DE102004026379A1 - Operation of evaporative light-scattering detector of low volatility substances arising in liquid chromatography, preheats atomization gas and eluent flows - Google Patents

Operation of evaporative light-scattering detector of low volatility substances arising in liquid chromatography, preheats atomization gas and eluent flows Download PDF

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Publication number
DE102004026379A1
DE102004026379A1 DE200410026379 DE102004026379A DE102004026379A1 DE 102004026379 A1 DE102004026379 A1 DE 102004026379A1 DE 200410026379 DE200410026379 DE 200410026379 DE 102004026379 A DE102004026379 A DE 102004026379A DE 102004026379 A1 DE102004026379 A1 DE 102004026379A1
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eluent
temperature
preheated
evaporative
scattered light
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DE200410026379
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DE102004026379B4 (en
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Herbert Dr. Knauer
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VERMOEGENSVERWALTUNGS KOMMANDI
Vermogensverwaltungs-Kommanditgesellschaft Dr Ing Herbert Knauer & Co & Cie GmbH
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VERMOEGENSVERWALTUNGS KOMMANDI
Vermogensverwaltungs-Kommanditgesellschaft Dr Ing Herbert Knauer & Co & Cie GmbH
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/47—Scattering, i.e. diffuse reflection
    • G01N21/49—Scattering, i.e. diffuse reflection within a body or fluid
    • G01N21/53—Scattering, i.e. diffuse reflection within a body or fluid within a flowing fluid, e.g. smoke
    • 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
    • G01N30/62—Detectors specially adapted therefor
    • G01N30/74—Optical detectors
    • 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
    • G01N2030/022—Column chromatography characterised by the kind of separation mechanism
    • G01N2030/027—Liquid chromatography
    • 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
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/28—Control of physical parameters of the fluid carrier
    • G01N30/30—Control of physical parameters of the fluid carrier of temperature
    • G01N2030/3038—Control of physical parameters of the fluid carrier of temperature temperature control of column exit, e.g. of restrictors

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  • Physics & Mathematics (AREA)
  • Biochemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

Atomization gas is preheated to the temperature of a hot tube heat exchanger, i.e. a vaporization tube. In an alternative, a separate heater is used to bring the temperature to a value between room temperature and temperatures exceeding those in the vaporization tube. When using a separate heater, the temperature is optionally controlled. Eluent flow is preheated in a separate heater having no dead volume, to between room temperature and 200[deg]C at most. Both atomization gas and eluent are heated. A high pressure pump delivers the eluent flow to the liquid chromatograph. Atomization takes place at a small nozzle plate. This is very thin and has a hole diameter of 10-100 mu m. On expansion, the eluent flow is disrupted into uniform, small droplets. Eluent flow and/or atomization gas can be preheated at the same time. The evaporation section comprises a round- or polygonal channel. This is formed by two plates (1) with milled channels. The impact wall (2), is sharp edged but rounded in form. It intercepts larger droplets. These run away through a drain (3) and siphon.

Description

Verdampfungsstreulicht-Detektoren werden in der Flüssigkeitschromatographie zur Detektion von Substanzen eingesetzt, die schwer zu verdampfen sind. Der Eluentenstrom von einer Säule wird mit einem Zerstäuber versprüht und die feinen Tropfen in einem beheizten Rohr verdampft. Wenn die Tropfen einen schwer verdampfbaren Anteil enthalten, bildet sich ein Nebel, der durch den Streulichteffekt detektiert wird.Evaporative light scattering detectors be in liquid chromatography used for the detection of substances that are difficult to vaporize. The eluent stream from a column is with a nebulizer sprayed and the fine drops are evaporated in a heated tube. If the Drops containing a heavy vaporizable portion forms a fog that is detected by the scattered light effect.

Die Verbesserung der Zerstäubung ist die Aufgabenstellung. Die normalen Zerstäuber arbeiten mit einer Düse und einem schnellen Gasstrom, der die Düse umhüllt und die Tropfen von der Düse abreißt. Der Zerstäubungsgasstrom hat normalerweise Raumtemperatur.The Improvement of atomization is the task. The normal atomizers work with one nozzle and one fast gas flow, the nozzle wrapped and the drops from the nozzle interrupted. The atomizing gas flow usually has room temperature.

