WO2009095494A1 - Thermal conductivity detector - Google Patents

Thermal conductivity detector Download PDF

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Publication number
WO2009095494A1
WO2009095494A1 PCT/EP2009/051106 EP2009051106W WO2009095494A1 WO 2009095494 A1 WO2009095494 A1 WO 2009095494A1 EP 2009051106 W EP2009051106 W EP 2009051106W WO 2009095494 A1 WO2009095494 A1 WO 2009095494A1
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WO
WIPO (PCT)
Prior art keywords
filament
thermal conductivity
conductivity detector
channel
silicon
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PCT/EP2009/051106
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German (de)
French (fr)
Inventor
Udo Gellert
Arno Steckenborn
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Siemens Aktiengesellschaft
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Publication of WO2009095494A1 publication Critical patent/WO2009095494A1/en

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • G01N27/14—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of an electrically-heated body in dependence upon change of temperature
    • G01N27/18—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of an electrically-heated body in dependence upon change of temperature caused by changes in the thermal conductivity of a surrounding material to be tested

Definitions

  • the invention relates to a heat conductivity detector with an electrically heatable filament, which is mounted in the middle of a channel flow around a fluid and is held at its two ends to two channels crossing the electrically conductive carriers.
  • thermal conductivity detector is known from EP 1381854 Bl.
  • Thermal conductivity detectors are used to detect certain liquid or gaseous substances (fluids) by means of their
  • Substance-typical thermal conductivity and are used in particular in gas chromatography.
  • the substances to be detected are after their chromatographic separation successively passed in a channel at a arranged there and electrically heated filament, depending on the thermal conductivity of the passing substance more or less heat is dissipated from the filament to the channel wall and the filament accordingly cools more or less , By cooling the filament, its electrical resistance changes, which is detected.
  • the filament is usually arranged in a measuring bridge which contains further resistors and a further filament in a further channel through which a reference fluid flows.
  • the detection sensitivity of the thermal conductivity detector is greater the greater the temperature difference between the filament and the channel wall, with high temperatures affect the life of the filament.
  • the sensitivity also depends on the specific electrical resistance of the heating filament, because it gives the total resistance for a given geometry of the heating filament. The greater this total resistance, the greater the detection sensitivity.
  • the filament consists of gold and / or platinum.
  • the service life of the filament is in need of improvement because of the relatively low melting temperature of gold.
  • the filament resistance achievable with gold is low at approx. 15 to 25 ohms and limits the detection sensitivity. To a filament resistance of typically
  • the gold thread must be realized in its dimensions very thin ( ⁇ 0.3 microns) and narrow (typically 6 microns) with a length of 1 mm.
  • filigree dimensions lead to a very small heat capacity and thus a very short response time, but also to a very low robustness.
  • hydrogen sulfide-containing fluids can destroy the gold thread.
  • Platinum has a much higher melting temperature than gold and five times the resistivity with almost the same temperature coefficient of electrical resistance.
  • the advantage of platinum is its chemical inertness, which, however, makes the production in thin-film technology very difficult. Another disadvantage is the catalytic effect of platinum in gas mixtures containing hydrogen and hydrocarbons.
  • the avoidance of these problems takes place in that, in the case of the thermal conductivity detector of the type specified in the introduction, the filament and the supports consist of doped silicon.
  • the melting point of silicon is higher than that of gold, so that very high heating temperatures can be selected without affecting the service life of the filament. Due to the property of silicon becoming intrinsic at high temperatures, the filament is largely protected against overheating.
  • Silicon is more than a thousand times larger than that of gold, so that a high detection sensitivity is achieved.
  • the electrical resistance of the base material can over the doping can be adjusted within wide limits.
  • the doping is chosen so that the resistance is as low as possible in order to provide the thermal conductivity detector with practical operating voltages (well below 100 V) and thus the temperature coefficient of electrical resistance as high as possible. This can be realized in the field of doping of approximately 1-10 15 cm “3 to 1-10 17 cm" 3.
  • the dimensions of the silicon filament must be chosen to be significantly larger in accordance with the higher base resistance, resulting in an overall much more robust structure; typical dimensions are 10 x 10 microns for the cross section of the filament.
  • SOI silicon on insulator
  • the support holding the filament are preferably formed with the interposition of a silicon dioxide layer on a support plate of silicon with a groove contained therein, wherein the channel of the channel and a further groove in one on the support plate resting cover plate is formed.
  • the filament has an oxidized surface of silicon dioxide which is chemically inert to hydrogen sulfide.
  • FIG. 2 shows the same thermal conductivity detector in cross-section (H-II ').
  • a cover plate 3 On a support plate 1 with a channel 2 contained therein is a cover plate 3 with a further groove 4 such that both channels 2 and 4 together form a channel 5 with a circular cross-section here.
  • a filament 6 In the middle of the channel 5 extends in the longitudinal direction of a filament 6, which is held at its two ends to two the channel 5 traversing electrically conductive carriers 7 and 8. The filament 6 is acted upon for heating via the two carriers 7 and 8 with an electric current.
  • the carrier plate 1 is first formed from a silicon substrate, on which an insulating layer 9 of silicon dioxide is applied. On the silicon dioxide layer 9, a layer of doped silicon is then applied, which later forms the carrier 7 and 8 and the filament 6.
  • etching processes by patterning the silicon substrate, the silicon dioxide layer 9 and the layer of doped silicon, the carriers 7 and 8 and the filament 6 are formed and the channel 2 is formed in the carrier plate 1.
  • the carrier 7 and 8 can be dispensed with a stay of the silicon dioxide layer 9 as support for the carrier 7 and 8.
  • the support plate 1 and the cover plate 3 are joined together, wherein formed in them grooves 2 and 4 form the channel 5.
  • the filament 6 receives a hydrogen sulfide-resistant surface of silicon dioxide.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
  • Investigating Or Analyzing Materials Using Thermal Means (AREA)

