CN109243962A - A kind of heating device of electrospray ionization mass spectrum transfer capillary - Google Patents

A kind of heating device of electrospray ionization mass spectrum transfer capillary Download PDF

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Publication number
CN109243962A
CN109243962A CN201811148689.7A CN201811148689A CN109243962A CN 109243962 A CN109243962 A CN 109243962A CN 201811148689 A CN201811148689 A CN 201811148689A CN 109243962 A CN109243962 A CN 109243962A
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CN
China
Prior art keywords
flexible heater
thermocouple
heater film
film
capillary
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CN201811148689.7A
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Chinese (zh)
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CN109243962B (en
Inventor
唐紫超
王可
黄如俊
施再发
林水潮
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Xiamen University
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Xiamen University
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00Particle spectrometers or separator tubes
    • H01J49/02Details
    • H01J49/04Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
    • H01J49/0431Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components for liquid samples
    • H01J49/0445Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components for liquid samples with means for introducing as a spray, a jet or an aerosol
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00Particle spectrometers or separator tubes
    • H01J49/02Details
    • H01J49/04Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
    • H01J49/0468Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components with means for heating or cooling the sample

Abstract

A kind of heating device of electrospray ionization mass spectrum transfer capillary, is related to mass spectral analysis field.Equipped with flexible heater film, thermocouple and fixed sleeving component;The flexible heater film is metal electric heating film, and the outside of flexible heater film is polyimides insulation film, and the inside of flexible heater film is metal foil resistance circuit;The thermocouple is for measuring transfer capillary heating temperature;The fixed sleeving component is made of two identical aluminum semicircular pillar body rods, is set on the axial cross section of fixed sleeving component there are two semi-circular recesses, described two semi-circular recesses are used for constant transmissions capillary and thermocouple;Two panels flexible heater film is clipped in the middle by the installation of fixed sleeving component alignment, fixed sleeving component, and transfer capillary and thermocouple are fixed in semi-circular recesses, and is wrapped up and being heated by two panels flexible heater film.

