. Über eine automatische Probenaufgabe, wie sie an sich bekannt ist, wird dem Gaschromatographen GC die Gasprobe eingespeist und ausgewertet. Dies geschieht ebenfalls automatisch. Der Auswerteeinheit kann eine Alarmanlage angeschlossen werden, beispielsweise bei Überschreiten von festgelegten Höchstwerten.From a liquid line, here a water line, a liquid sample is fed into an autoclave via a buffer tank and the controllable valve V 1 . The autoclave can be heated. 60 C are usually set. The headspace above the water level, ie headspace, is largely cleared of air via a controllable valve and a vacuum pump. After the sample has been heated, a gas mixture is formed in the headspace, which consists of water vapor and gases that are contained in the water and which are released by the heating. After a specified measurement time has passed, a carrier gas with a pressure of 0.5-1 bar is fed in via a second controllable valve V 4 . The carrier gas is, for example, nitrogen or argon. After the carrier gas has been mixed with the gas in the headspace, a gas sample is taken via a third controllable valve V 5 and a sample line, which is also heated. The sample waits for the actual measurement in a test loop, ie waiting station, which can be actuated by a further valve V 6 . The gas sample is fed to the gas chromatograph GC and evaluated via an automatic sample feed, as is known per se. This also happens automatically. An alarm system can be connected to the evaluation unit, for example when predetermined maximum values are exceeded.

Im unteren Teil der Zeichnung ist ferner in Diagramm der jeweiligen Schaltsequenzen der Ventile V 1-V 5 dargestellt.In the lower part of the drawing is also shown in diagram of the respective switching sequences of the valves V 1 - V 5 .

Claims (1)

Meßvorrichtung zur Bestimmung flüchtiger Bestandteile in einer Flüssigkeitsprobe nach dem Headspace-Verfahren, bei der die genannte Meßvorrichtung einen beheizbaren Autoklaven, in den die Flüssigkeitsprobe einspeisbar und auf eine festgelegte Temperatur erwärmbar ist, sowie einen Gaschromatographen zur Auswertung der im Headspace des Autoklaven anfallenden, gasförmigen Proben umfaßt, dadurch gekennzeichnet, daß
über ein erstes steuerbares Ventil (V 1) die Flüssigkeitsprobe in den Autoklaven dosiert einspeisbar ist,
daß über ein zweites steuerbares Ventil (V 4) ein Trägergas in den Headspace einspeisbar ist,
daß über ein drittes steuerbares Ventil (V 5) gasförmige Proben entnehmbar sind, die über eine Rohrleitung und eine automatische Probenaufgabe dem Gaschromatographen zuführbar sind,
daß die bearbeitete Probe über ein steuerbares Ventil (V 3) aus dem Autoklaven ablaßbar ist, und
daß dem Gaschromatographen eine Auswerteeinheit angeschlossen ist, wobei die Ventile durch eine automatische Ablaufsteuerung in der für die Probenaufnahme und Auswertung erforderlichen Sequenz über eine elektronische Steuervorrichtung betätigbar sind.Measuring device for determining volatile constituents in a liquid sample according to the headspace method, in which the said measuring device comprises a heatable autoclave, into which the liquid sample can be fed and heated to a specified temperature, and a gas chromatograph for evaluating the gaseous samples accumulating in the headspace of the autoclave comprises, characterized in that
The liquid sample can be metered into the autoclave via a first controllable valve (V 1 ),
that a carrier gas can be fed into the headspace via a second controllable valve (V 4 ),
that gaseous samples can be removed via a third controllable valve (V 5 ), which can be fed to the gas chromatograph via a pipeline and an automatic sample application,
that the processed sample can be discharged from the autoclave via a controllable valve (V 3 ), and
that an evaluation unit is connected to the gas chromatograph, wherein the valves can be actuated by an automatic sequence control in the sequence required for sampling and evaluation via an electronic control device.
DE19893900799 1988-08-05 1989-01-13 Measuring apparatus for determining volatile constituents in a liquid by the headspace method Withdrawn DE3900799A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DE19893900799 DE3900799A1 (en) 1988-08-05 1989-01-13 Measuring apparatus for determining volatile constituents in a liquid by the headspace method

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE8809999 1988-08-05
DE19893900799 DE3900799A1 (en) 1988-08-05 1989-01-13 Measuring apparatus for determining volatile constituents in a liquid by the headspace method

