DE29613330U1 - Arrangement for tempering a capillary separation column for gas chromatography - Google Patents
Arrangement for tempering a capillary separation column for gas chromatographyInfo
- Publication number
- DE29613330U1 DE29613330U1 DE29613330U DE29613330U DE29613330U1 DE 29613330 U1 DE29613330 U1 DE 29613330U1 DE 29613330 U DE29613330 U DE 29613330U DE 29613330 U DE29613330 U DE 29613330U DE 29613330 U1 DE29613330 U1 DE 29613330U1
- Authority
- DE
- Germany
- Prior art keywords
- separation column
- tube
- arrangement
- gas chromatography
- resistance layer
- 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.)
- Expired - Lifetime
Links
- 238000000926 separation method Methods 0.000 title claims description 30
- 238000004817 gas chromatography Methods 0.000 title claims description 5
- 238000005496 tempering Methods 0.000 title description 2
- 239000004642 Polyimide Substances 0.000 claims description 7
- 229920001721 polyimide Polymers 0.000 claims description 7
- 239000010453 quartz Substances 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 239000004922 lacquer Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims 1
- 238000000576 coating method Methods 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
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
- G01N30/26—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
-
- 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
- G01N2030/3007—Control of physical parameters of the fluid carrier of temperature same temperature for whole column
-
- 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
- G01N2030/3015—Control of physical parameters of the fluid carrier of temperature temperature gradients along column
-
- 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
- G01N2030/3053—Control of physical parameters of the fluid carrier of temperature using resistive heating
- G01N2030/3061—Control of physical parameters of the fluid carrier of temperature using resistive heating column or associated structural member used as heater
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
Description
GH 96 G 44=48 DEGH 96 G 44=48 DE
Be s ehre ibungHonor
Anordnung zur Temperierung einer Kapillartrennsäule für die Gas chromat ographi e
5Arrangement for temperature control of a capillary separation column for gas chromatography
5
Die Erfindung betrifft eine Anordnung zur Temperierung einer Kapillartrennsäule für die Gaschromatographie.The invention relates to an arrangement for tempering a capillary separation column for gas chromatography.
Kapillartrennsäulen mit geringem Innendurchmesser von beispielsweise 0,15 mm ermöglichen Trennungen von Gasgemischen im Zeitbereich von Sekunden bis wenigen Minuten. Werden diese Trennsäulen temperaturprogrammiert betrieben, so kann die Geschwindigkeit der Trennung erhöht werden, es können Proben mit größerem Siedebereich getrennt werden, die Nachweisgrenze von Komponenten mit höherem Siedepunkt verbessert sich und das Analysenende kann ohne Rückspülung herbeigeführt werden. Wegen der kurzen Analysenzeiten auf den genannten Trennsäulen werden entsprechend schnelle Temperaturprogramme benötigt.Capillary separation columns with a small inner diameter of, for example, 0.15 mm enable gas mixtures to be separated in a time range from seconds to a few minutes. If these separation columns are operated with a temperature program, the speed of the separation can be increased, samples with a larger boiling range can be separated, the detection limit of components with a higher boiling point is improved and the end of the analysis can be achieved without backflushing. Due to the short analysis times on the separation columns mentioned, correspondingly fast temperature programs are required.
Aus "Journal of Chromatographie Science", Bd. 33, November 1995, Seiten 601 bis 605, ist es bekannt, Trennsäulen mit einer dünnen, elektrisch leitenden Farbe zu beschichten und diese durch Wärmezufuhr zu trocknen. Zum Temperieren der Trennsäule wird durch die so erhaltene leitende Schicht ein elektrischer Strom geschickt.From "Journal of Chromatography Science", Vol. 33, November 1995, pages 601 to 605, it is known to coat separation columns with a thin, electrically conductive paint and to dry it by applying heat. To control the temperature of the separation column, an electric current is passed through the conductive layer thus obtained.
Handelsübliche Trennsäulen bestehen aus einem polyimidummantelten Quarzrohr, dessen Innenoberfläche mit einem viskosen Flüssigkeitsfilm als Trennphase belegt ist. Damit ergibt sich das Problem, daß beim Aufbringen einer leitendenCommercially available separation columns consist of a polyimide-coated quartz tube, the inner surface of which is covered with a viscous liquid film as a separation phase. This results in the problem that when applying a conductive
96 G 4448 DE , ,. „96 G 4448 DE , ,. „
Schicht auf die Trennsäule durch die nachfolgende Wärmebehandlung die Trennphase beschädigt werden kann.layer on the separation column, the separation phase may be damaged by the subsequent heat treatment.