Description

A kind of heating device of electrospray ionization mass spectrum transfer capillary
Technical field
The present invention relates to mass spectral analysis fields, more particularly, to a kind of heating device of electrospray ionization mass spectrum transfer capillary.
Background technique
Mass spectrum ([1] El-Aneed, A.;Cohen,A.;Banoub,J.Applied Spectroscopy Reviews It 2009,44,210) is a kind of widely applied instrument analysis means, primary structure includes ion source, ion transport device, quality Analyzer, signal detection system and vacuum system etc..Sample initially enters ion source and is ionized, and enters by ion transport device Mass analyzer, ion are successively separated and are detected according to mass-to-charge ratio, generate mass spectrogram.Electrospray ionisation technology (ESI) is one Kind atmospheric pressure fluid sample ionization technique.During electron spray, sample is introduced into the capillary with high voltage, from The other end sprays, and forms electrification droplet and enters transmitting device, is analyzed detection after gradually ionizing.Due to ionization process temperature With can form multiple-charged ion, electrospray techniques are widely used in the analysis detection of large biological molecule, cluster substance etc..
Ion transport device is particularly significant to electrospray ionization mass spectrum.On the one hand, ion transport device needs to pass through multi-level differential Vacuum degree transition between guaranteeing from mass spectrum entrance to mass spectrometer;On the other hand, ion transport device undertake to enter mass spectrum Charged drop carry out the task of desolvation and ionization.Damaed cordition and kinetic energy of the sample in ion transport device Distribution situation all can produce instrument detection sensitivity and resolution ratio and directly affect.Common ion transmission part, which mainly has, to be added Thermo-capillary, Skimmer, ring electrode group, radio frequency multi-pole, ion funnel etc..Wherein, heating capillary, which is one, to be added The capillary device of heat.Sample drop enters in capillary, and solvent accelerates volatilization under heat effect, promotes sample ionization. Capillary is heated because of its good desolvation, be frequently utilized for mass spectrum entrance to level-one vacuum chamber vacuum transition and sample Product transmission.The size of capillary directly affects vacuum degree ([2] Guo Changjuan of chamber;Huang Zhengxu;Gao Wei;Glue intelligent blueness;Zhou Zhen; Huang,Z.;Gao,W.;Zhan,H.;Zhou, Z. analysis test journal 2008,339);The temperature for adjusting capillary then can be effective Improve efficiency of transmission of the sample in capillary, to influence sensitivity ([3] Page, J.S. of Mass Spectrometer Method;Kelly, R.T.;Tang,K.;Smith,R.D.Journal of the American Society for Mass Spectrometry 2007,18,1582)。
Complete heating capillary device includes capillary, metal sleeve and heating temperature-controlled member.Metallic sheath pipe sleeve is in hair Outside tubule, capillary is fixed and is heated to facilitate.Common heating temperature control setting is on metal sleeve cross section It is punched around capillary, is inserted into heating tube and thermocouple respectively.The setting easily causes capillary uneven heating, and at thermocouple There are certain temperature difference at capillary, cause temperature control inaccurate.Another kind setting is that heating tape is wound on metal sleeve, makes hair Tubule is uniformly heated, but this processing still can not effectively solve the problems, such as the former temperature control inaccuracy.
Summary of the invention
The purpose of the present invention is to provide can solve electrospray ionization mass spectrum transfer capillary uneven heating and temperature control is not allowed to ask A kind of heating device of electrospray ionization mass spectrum transfer capillary of topic.
The present invention is equipped with flexible heater film, thermocouple and fixed sleeving component;The flexible heater film is metal electric heating Film, the outside of flexible heater film are polyimides insulation film, and the inside of flexible heater film is metal foil resistance circuit; The thermocouple is for measuring transfer capillary heating temperature;The fixed sleeving component is by two identical aluminum semicircular pillars Body rod forms, and is set on the axial cross section of fixed sleeving component there are two semi-circular recesses, described two semi-circular recesses are used for solid Determine transfer capillary and thermocouple;Fixed sleeving component alignment installation, during two panels flexible heater film is clipped in by fixed sleeving component Between, transfer capillary and thermocouple are fixed in semi-circular recesses, and are wrapped up and being heated by two panels flexible heater film.
The length of the flexible heater film can be 100mm, and width can be 15mm, and thickness can be 0.2mm, be able to achieve larger curved Folding, and can at 200 DEG C of highest steady operation.
The K-type thermocouple that diameter is 3mm can be used in the thermocouple.
The cylinder length of described two identical aluminum semicircular pillar body rods can be 100mm, and half circular diameter can be 10mm.
The beneficial effects of the present invention are: the present invention can be evenly heated the transfer capillary of electrospray ionization mass spectrum, and temperature Control is accurate.Existing heating device carries out indirect heating to transfer capillary by fixed sleeving, and the present invention uses flexible heater Film package transfer capillary is heated, and heating film surface and transfer capillary are in close contact, and keeps transfer capillary heated more Uniformly.In addition, the present invention places thermocouple close to transfer capillary, and wrapped up by same flexible heater film, flexible heater Film fever is more uniform, therefore the temperature-measuring results of thermocouple and the actual temperature of transfer capillary are very close, effectively improve The situation for having device thermometric inaccurate.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the embodiment of the present invention.
Specific embodiment
The present invention will be further described below with reference to the drawings.
Fixed sleeving component 1, the 1st flexible heater film 2, the 2nd flexible heater film 3 and thermocouple 4.
As shown in Figure 1, the embodiment of the present invention is equipped with fixed sleeving component 1, the 1st flexible heater film 2, the 2nd flexible heater film 3, thermocouple 4 and transfer capillary 5;1st flexible heater film 2 and the 2nd flexible heater film 3 are metal electric heating film, and the 1st is soft Property heating film 2 and the outside of the 2nd flexible heater film 3 be polyimides insulation film, the 1st flexible heater film the 2 and the 2nd it is flexible plus The inside of hotting mask 3 is metal foil resistance circuit;The thermocouple 4 is for measuring 5 heating temperature of transfer capillary;It is described solid Determine sheath assembly 1 to be made of two identical aluminum semicircular pillar body rods, set on the axial cross section of fixed sleeving component 1 there are two Semi-circular recesses, described two semi-circular recesses are used for constant transmissions capillary 5 and thermocouple 4;The alignment peace of fixed sleeving component 1 1st flexible heater film 2 and the 2nd flexible heater film 3 are clipped in the middle by dress, fixed sleeving component 1, transfer capillary 5 and thermocouple 4 It is fixed in semi-circular recesses, and is wrapped up and being heated by two panels flexible heater film.
The length of 1st flexible heater film 2 and the 2nd flexible heater film 3 be 100mm, width 15mm, with a thickness of 0.2mm is able to achieve larger bending, and the steady operation at 200 DEG C of highest.
The thermocouple 4 uses diameter for the K-type thermocouple of 3mm.
The cylinder length of described two identical aluminum semicircular pillar body rods is 100mm, and half circular diameter is 10mm.
The length of the transfer capillary 5 is 100mm, outer diameter 1.6mm, internal diameter 0.5mm, and stainless steel is located at and adds The center of thermal.Fixed sleeving component 1 is made of a root long 100mm, the aluminum metallic rod of diameter 10mm.For fixed peace Fill transfer capillary 5 and thermocouple 4, the center of metallic rod radial section and eccentric position process respectively diameter be 2mm and 3.4mm's runs through through-hole, through hole center spacing 3mm.Metallic rod is cut apart to get solid to being used as along two through hole is central axial Determine one group of semicircular pillar body rod of sheath assembly 1.The 1st flexible heater film is covered on the cutting section of a semicircular pillar body rod 2, transfer capillary 5 and thermocouple 4 are placed in the 1st flexible heater film 2, the groove being respectively clamped on semicircular pillar body section, Transfer capillary 5 is located at centre, and thermocouple 4 is close in 5 side of transfer capillary.Above transfer capillary 5 and thermocouple 4 again The 2nd flexible heater film 3 is covered, another semicircular pillar body rod of fixed sleeving component 1 is pressed in the 2nd flexible heater film 3, it is right Neat and two semicircular pillar body rods of fastening, by the 1st flexible heater film 2, the 2nd flexible heater film 3, transfer capillary 5 and thermocouple 4 It is fixed between fixed sleeving component 1, entire heating device is just installed, and passes through the 1st flexible heater film 2, the 2nd flexible heater Film 3 and thermocouple 4 can realize being evenly heated and accurate temperature control to transfer capillary 5.