Abstract

A thermal conductivity detector comprises an electrically heatable filament, which is disposed in the center of a channel so that fluid can flow around it and, for this purpose, is held on the two ends thereof on two electrically conductive carriers traversing the channel. In order to achieve a long service life and inertness toward chemically corrosive gas mixtures, the filament (6) and the carriers (7, 8) are made of doped silicon.

Description

Beschreibungdescription
Wärmeleitfähigkeitsdetektorthermal conductivity detector
Die Erfindung betrifft einen Wärmeleitfähigkeitsdetektor mit einem elektrisch beheizbaren Heizfaden, der in der Mitte eines Kanals von einem Fluid umströmbar gelagert ist und dazu an seinen beiden Enden an zwei den Kanal durchquerenden elektrisch leitenden Trägern gehalten ist.The invention relates to a heat conductivity detector with an electrically heatable filament, which is mounted in the middle of a channel flow around a fluid and is held at its two ends to two channels crossing the electrically conductive carriers.
Ein derartiger Wärmeleitfähigkeitsdetektor ist aus der EP 1381854 Bl bekannt.Such a thermal conductivity detector is known from EP 1381854 Bl.
Wärmeleitfähigkeitsdetektoren dienen zum Nachweis bestimmter flüssiger oder gasförmiger Stoffe (Fluide) anhand ihrerThermal conductivity detectors are used to detect certain liquid or gaseous substances (fluids) by means of their
Stofftypischen Wärmeleitfähigkeit und werden insbesondere in der Gaschromatographie eingesetzt. Dazu werden die nachzuweisenden Stoffe nach ihrer chromatographischen Trennung nacheinander in einem Kanal an einem dort angeordneten und elektrisch beheizten Heizfaden vorbeigeführt, wobei je nach Wärmeleitfähigkeit des vorbeiströmenden Stoffes mehr oder weniger Wärme von dem Heizfaden auf die Kanalwandung abgeleitet wird und der Heizfaden dementsprechend mehr oder weniger abkühlt. Durch die Abkühlung des Heizfadens ändert sich des- sen elektrischer Widerstand, was detektiert wird. Dazu ist der Heizfaden üblicherweise in einer Messbrücke angeordnet, die weitere Widerstände und einen weiteren Heizfaden in einem von einem Referenzfluid durchströmten weiteren Kanal enthält.Substance-typical thermal conductivity and are used in particular in gas chromatography. For this purpose, the substances to be detected are after their chromatographic separation successively passed in a channel at a arranged there and electrically heated filament, depending on the thermal conductivity of the passing substance more or less heat is dissipated from the filament to the channel wall and the filament accordingly cools more or less , By cooling the filament, its electrical resistance changes, which is detected. For this purpose, the filament is usually arranged in a measuring bridge which contains further resistors and a further filament in a further channel through which a reference fluid flows.
Die Detektionsempfindlichkeit des Wärmeleitfähigkeitsdetektors ist umso größer je größer die Temperaturdifferenz zwischen dem Heizfaden und der Kanalwandung ist, wobei hohe Temperaturen die Standzeit des Heizfadens beeinträchtigen. Die Empfindlichkeit hängt auch von dem spezifischen elektri- sehen Widerstand des Heizfadens ab, weil dadurch bei vorgegebener Geometrie des Heizfadens dessen Gesamtwiderstand gegeben ist. Je größer dieser Gesamtwiderstand ist, umso größer ist auch die Detektionsempfindlichkeit . Schließlich können chemisch aggressive Fluide den Heizfaden angreifen und zersetzen .The detection sensitivity of the thermal conductivity detector is greater the greater the temperature difference between the filament and the channel wall, with high temperatures affect the life of the filament. The sensitivity also depends on the specific electrical resistance of the heating filament, because it gives the total resistance for a given geometry of the heating filament. The greater this total resistance, the greater the detection sensitivity. Finally, you can Chemically aggressive fluids attack the filament and decompose.