Die erfindungsgemäße Anordnung zur Temperierung einer Kapillartrennsäule für die Gaschromatographie vermeidet dieses Problem durch ein Rohr, in dem die Trennsäule eingeführt ist und das außen eine elektrisch beheizbare Widerstandsschicht trägt. Da die Trennsäule erst nach dem Fertigstellen der Widerstandsschicht in das Rohr eingeführt wird, kann es zu keiner Beschädigung der Trennphase bei der Wärmebehandlung der Widerstandsschicht kommen.The arrangement according to the invention for controlling the temperature of a capillary separation column for gas chromatography avoids this problem by means of a tube into which the separation column is inserted and which has an electrically heatable resistance layer on the outside. Since the separation column is only inserted into the tube after the resistance layer has been completed, the separation phase cannot be damaged during the heat treatment of the resistance layer.
Bei dem Rohr handelt es sich vorzugsweise um ein polyimidummanteltes Quarzrohr, auf dessen Polyimidoberfläche ein kohlenstoffpartikelhaltiger Lack aufgebracht und eingebrannt ist.The tube is preferably a polyimide-coated quartz tube, onto whose polyimide surface a lacquer containing carbon particles is applied and baked.
Eine Einstellung eines vorgegebenen Temperaturprofils entlang der Trennsäule wird in vorteilhafter Weise dadurch ermöglicht, daß die Widerstandsschicht einen über die Rohrlänge variierenden Querschnitt aufweist. Dies kann in der Weise realisiert werden, daß die Widerstandsschicht mit einer über die Rohrlänge variierenden Schichtdicke aufgebracht wird oder spiralförmig auf dem Rohr aufgebracht wird, wobei die spiralförmige Widerstandsbahn bezüglich ihrer Dicke oder Breite variiert.Setting a predetermined temperature profile along the separation column is advantageously made possible by the resistance layer having a cross-section that varies over the length of the tube. This can be achieved by applying the resistance layer with a layer thickness that varies over the length of the tube or by applying it to the tube in a spiral shape, with the spiral resistance path varying in terms of its thickness or width.
Um Wärmeverluste soweit wie möglich zu verringern und ein genaues Temperaturprograitim einstellen zu können, ist das Rohr mit der Trennsäule vorzugsweise in einem isotherm betriebenen Ofen angeordnet.In order to reduce heat losses as much as possible and to be able to set a precise temperature program, the tube with the separation column is preferably arranged in an isothermally operated furnace.
96 G 4448 DE96 G 4448 EN
Zur weiteren Erläuterung der Erfindung wird im folgenden auf die Figuren der Zeichnung Bezug genommen,- im einzelnen zeigen: To further explain the invention, reference is made to the figures of the drawing, which show in detail:
Figur 1 einen Abschnitt einer Trennsäule in einem eine Widerstandsschicht tragenden Rohr undFigure 1 shows a section of a separation column in a tube carrying a resistance layer and
Figur 2 das Rohr mit der Trennsäule in einem isotherm beheizbaren Ofen.Figure 2 the tube with the separation column in an isothermally heated oven.