Die erfindungsgemäße Lösung wird durch folgende Verbesserungen erreicht:

  • • Der Zerstäubungsgasstrom wird vorgeheizt und bringt dadurch eine schnellere Verdampfung. Die entstehenden Tröpfchen sind durch Verringerung der Viskosität kleiner und in der Größe gleichmäßiger.
  • • Durch Vorheizung des Eluentenstromes wird auch eine Verbesserung der Zerstäubung erreicht.
The solution according to the invention is achieved by the following improvements:
  • • The atomizing gas stream is preheated, resulting in faster evaporation. The resulting droplets are smaller by reducing the viscosity and more uniform in size.
  • • Preheating the eluent stream also improves atomization.

Da der Eluentenstrom durch eine Hochdruckpumpe in der Flüssigkeitschromatographie geliefert wird, kann die Zerstäubung auch an einem Düsenplättchen sehr kleiner Dicke z.B. 0,1 mm mit einem Lochdurchmesser zwischen 10 und 100 μm erfolgen. Hierbei entspannt sich der Eluentenstrom von z.B. 50 bar auf Atmosphärendruck auf einer Laufstrecke von z.B. 0,1 mm. Dies bewirkt ein Zerreißen des Stromes in gleichmäßig kleine Tröpfchen von ca. 20 μ ∅. Der Eluentenstrom und/oder das Zerstäubergas kann dabei auch vorgewärmt werden (4).Since the eluent stream is supplied by a high-pressure pump in liquid chromatography, the atomization can also be done on a nozzle plate of very small thickness, for example, 0.1 mm with a hole diameter between 10 and 100 microns. In this case, the eluent stream of eg 50 bar relaxed to atmospheric pressure over a running distance of eg 0.1 mm. This causes a tearing of the stream in evenly small droplets of about 20 μ ∅. The eluent stream and / or the atomizing gas can also be preheated ( 4 ).

Diese Zerstäubungsmethode wurde bisher für Verdampfungsstreulicht-Detektoren noch nicht angewandt.These sputtering was previously for Evaporative scattered light detectors not yet applied.

Eine weitere bekannte Methode, die Qualität des zerstäubten Eluenten zu verbessern, besteht darin, die größten Tröpfchen durch eine Prallplatte abzufangen.A another known method to improve the quality of the atomized eluent, is the biggest droplets through to catch a baffle plate.

Erfindungsgemäß wird das erhitzte Verdampfungsrohr ersetzt durch 2 Metallplatten (1), in die Verdampfungskanäle so eingefräßt sind, dass eine Prallwand (2) entsteht. An der Prallwand würden größere Tröpfchen abgeschieden. Das System ist leicht geneigt, so dass die sich an der Prallwand sammelnden Tröpfchen durch den Ablauf (3) fließen können. Das Verdampfungsrohr ist normalerweise ein temperiertes gerades Rohr oder ein aufgewickeltes Rohr, um die Länge des Rohres zu erhöhen.According to the invention, the heated evaporation tube is replaced by 2 metal plates ( 1 ) are immersed in the evaporation channels so that a baffle ( 2 ) arises. On the baffle larger droplets were deposited. The system is slightly inclined, so that the droplets collecting at the baffle wall are blocked by the drain ( 3 ) can flow. The evaporation tube is normally a tempered straight tube or a coiled tube to increase the length of the tube.

Erfindungsgemäß besteht die Verdampfungsstrecke aus einem runden oder eckigen Kanal, der so durch zwei Platten (1) mit Einfräsungen gebildet wird, dass eine vorzugsweise scharfkantige, aber auch runde Prallwand (2) entsteht.According to the invention, the evaporation path consists of a round or square channel, which is defined by two plates ( 1 ) is formed with milled grooves that a preferably sharp-edged, but also round baffle wall ( 2 ) arises.

Das System ist leicht geneigt, so dass die sich an der Prallwand sammelnden Tröpfchen durch den Ablauf fließen können.The System is slightly inclined, so that the collecting on the baffle droplet flow through the drain can.