Bei dem aus der oben genannten EP 1381854 Bl bekannten Wärme- leitfähigkeitsdetektor besteht der Heizfaden aus Gold und/ oder Platin. Die Standzeit des Heizfadens ist wegen der relativ niedrigen Schmelztemperatur von Gold verbesserungsbedürftig. Der mit Gold realisierbare Heizfadenwiderstand ist mit ca. 15 bis 25 Ohm niedrig und begrenzt die Detektionsempfind- lichkeit. Um einen Heizfadenwiderstand von typischerweiseIn the case of the thermal conductivity detector known from the abovementioned EP 1381854 B1, the filament consists of gold and / or platinum. The service life of the filament is in need of improvement because of the relatively low melting temperature of gold. The filament resistance achievable with gold is low at approx. 15 to 25 ohms and limits the detection sensitivity. To a filament resistance of typically
20 Ohm zu erreichen muss der Goldfaden in seinen Abmessungen sehr dünn (< 0,3 μm) und schmal (typ. 6 μm) bei einer Länge von 1 mm realisiert werden. Solch filigrane Abmessungen führen zu einer sehr kleinen Wärmekapazität und damit einer sehr kurzen Ansprechzeit, aber auch zu einer sehr geringen Robustheit. Nicht zuletzt können Schwefelwasserstoffhaltige Fluide den Goldfaden zerstören. Platin hat eine sehr viel höhere Schmelztemperatur als Gold und den fünffachen spezifischen Widerstand bei fast gleichem Temperaturkoeffizienten des elektrischen Widerstands. Der Vorteil von Platin ist seine chemische Inertheit, wodurch sich allerdings die Herstellung in Dünnfilmtechnologie als sehr schwierig erweist. Ein weiterer Nachteil ist die katalytische Wirkung von Platin in Gasgemischen, die Wasserstoff und Kohlenwasserstoffe enthal- ten.To achieve 20 ohms, the gold thread must be realized in its dimensions very thin (<0.3 microns) and narrow (typically 6 microns) with a length of 1 mm. Such filigree dimensions lead to a very small heat capacity and thus a very short response time, but also to a very low robustness. Last but not least, hydrogen sulfide-containing fluids can destroy the gold thread. Platinum has a much higher melting temperature than gold and five times the resistivity with almost the same temperature coefficient of electrical resistance. The advantage of platinum is its chemical inertness, which, however, makes the production in thin-film technology very difficult. Another disadvantage is the catalytic effect of platinum in gas mixtures containing hydrogen and hydrocarbons.
Gemäß der Erfindung erfolgt die Vermeidung dieser Probleme dadurch, dass bei dem Wärmeleitfähigkeitsdetektor der eingangs angegebenen Art der Heizfaden und die Träger aus do- tiertem Silizium bestehen. Der Schmelzpunkt von Silizium ist höher als der von Gold, so dass sehr hohe Heiztemperaturen gewählt werden können, ohne die Standzeit des Heizfadens zu beeinträchtigen. Durch die Eigenschaft von Silizium bei hohen Temperaturen intrinsisch zu werden, ist der Heizfaden weit- gehend gegen Überhitzung geschützt. Der Kaltwiderstand vonAccording to the invention, the avoidance of these problems takes place in that, in the case of the thermal conductivity detector of the type specified in the introduction, the filament and the supports consist of doped silicon. The melting point of silicon is higher than that of gold, so that very high heating temperatures can be selected without affecting the service life of the filament. Due to the property of silicon becoming intrinsic at high temperatures, the filament is largely protected against overheating. The cold resistance of