Claims (4)

1. a kind of heating device of electrospray ionization mass spectrum transfer capillary, it is characterised in that be equipped with flexible heater film, thermocouple and consolidate Determine sheath assembly;The flexible heater film is metal electric heating film, and the outside of flexible heater film is polyimides insulation film, The inside of flexible heater film is metal foil resistance circuit;The thermocouple is for measuring transfer capillary heating temperature;Institute It states fixed sleeving component to be made of two identical aluminum semicircular pillar body rods, the axial cross section of fixed sleeving component is equipped with two A semi-circular recesses, described two semi-circular recesses are used for constant transmissions capillary and thermocouple;Fixed sleeving component alignment peace Two panels flexible heater film is clipped in the middle by dress, fixed sleeving component, and transfer capillary and thermocouple are fixed on semi-circular recesses In, and wrapped up and being heated by two panels flexible heater film.
2. a kind of heating device of electrospray ionization mass spectrum transfer capillary as described in claim 1, it is characterised in that the flexibility adds The length of hotting mask is 100mm, width 15mm, with a thickness of 0.2mm.
3. a kind of heating device of electrospray ionization mass spectrum transfer capillary as described in claim 1, it is characterised in that the thermocouple Use diameter for the K-type thermocouple of 3mm.
4. a kind of heating device of electrospray ionization mass spectrum transfer capillary as described in claim 1, it is characterised in that described two phases The cylinder length of same aluminum semicircular pillar body rod is 100mm, and half circular diameter is 10mm.
CN201811148689.7A 2018-09-29 2018-09-29 A kind of heating device of electrospray ionization mass spectrum transfer capillary Active CN109243962B (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3888107A (en) * 1969-10-08 1975-06-10 Dow Chemical Co Differential thermal analysis cell assembly
US5504327A (en) * 1993-11-04 1996-04-02 Hv Ops, Inc. (H-Nu) Electrospray ionization source and method for mass spectrometric analysis
CN102103126A (en) * 2009-12-16 2011-06-22 中国科学院大连化学物理研究所 On-line continuous detection sample injector for mass spectrometer and application thereof
CN203519572U (en) * 2013-09-04 2014-04-02 北京普析通用仪器有限责任公司 Transmission device and gas chromatography-mass spectrometry system
US20150060566A1 (en) * 2013-08-30 2015-03-05 Shimadzu Corporation Ionization probe
US20160035557A1 (en) * 2011-11-02 2016-02-04 Micromass Uk Limited Multi Inlet For Solvent Assisted Inlet Ionisation
CN106706817A (en) * 2017-03-15 2017-05-24 厦门宜柱科技有限公司 Capillary liquid chromatographic column temperature control device

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3888107A (en) * 1969-10-08 1975-06-10 Dow Chemical Co Differential thermal analysis cell assembly
US5504327A (en) * 1993-11-04 1996-04-02 Hv Ops, Inc. (H-Nu) Electrospray ionization source and method for mass spectrometric analysis
CN102103126A (en) * 2009-12-16 2011-06-22 中国科学院大连化学物理研究所 On-line continuous detection sample injector for mass spectrometer and application thereof
US20160035557A1 (en) * 2011-11-02 2016-02-04 Micromass Uk Limited Multi Inlet For Solvent Assisted Inlet Ionisation
US20150060566A1 (en) * 2013-08-30 2015-03-05 Shimadzu Corporation Ionization probe
CN203519572U (en) * 2013-09-04 2014-04-02 北京普析通用仪器有限责任公司 Transmission device and gas chromatography-mass spectrometry system
CN106706817A (en) * 2017-03-15 2017-05-24 厦门宜柱科技有限公司 Capillary liquid chromatographic column temperature control device

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