Publications (1)

Publication Number Publication Date
DE3900799A1 true DE3900799A1 (en) 1990-06-07

Family

ID=25876728

Family Applications (1)

Application Number Title Priority Date Filing Date
DE19893900799 Withdrawn DE3900799A1 (en) 1988-08-05 1989-01-13 Measuring apparatus for determining volatile constituents in a liquid by the headspace method

Country Status (1)

Country Link
DE (1) DE3900799A1 (en)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5174149A (en) * 1990-06-11 1992-12-29 Carlo Erba Strumentazione S.P.A. Process and device for the vaporization injection of liquid samples in gas chromatographic analysis apparatuses
EP0847522A1 (en) * 1995-08-31 1998-06-17 Olin Corporation System and method for monitoring volatile species
EP1150111A1 (en) * 2000-04-24 2001-10-31 General Electric Company Headspace sampling and monitoring devices and methods
EP1150112A1 (en) * 2000-04-24 2001-10-31 General Electric Company On-line sparging sampling and monitoring devices and methods
DE102004039210B4 (en) * 2004-08-12 2007-04-05 Rudolf Wild Gmbh & Co. Kg Method for evaluating product shelf life in a packaging
CN103344728A (en) * 2013-06-18 2013-10-09 华东师范大学 In-situ headspace sample injector
WO2016098055A1 (en) * 2014-12-18 2016-06-23 Cork Supply Portugal, Sa Method for detecting a volatile analyte for classing and sorting cork stoppers depending on the concentration of the analyte

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3120752A (en) * 1960-11-25 1964-02-11 Pure Oil Co Apparatus for handling volatile liquids and determining volatile contaminants

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3120752A (en) * 1960-11-25 1964-02-11 Pure Oil Co Apparatus for handling volatile liquids and determining volatile contaminants

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
A. Hussam et al., Rapid and Precise Method for the Measurement of Vapor/Liquid Equilibria by Headspace Gas Chromatography, Anal. Chem. 1985, 57, 793-801 *
H. Hackenberg et al., Gas Chromatography Head- space Analysis, Heyden Verlag, London, New York, Rheine 1977n S. 20-44 *

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5174149A (en) * 1990-06-11 1992-12-29 Carlo Erba Strumentazione S.P.A. Process and device for the vaporization injection of liquid samples in gas chromatographic analysis apparatuses
EP0847522A1 (en) * 1995-08-31 1998-06-17 Olin Corporation System and method for monitoring volatile species
EP0847522A4 (en) * 1995-08-31 1999-12-22 Olin Corp System and method for monitoring volatile species
EP1150111A1 (en) * 2000-04-24 2001-10-31 General Electric Company Headspace sampling and monitoring devices and methods
EP1150112A1 (en) * 2000-04-24 2001-10-31 General Electric Company On-line sparging sampling and monitoring devices and methods
US6436710B1 (en) 2000-04-24 2002-08-20 General Electric Company Headspace sampling and monitoring systems and methods
DE102004039210B4 (en) * 2004-08-12 2007-04-05 Rudolf Wild Gmbh & Co. Kg Method for evaluating product shelf life in a packaging
DE102004039210C5 (en) * 2004-08-12 2012-11-15 Rudolf Wild Gmbh & Co. Kg Method for evaluating product shelf life in a packaging
CN103344728A (en) * 2013-06-18 2013-10-09 华东师范大学 In-situ headspace sample injector
CN103344728B (en) * 2013-06-18 2014-10-15 华东师范大学 In-situ headspace sample injector
WO2016098055A1 (en) * 2014-12-18 2016-06-23 Cork Supply Portugal, Sa Method for detecting a volatile analyte for classing and sorting cork stoppers depending on the concentration of the analyte
CN107076717A (en) * 2014-12-18 2017-08-18 科克供应葡萄牙股份有限公司 Detect method of the volatile analytes thing to be classified to cork and separated according to the concentration of the analyte
US10261062B2 (en) * 2014-12-18 2019-04-16 Cork Supply Portugal, Sa Method for detecting a volatile analyte for classing and sorting cork stoppers depending on the concentration of the analyte
AU2015365349B2 (en) * 2014-12-18 2021-04-22 Cork Supply Portugal, Sa Method for detecting a volatile analyte for classing and sorting cork stoppers depending on the concentration of the analyte

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