Silizium ist um mehr als das tausendfache größer als der von Gold, so dass eine hohe Detektionsempfindlichkeit erreicht wird. Der elektrische Widerstand des Grundmaterials kann über die Dotierung in weiten Bereichen eingestellt werden. Vorzugsweise wird die Dotierung so gewählt, dass der Widerstand möglichst niedrig liegt, um den Wärmeleitfähigkeitsdetektor mit praktischen Betriebsspannungen (deutlich unter 100 V) versorgen zu können und damit der Temperaturkoeffizient des elektrischen Widerstands möglichst hoch ausfällt. Dies ist im Bereich der Dotierung von ca. 1-1015 cm"3 bis 1-1017 cm"3 realisierbar. Die Abmessungen des Siliziumheizfadens müssen entsprechend dem höheren Grundwiderstand deutlich größer gewählt werden, wodurch sich ein insgesamt sehr viel robusterer Aufbau ergibt; typische Abmessungen liegen bei 10 x 10 μm für den Querschnitt des Heizfadens.Silicon is more than a thousand times larger than that of gold, so that a high detection sensitivity is achieved. The electrical resistance of the base material can over the doping can be adjusted within wide limits. Preferably, the doping is chosen so that the resistance is as low as possible in order to provide the thermal conductivity detector with practical operating voltages (well below 100 V) and thus the temperature coefficient of electrical resistance as high as possible. This can be realized in the field of doping of approximately 1-10 15 cm "3 to 1-10 17 cm" 3. The dimensions of the silicon filament must be chosen to be significantly larger in accordance with the higher base resistance, resulting in an overall much more robust structure; typical dimensions are 10 x 10 microns for the cross section of the filament.
Prinzipiell kann der Heizfaden durch Abscheidung von poly- kristallinem Silizium oder aus einkristallinem Silizium, vorzugsweise aus SOI-Wafermaterial (SOI = Silicon on Insula- tor) hergestellt werden. Durch chemische Prozesse an Korngrenzen sind freitragende Heizfäden aus polykristallinem Material mechanisch und elektrisch weniger langzeitstabil .In principle, the filament can be produced by depositing polycrystalline silicon or monocrystalline silicon, preferably from SOI wafer material (SOI = silicon on insulator). By chemical processes at grain boundaries are self-supporting filaments of polycrystalline material mechanically and electrically less long-term stability.
Insbesondere im Hinblick auf eine mikromechanische Herstellung des erfindungsgemäßen Wärmeleitfähigkeitsdetektors sind vorzugsweise die den Heizfaden haltenden Träger unter Zwischenlage einer Siliziumdioxid-Schicht auf einer Trägerplatte aus Silizium mit einer darin enthaltenen Rinne ausgebildet, wobei der Kanal von der Rinne und einer weiteren Rinne in einer auf der Trägerplatte aufliegenden Abdeckplatte gebildet ist .With particular regard to a micromechanical production of the thermal conductivity detector according to the invention, the support holding the filament are preferably formed with the interposition of a silicon dioxide layer on a support plate of silicon with a groove contained therein, wherein the channel of the channel and a further groove in one on the support plate resting cover plate is formed.
Vorzugsweise weist der Heizfaden eine durch Oxidation gebildete Oberfläche aus Siliziumdioxid auf, das sich gegenüber Schwefelwasserstoff chemisch inert verhält.Preferably, the filament has an oxidized surface of silicon dioxide which is chemically inert to hydrogen sulfide.
