WO2017137517A1 - Dispositif pour la liaison à haute pression et l'étanchéification de capillaires en silice fondue pour des liquides en microtechnologie et en nanotechnologie - Google Patents

Dispositif pour la liaison à haute pression et l'étanchéification de capillaires en silice fondue pour des liquides en microtechnologie et en nanotechnologie Download PDF

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Publication number
WO2017137517A1
WO2017137517A1 PCT/EP2017/052927 EP2017052927W WO2017137517A1 WO 2017137517 A1 WO2017137517 A1 WO 2017137517A1 EP 2017052927 W EP2017052927 W EP 2017052927W WO 2017137517 A1 WO2017137517 A1 WO 2017137517A1
Authority
WO
WIPO (PCT)
Prior art keywords
fused silica
silica capillary
outer sleeve
compound according
intermediate sleeve
Prior art date
Application number
PCT/EP2017/052927
Other languages
German (de)
English (en)
Inventor
Werner DÖBELIN
Original Assignee
Döbelin Werner
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 Döbelin Werner filed Critical Döbelin Werner
Publication of WO2017137517A1 publication Critical patent/WO2017137517A1/fr

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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
    • G01N30/60—Construction of the column
    • G01N30/6004—Construction of the column end pieces
    • G01N30/6026—Fluid seals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08—Selective adsorption, e.g. chromatography
    • B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
    • B01D15/22—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the construction of the 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
    • G01N30/60—Construction of the column
    • G01N30/6095—Micromachined or nanomachined, e.g. micro- or nanosize