Figur 1 zeigt einen Abschnitt einer Trennsäule 1, die aus einem Quarzrohr 2 besteht, welches einen äußeren Polyimidmantel 3 trägt und dessen Innenoberfläche mit einer Trennphase 4, bestehend aus einem viskosen Flüssigkeitsfilm, belegt ist. Die Trennsäule 1 mit einem Außendurchmesser von etwa 250 &mgr;&pgr;&agr; ist in einem Quarzrohr 5 mit einem Innendurchmesser von etwa 320 &mgr;&tgr;&eegr; eingeführt. Das Quarzrohr 5 weist einen äußeren Polyimidmantel 6 auf, auf dem ein kohlenstoffpartikelhaltiger Lack aufgebracht und eingebrannt ist. Durch die so erzeugte Widerstandsschicht 7 wird zur Temperierung der Trennsäule 1 ein elektrischer Strom geschickt. Um ein vorgegebenes Temperaturprofil einstellen zu können, weist die Widerstandsschicht 7 einen über die Länge des Rohres 5 variierenden Querschnitt auf. Hierzu kann entweder die Dicke der Widerstandsschicht 7 variieren oder die Widerstandsschicht 7 in Form einer spiralförmigen Bahn auf dem Rohr 5 aufgebracht sein, wobei die Dicke oder Breite der Bahn variiert.Figure 1 shows a section of a separation column 1, which consists of a quartz tube 2, which has an outer polyimide jacket 3 and whose inner surface is covered with a separation phase 4, consisting of a viscous liquid film. The separation column 1 with an outer diameter of about 250 μπα is inserted into a quartz tube 5 with an inner diameter of about 320 μπη. The quartz tube 5 has an outer polyimide jacket 6, on which a lacquer containing carbon particles is applied and baked. An electric current is sent through the resistance layer 7 thus produced to control the temperature of the separation column 1. In order to be able to set a predetermined temperature profile, the resistance layer 7 has a cross-section that varies over the length of the tube 5. For this purpose, either the thickness of the resistance layer 7 can vary or the resistance layer 7 can be applied to the tube 5 in the form of a spiral path, whereby the thickness or width of the path varies.
Figur 2 zeigt schematisch einen GasChromatographen 8 mit einem isotherm betriebenen Ofen 9, in dem die Trennsäule 1 mit dem sie umgebenden Rohr 5 angeordnet ist. Die zur GasanalyseFigure 2 shows a schematic of a gas chromatograph 8 with an isothermal oven 9 in which the separation column 1 with the surrounding tube 5 is arranged. The
GR 96 G 4448 DEGR 96 G 4448 DE
weiterhin erforderlichen Gerätekomponenten, an denen die Trennsäule 1 angeschlossen ist, sind mit 10 bezeichnet. Das Quarzrohr 5 mit der Widerstandsschicht 7 ist an einer einstellbaren Heizstromquelle 11 angeschlossen.The other required device components to which the separation column 1 is connected are designated 10. The quartz tube 5 with the resistance layer 7 is connected to an adjustable heating current source 11.
Claims (4)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE29613330U DE29613330U1 (en) | 1996-08-01 | 1996-08-01 | Arrangement for tempering a capillary separation column for gas chromatography |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE29613330U DE29613330U1 (en) | 1996-08-01 | 1996-08-01 | Arrangement for tempering a capillary separation column for gas chromatography |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE29613330U1 true DE29613330U1 (en) | 1996-09-26 |
Family
ID=8027286
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DE29613330U Expired - Lifetime DE29613330U1 (en) | 1996-08-01 | 1996-08-01 | Arrangement for tempering a capillary separation column for gas chromatography |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE29613330U1 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7228067B2 (en) * | 2000-11-15 | 2007-06-05 | Thermo Finnigan Italia S.P.A. | Chromatography column assembly with woven tubular mesh heater element |
| DE102017110258B3 (en) * | 2017-05-11 | 2018-11-08 | Sim Scientific Instruments Manufacturer Gmbh | Chemical analyzer with a medium processing unit and medium processing unit |
| DE102021109060A1 (en) | 2021-04-12 | 2022-10-13 | Gottfried Wilhelm Leibniz Universität Hannover | Separation column device for a gas chromatograph and gas chromatograph |
-
1996
- 1996-08-01 DE DE29613330U patent/DE29613330U1/en not_active Expired - Lifetime
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7228067B2 (en) * | 2000-11-15 | 2007-06-05 | Thermo Finnigan Italia S.P.A. | Chromatography column assembly with woven tubular mesh heater element |
| DE102017110258B3 (en) * | 2017-05-11 | 2018-11-08 | Sim Scientific Instruments Manufacturer Gmbh | Chemical analyzer with a medium processing unit and medium processing unit |
| DE102021109060A1 (en) | 2021-04-12 | 2022-10-13 | Gottfried Wilhelm Leibniz Universität Hannover | Separation column device for a gas chromatograph and gas chromatograph |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| R207 | Utility model specification |
Effective date: 19961107 |
|
| R150 | Utility model maintained after payment of first maintenance fee after three years |
Effective date: 20000209 |
|
| R151 | Utility model maintained after payment of second maintenance fee after six years |
Effective date: 20021204 |
|
| R152 | Utility model maintained after payment of third maintenance fee after eight years |
Effective date: 20041220 |
|
| R071 | Expiry of right |