Im Weiteren wird die Erfindung anhand eines in den Figuren gezeigten Ausführungsbeispiels des erfindungsgemäßen Wärmeleitfähigkeitsdetektors erläutert, wobei Figur 1 den Wärmeleitfähigkeitsdetektor im Längsschnitt (I-I1) undIn the following, the invention will be explained with reference to an embodiment of the thermal conductivity detector according to the invention shown in the figures, wherein Figure 1 shows the heat conductivity detector in longitudinal section (II 1 ) and
Figur 2 denselben Wärmeleitfähigkeitsdetektor im Quer- schnitt (H-II') zeigen.FIG. 2 shows the same thermal conductivity detector in cross-section (H-II ').
Auf einer Trägerplatte 1 mit einer darin enthaltenen Rinne 2 liegt eine Abdeckplatte 3 mit einer weiteren Rinne 4 derart auf, dass beide Rinnen 2 und 4 zusammen einen Kanal 5 mit hier kreisrundem Querschnitt bilden. In der Mitte des Kanals 5 erstreckt sich in dessen Längsrichtung ein Heizfaden 6, der an seinen beiden Enden an zwei den Kanal 5 durchquerenden elektrisch leitenden Trägern 7 und 8 gehalten ist. Der Heizfaden 6 wird zum Aufheizen über die beiden Träger 7 und 8 mit einem elektrischen Strom beaufschlagt.On a support plate 1 with a channel 2 contained therein is a cover plate 3 with a further groove 4 such that both channels 2 and 4 together form a channel 5 with a circular cross-section here. In the middle of the channel 5 extends in the longitudinal direction of a filament 6, which is held at its two ends to two the channel 5 traversing electrically conductive carriers 7 and 8. The filament 6 is acted upon for heating via the two carriers 7 and 8 with an electric current.
Zur mikromechanischen Herstellung des Wärmeleitfähigkeitsdetektors wird zunächst die Trägerplatte 1 aus einem Siliziumsubstrat gebildet, auf dem eine Isolierschicht 9 aus Siliziumdioxid aufgebracht wird. Auf der Siliziumdioxid- Schicht 9 wird anschließend eine Schicht aus dotiertem Silizium aufgebracht, die später die Träger 7 und 8 und den Heizfaden 6 bildet. In Ätzprozessen werden durch Strukturieren des Siliziumsubstrats, der Siliziumdioxid-Schicht 9 und der Schicht aus dotiertem Silizium die Träger 7 und 8 und der Heizfaden 6 gebildet und die Rinne 2 in der Trägerplatte 1 ausgeformt. Bei der Ausbildung der Träger 7 und 8 kann auf ein Verbleiben der Siliziumdioxid-Schicht 9 als Unterstützung für die Träger 7 und 8 verzichtet werden. Schließlich werden die Trägerplatte 1 und die Abdeckplatte 3 zusammengefügt, wobei die in ihnen ausgeformten Rinnen 2 und 4 den Kanal 5 bilden. Durch Oxidieren erhält der Heizfaden 6 eine gegenüber Schwefelwasserstoff resistente Oberfläche aus Siliziumdioxid. For micromechanical production of the thermal conductivity detector, the carrier plate 1 is first formed from a silicon substrate, on which an insulating layer 9 of silicon dioxide is applied. On the silicon dioxide layer 9, a layer of doped silicon is then applied, which later forms the carrier 7 and 8 and the filament 6. In etching processes, by patterning the silicon substrate, the silicon dioxide layer 9 and the layer of doped silicon, the carriers 7 and 8 and the filament 6 are formed and the channel 2 is formed in the carrier plate 1. In the formation of the carrier 7 and 8 can be dispensed with a stay of the silicon dioxide layer 9 as support for the carrier 7 and 8. Finally, the support plate 1 and the cover plate 3 are joined together, wherein formed in them grooves 2 and 4 form the channel 5. By oxidation, the filament 6 receives a hydrogen sulfide-resistant surface of silicon dioxide.