Definitions

  • the invention relates to a fused silica capillary connection to
  • the invention is therefore based on the object to provide a system to produce fused silica capillary easily and safely, which preferably fit on the existing standard ports and / or still the requirements for the tightness of the HPLC in particular the nano and micro ultra High pressure HPLC is fair.
  • the first crimping region ensures a sealing connection between the intermediate sleeve and the outer sleeve.
  • the clamping area a sealing connection between the
  • the outer sleeve Ensuring intermediate sleeve and the fused silica capillary.
  • the outer sleeve encloses the intermediate sleeve in the first and / or in the second
  • the fused silica capillary is characterized by the invention
  • Fused silica capillary securely and tightly held in the intermediate sleeve of the fused silica capillary connection.
  • the fused silica capillary compound according to the invention is not limited to the combination of a clamping region and a crimping region or crimping regions, but each crimping region can be replaced by a plurality of crimping regions or the clamping region can be replaced by a plurality of clamping regions, which on the one hand results in a better sealing effect with greater space requirements and bigger
  • a preferred fused silica capillary compound exhibits at least one
  • the outer sleeve is preferably crimped at several points, in particular simultaneously by means of a crimping tool.
  • a particularly advantageous fused silica capillary connection has an outer sleeve enclosing the intermediate sleeve in a crimping area, sealingly connected to one another by crimping.
  • a special seal is achieved in that by means of an intermediate sleeve with several clamping / crimping sections the sleeve on the one hand with the standard cone (ferrules) seals the sleeve to the standard connection and on the other hand, the intermediate sleeve with a metal outer sleeve so crimps This is because the internal fused silica capillary sticks so tightly that the fused silica capillary can not push out of the intermediate sleeve or liquid can escape due to the internal pressure acting on the front side of the fused silica capillary.
  • Capillary compound made of metal, in particular made of stainless steel, whereby a particularly reliable sealing effect by crimping and a particularly robust and durable fused silica capillary connection is made possible.
  • a particularly advantageous fused silica capillary connection shows an intermediate sleeve of solid plastic, in particular of PEEK.
  • Polyetheretherketori is a high temperature resistant thermoplastic. He belongs to the group of polyaryletherketones. The plastic is chosen so that it with resistance to the pressure through the
  • Crimping or clamping by the conical clamping area can be deformed so that a reliable sealing connection to the outer sleeve or the fused silica capillary is achieved.
  • PEEK has proved to be particularly suitable for this purpose.
  • this intermediate sleeve exhibits a stepped structure which is suitable for the outer sleeve, in particular made of metal, sealingly enclosing the cylindrical area of lesser diameter by crimping.
  • the sealing effect is achieved in particular by crimping or alternatively or additionally by clamping.
  • This design makes it possible to form the outer diameter of the outer sleeve preferably not larger than the larger diameter of the intermediate sleeve in particular equal to this and thereby achieve a particularly good handling of the arrangement of intermediate sleeve and outer sleeve. This good handling also ensures safe production of the fused silica capillary connection.
  • an outer sleeve in particular made of metal, with an end face which is provided with an opening for receiving the fused silica capillary, it is possible to form the fused silica capillary particularly safe against damage and particularly dense.
  • a preferred fused silica capillary shows an outer sleeve, which is guided in a hole of a hollow screw for screwing into a counterpart of a compound and which preferably in particular in a hole of a clamping cone, which is arranged in the connecting direction of the hollow screw in front of the outer sleeve is.
  • fused silica capillary a protective sheath hose which is pulled over the fused silica capillary and / or over the intermediate sleeve and / or the outer sleeve and is fixed in particular by crimping.
  • Preferred crimping also has proven to be gluing or welding.
  • a particularly preferred development of the fused silica capillary connection shows an intermediate sleeve and an inner fused silica capillary, which are crimped together in particular crimped together several times, wherein optionally the outer sleeve is additionally crimped sealingly with the inner intermediate sleeve in particular repeatedly crimped together.
  • the sealing of the fused silica capillary connection is independent of an additional standard cone seal. This can advantageously be dispensed with the use of a standard cone and the inventive fused silica capillary connection are very compact and simple.
  • a fused silica capillary according to the invention is provided with a fused silica capillary compound according to the invention at one or both ends.
  • the fused silica capillary according to the invention also shows the advantages of the fused silica capillary compound according to the invention.
  • the invention also relates to an HPLC column with an outer sleeve
  • This HPLC column according to the invention proves to be so dense that it can be used as a UHPLC column. It has proved to be particularly advantageous to further develop this HPLC column according to the invention such that at least one filter element and / or HPLC packing material is arranged in the one outer sleeve between the ends of the two fused silica capillaries.
  • the outer sleeve can be extended so that is introduced and crimped on both sides of an intermediate sleeve with an inner fused silica capillary, so that creates a sealed to the outside cavity, which previously with
  • Filter elements and HPLC packaging material is filled as a stationary phase, so that so that a particularly compact HPLC / UHPLC column is produced.
  • This arrangement ensures a particularly safe operation of the HPLC column, in particular, this shows a falsified by small disturbances measurement or analysis result.
  • This tempering unit is preferably provided with at least one Peltier element and / or with at least one PTC element.
  • PTC elements or Peltier elements in the vicinity of the HPLC column, it has proven particularly useful to arrange them flat on the outer sleeve. Both solutions allow a targeted heating and thus an efficient and fast adjusting the desired process temperature of the HPLC column, because the HPLC column according to the invention with the fused silica capillary according to the invention makes it possible to dispense with massive fittings such as clamping cones or hollow screws, which are characterized by a high heat capacity and thereby rapid adaptation and
  • Prevent regulation of the process temperature By further developing this HPLC column according to the invention, it is possible to variably select the process temperature during the analysis by means of chromatography and thereby to use a new hitherto inaccessible process parameter (temperature) for controlling the separation properties of the HPLC column.
  • a new hitherto inaccessible process parameter temperature
  • FIG. 1 shows a metal outer sleeve
  • Fig. 2 shows an intermediate sleeve made of PEEK with fused silica capillary
  • Fig. 3 shows a crimped outer and inner sleeve with fused silica
  • FIG. 4 a sleeve with clamping cone (ferrules)
  • FIG. 5 a sleeve with cone and hollow screw
  • Fig. 6 is a connection counterpart
  • Fig. 7 shows an HPLC / UHPLC column
  • Fig. 1 shows the outer sleeve 1 made of stainless steel with a
  • Crimping area on the total length of the outside 2a. 2 shows the intermediate sleeve 6 made of PEEK with the introduced up to the end surface 16 of the intermediate sleeve to the opening 13 fused silica capillary 3, with the standard
  • the intermediate sleeve 6 shows a stepped structure.
  • the smaller-diameter cylindrical portion 5 serves as the insertion portion for the outer sleeve-1, which then encloses the smaller-diameter cylindrical portion 5 and defines the crimping portion 20.
  • FIG. 3 shows that over the entire length crimped outer sleeve 1 wherein the gap is compressed by the crimping between the intermediate sleeve 6 and fused silica capillary 3 and between outer sleeve 1 and intermediate sleeve 6 so that also by
  • Fig. 4 shows the standard cone 8 (ferrules) 1/16 "on the clamping portion 10 of the intermediate sleeve 6.
  • the task of the metal cone 8 is primarily responsible for the sealing of the intermediate sleeve 6 of Figure 2 and the inner cone 1 1 of Figure 6.
  • Fig. 7 shows an HPLC column according to the invention.
  • the extended outer sleeve 1 of the HPLC column is connected to the inserted on both sides PEEK intermediate sleeves 15 and the fused silica capillaries 3 with the filter elements 13 and the HPLC packing material 14, wherein the outer sleeve 1 on both sides with the
  • the process temperature can be selected dynamically during the analysis and is thus available as a new and additional parameter for optimizing the analysis.