Claims (5)

Verfahren zum Betrieb eines Verdampfungsstreulicht-Detektors dadurch gekennzeichnet, dass das Zerstäubergas vorgewärmt wird. Die Vorwärmung kann durch Wärmeaustausch am Heizrohr (Verdampfungsrohr) erfolgen auf die Temperatur am Verdampfungsrohr oder durch einen separaten Heizer auf eine Temperatur zwischen Raumtemperatur und Temperaturen höher als im Verdampfungsrohr. Bei dem separaten Heizer kann die Temperatur ungeregelt oder geregelt sein.Method for operating an evaporative scattered light detector, characterized in that the atomizing gas is preheated. The preheating can be done by heat exchange at the heating tube (evaporation tube) to the temperature at the evaporation tube or by a separate heater to a temperature between room temperature and higher temperatures than in the evaporation tube. In the separate heater, the temperature can be unregulated or regulated. Verfahren zum Betrieb eines Verdampfungsstreulicht-Detektors dadurch gekennzeichnet, dass der Eluentenstrom vorgewärmt wird. Die Vorwärmung soll durch einen totvolumenarmen separaten Heizer zwischen Raumtemperatur und bis maximal 200°C erwärmt werden.Method for operating an evaporative scattered light detector characterized in that the eluent stream is preheated. The preheating should by a dead volume low separate heater between room temperature and up to a maximum of 200 ° C heated become. Verfahren zum Betrieb eines Verdampfungsstreulicht-Detektors dadurch gekennzeichnet, dass sowohl das Zerstäubungsgas als auch der Eluent erwärmt wird.Method for operating an evaporative scattered light detector characterized in that both the atomizing gas and the eluent heated becomes. Verfahren zum Betrieb eines Verdampfungsstreulicht-Detektors dadurch gekennzeichnet, dass der Eluentenstrom durch eine Hochdruckpumpe in der Flüssigkeitschromatographie geliefert wird und die Zerstäubung an einem Düsenplättchen sehr kleiner Dicke mit einem Lochdurchmesser zwischen 10 und 100 μm erfolgt. Durch die Entspannung zerreißt sich der Eluentenstrom in gleichmäßig kleine Tröpfchen. Der Eluentenstrom und/oder das Zerstäubergas kann dabei auch vorgewärmt sein.Method for operating an evaporative scattered light detector characterized in that the eluent flow through a high pressure pump in liquid chromatography is delivered and the atomization on a nozzle plate very much small thickness with a hole diameter between 10 and 100 microns. Through the relaxation tears the eluent stream in evenly small Droplet. The eluent stream and / or the Zerstäubergas can also be preheated. Verfahren zum Betrieb eines Verdampfungsstreulicht-Detektors dadurch gekennzeichnet, dass die Verdampfungsstrecke aus einem runden oder eckigen Kanal besteht, der so durch zwei Platten mit Einfräsungen gebildet wird, dass eine vorzugsweise scharfkantige, aber auch runde Prallwand entsteht, die die größeren Tröpfchen abfängt. Die Tröpfchen laufen durch einen mit einem Syphon versehenen Ablauf ab.Method for operating an evaporative scattered light detector, characterized in that the evaporation path consists of a round or square channel, which is formed by two plates with milled grooves, that a preferably sharp-edged, but also round baffle wall is formed, which intercepts the larger droplets. The droplets pass through a siphon Expiration.
DE200410026379 2004-05-29 2004-05-29 Scattered light detector Expired - Fee Related DE102004026379B4 (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4958529A (en) * 1989-11-22 1990-09-25 Vestec Corporation Interface for coupling liquid chromatography to solid or gas phase detectors
US6122055A (en) * 1996-04-09 2000-09-19 Polymer Laboratories Limited ELSD diffuser
US6229605B1 (en) * 2000-03-10 2001-05-08 Alltech Associates, Inc. Evaporative light scattering device
US20010001575A1 (en) * 1997-09-17 2001-05-24 James M. Anderson, Jr. Low temperature adaptor for evaporative light dectection
WO2002018939A2 (en) * 2000-09-02 2002-03-07 Phlogiston Scientific Limited Analyte detection system
US20030086092A1 (en) * 2001-07-11 2003-05-08 Henry Gangloff Method of controlling an evaporative light scattering detector

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4958529A (en) * 1989-11-22 1990-09-25 Vestec Corporation Interface for coupling liquid chromatography to solid or gas phase detectors
US6122055A (en) * 1996-04-09 2000-09-19 Polymer Laboratories Limited ELSD diffuser
US20010001575A1 (en) * 1997-09-17 2001-05-24 James M. Anderson, Jr. Low temperature adaptor for evaporative light dectection
US6229605B1 (en) * 2000-03-10 2001-05-08 Alltech Associates, Inc. Evaporative light scattering device
WO2002018939A2 (en) * 2000-09-02 2002-03-07 Phlogiston Scientific Limited Analyte detection system
US20030086092A1 (en) * 2001-07-11 2003-05-08 Henry Gangloff Method of controlling an evaporative light scattering detector

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Effective date: 20131203