Claims

Patentansprüche claims
1. Wärmeleitfähigkeitsdetektor mit einem elektrisch beheizbaren Heizfaden (6), der in der Mitte eines Kanals (5) von einem Fluid umströmbar gelagert ist und dazu an seinen beiden Enden an zwei den Kanal (5) durchquerenden elektrisch leitenden Trägern (7, 8) gehalten ist, dadurch gekennzeichnet, dass der Heizfaden (6) und die Träger (7, 8) aus dotiertem Silizium bestehen.1. Thermal conductivity detector with an electrically heatable filament (6) which is mounted in the middle of a channel (5) flow around a fluid and held at its two ends to two the channel (5) passing through electrically conductive carriers (7, 8) is, characterized in that the filament (6) and the carrier (7, 8) made of doped silicon.
2. Wärmeleitfähigkeitsdetektor nach Anspruch 1, dadurch gekennzeichnet, dass die den Heizfaden (6) haltenden Träger (7, 8) unter Zwischenlage einer Siliziumdioxid-Schicht (9) auf einer Trägerplatte (1) aus Silizium mit einer darin enthalte- nen Rinne (2) ausgebildet sind, wobei der Kanal (5) von der Rinne (2) und einer weiteren Rinne (4) in einer auf der Trägerplatte (1) aufliegenden Abdeckplatte (3) gebildet ist.2. Thermal conductivity detector according to claim 1, characterized in that the filament (6) holding carrier (7, 8) with the interposition of a silicon dioxide layer (9) on a support plate (1) made of silicon with a groove contained therein (2 ), wherein the channel (5) of the channel (2) and a further channel (4) in a on the support plate (1) resting cover plate (3) is formed.
3. Wärmeleitfähigkeitsdetektor nach Anspruch 1 oder 2, da- durch gekennzeichnet, dass der Heizfaden (6) eine Oberfläche aus Siliziumdioxid aufweist.3. Thermal conductivity detector according to claim 1 or 2, character- ized in that the filament (6) has a surface of silicon dioxide.
4. Wärmeleitfähigkeitsdetektor nach Anspruch 1, 2 oder 3, dadurch gekennzeichnet, dass der Heizfaden (6) aus einkristal- linem Silizium besteht.4. Thermal conductivity detector according to claim 1, 2 or 3, characterized in that the filament (6) consists of monocrystalline silicon.
5. Wärmeleitfähigkeitsdetektor nach Anspruch 4, dadurch gekennzeichnet, dass der Heizfaden (6) aus einkristallinem Silizium eines SOI-Wafers hergestellt ist.5. Thermal conductivity detector according to claim 4, characterized in that the filament (6) is made of monocrystalline silicon of an SOI wafer.
6. Wärmeleitfähigkeitsdetektor nach Anspruch 1, 2 oder 3, dadurch gekennzeichnet, dass der Heizfaden 6 aus polykristallinem Silizium besteht. 6. Thermal conductivity detector according to claim 1, 2 or 3, characterized in that the filament 6 consists of polycrystalline silicon.
PCT/EP2009/051106 2008-01-31 2009-01-30 Thermal conductivity detector WO2009095494A1 (en)

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WO2011064310A1 (en) * 2009-11-25 2011-06-03 Siemens Aktiengesellschaft Method and arrangement for gas chromatographic analysis of a gas sample
DE102009055785B3 (en) * 2009-11-25 2011-09-01 Siemens Aktiengesellschaft Method for gas chromatographic analysis of gas sample, involves generating peak for analyte such as hydrogen sulfide by differentiating chromatogram at location of analyte
US9116160B2 (en) 2009-11-25 2015-08-25 Siemens Aktiengesellschaft Method and arrangement for gas chromatographic analysis of a gas sample
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EP3096133A1 (en) 2015-05-20 2016-11-23 Siemens Aktiengesellschaft Thermal conductivity detector
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