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)
  • Silicon Compounds (AREA)

Abstract

L'invention concerne une liaison de capillaires en silice fondue (1) pour réaliser la liaison à haute pression et l'étanchéification de capillaires en silice fondue pour des liquides en microtechnologie et en nanotechnologie. La liaison de capillaires en silice fondue (3) selon l'invention présente une douille intermédiaire (6) de manière à présenter une zone de serrage conique (10) et/ou une première zone de sertissage (20) et une seconde zone de sertissage (20) séparée de celle-ci, la zone de serrage (10) ou les zones de sertissage (20) agissant sur la même douille intermédiaire (6) et permettant ainsi d'étanchéifier les capillaires en silice fondue (3). La première ou la seconde zone de sertissage (20) assure selon l'invention une liaison étanche entre les capillaires en silice fondue (3) et la douille intermédiaire (6), tandis que la zone de serrage (10) ou la seconde ou la première zone de sertissage (20) assure une liaison étanche entre la douille intermédiaire (6) et la douille extérieure (1). En variante, il est également possible que la zone de serrage (10) assure une liaison étanche entre la douille intermédiaire (6) et les capillaires en silice fondue (3).
PCT/EP2017/052927 2016-02-09 2017-02-09 Dispositif pour la liaison à haute pression et l'étanchéification de capillaires en silice fondue pour des liquides en microtechnologie et en nanotechnologie WO2017137517A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CH00171/16A CH712103A2 (de) 2016-02-09 2016-02-09 Fused-Silica-Kapillarverschraubung.
CH171/16 2016-02-09

Publications (1)

Publication Number Publication Date
WO2017137517A1 true WO2017137517A1 (fr) 2017-08-17

Family

ID=58228067

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP2017/052927 WO2017137517A1 (fr) 2016-02-09 2017-02-09 Dispositif pour la liaison à haute pression et l'étanchéification de capillaires en silice fondue pour des liquides en microtechnologie et en nanotechnologie

Country Status (2)

Country Link
CH (1) CH712103A2 (fr)
WO (1) WO2017137517A1 (fr)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009088663A1 (fr) * 2008-01-02 2009-07-16 Waters Technologies Corporation Ensembles de conduits de chromatographie en phase liquide pourvus de joints haute pression
WO2010133192A1 (fr) * 2009-05-22 2010-11-25 Dionex Softron Gmbh Unité d'enfichage et système de liaison permettant la liaison de capillaires, notamment en chromatographie en phase liquide à hautes performances
WO2013032832A1 (fr) * 2011-08-26 2013-03-07 Waters Technologies Corporation Ensemble de colonnes de chromatographie
DE102012110991A1 (de) * 2012-11-15 2014-05-15 Dionex Softron Gmbh Steckereinheit und Verbindungssystem zum Verbinden von Kapillaren, insbesondere für die Hochleistungsflüssigkeitschromatographie

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009088663A1 (fr) * 2008-01-02 2009-07-16 Waters Technologies Corporation Ensembles de conduits de chromatographie en phase liquide pourvus de joints haute pression
WO2010133192A1 (fr) * 2009-05-22 2010-11-25 Dionex Softron Gmbh Unité d'enfichage et système de liaison permettant la liaison de capillaires, notamment en chromatographie en phase liquide à hautes performances
WO2013032832A1 (fr) * 2011-08-26 2013-03-07 Waters Technologies Corporation Ensemble de colonnes de chromatographie
WO2013032833A1 (fr) * 2011-08-26 2013-03-07 Waters Technologies Corporation Ensembles de conduits de chromatographie liquide pourvus de joints d'étanchéité haute pression
DE102012110991A1 (de) * 2012-11-15 2014-05-15 Dionex Softron Gmbh Steckereinheit und Verbindungssystem zum Verbinden von Kapillaren, insbesondere für die Hochleistungsflüssigkeitschromatographie

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Publication number Publication date
CH712103A2 (de) 2017-08-15

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