CN110487884A - A kind of application method of the transference tube for complex sample separation analysis - Google Patents

A kind of application method of the transference tube for complex sample separation analysis Download PDF

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Publication number
CN110487884A
CN110487884A CN201811412003.0A CN201811412003A CN110487884A CN 110487884 A CN110487884 A CN 110487884A CN 201811412003 A CN201811412003 A CN 201811412003A CN 110487884 A CN110487884 A CN 110487884A
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China
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ion
gas
migration area
application method
transference tube
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CN201811412003.0A
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CN110487884B (en
Inventor
陈创
李海洋
王卫国
蒋丹丹
陈红
厉梅
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Dalian Institute of Chemical Physics of CAS
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Dalian Institute of Chemical Physics of CAS
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
    • G01N27/622Ion mobility spectrometry

Abstract

The application method that the present invention discloses a kind of transference tube for complex sample separation analysis realizes the successive ionization of different compounds in complex sample using the difference of proton affinity based on the ionization depression effect in atmospheric pressure molecular ion reaction mechanism.The present invention is conducive to eliminate the influence that complex matrices accurately identify ion mobility spectrometry and detect target compound, improves the selectivity and sensitivity of ion mobility spectrometry.

Description

A kind of application method of the transference tube for complex sample separation analysis
Technical field
The present invention relates to the methods that ion mobility spectrometry separates analysis complex sample, further relate in the reaction of atmospheric pressure molecular ion Ionization depression effect, it is specifically a kind of using compound proton affinity height difference to complex sample carry out separation point The method of analysis.
Background technique
Ion mobility spectrometry is a kind of mainstream detection technique for being widely used in explosive, drugs, chemical warfare agent.In recent years, With the development of atmospheric pressure ionization technique, the application range of ion mobility spectrometry has been expanded to clinical expiratory air detection, environment Many chemical analysis fields such as pollutant monitoring, food safety detection, process analysis procedure analysis.
In these diversified application fields, the analysis object of ion mobility spectrometry is usually associated with complicated matrix.One Aspect, the resolution capability of ion mobility spectrometry itself still only has 50 or so at present, significantly limits ion mobility spectrometry to complexity Object ion accurately identifies ability in background.On the other hand, ion mobility spectrometry generallys use continuous purging sample introduction at present Mode, this input mode usually along with serious ionization depression effect, cause object that can not be ionized, influence ion and move Move the detection sensitivity of spectrum.
In order to improve the selectivity and detection sensitivity of ion mobility spectrometry, the present invention is based on atmospheric pressure molecular ions to react machine Ionization depression effect in reason realizes the successive ionization of different compounds in complex sample using the difference of proton affinity, The influence that complex matrices accurately identified to ion mobility spectrometry and detected target compound is eliminated, the selectivity of ion mobility spectrometry is improved And detection sensitivity.
Summary of the invention:
It is an object of the invention to ionize depression effect using caused by proton affinity difference, provided for ion mobility spectrometry A kind of device and method of separation analysis complication and object sample.
To achieve the goals above, the technical solution adopted by the present invention are as follows:
A kind of application method of the transference tube for complex sample separation analysis, the transference tube is one hollow Tubular cavity, the axial direction along transference tube are disposed with ion source, ionized region, ion gate, migration area from left to right With ion receiving pole.
It is provided with air inlet in the side wall surface of ion source one end in ionized region, air inlet is through airflow channel and a two-way valve Door is connected.
Ion receiving pole one end is provided with drift gas air inlet in migration area, is arranged in migration area close to ion gate one end Gas outlet.
Ion source is that any ion source of protonated ion can be generated.
When transference tube works, the drift gas air inlet that gas is arranged from migration area is floated all the way and is entered inside migration area, and Flow out transference tube in gas outlet along the direction contrary with ion flight through being arranged on migration area;In a preset period of time Time span in, two-way valve is opened, and sample to be tested gas enters in ionized region through two-way valve;In prefixed time interval knot Shu Hou, two-way valve are closed.
The height difference of the respective proton affinity of compounds not of the same race contained in sample to be tested gas in ionized region, The protonated ion successively generated with ion source occurs Proton-Transfer Reactions and forms product ion, and product ion is opened through the period Ion gate enters migration area, ion receiving pole is successively reached under the driving of migration area internal electric field, and be converted into current strength Spectrogram information output to the time.
The time span of the preset period of time is between 0.001~5ms.
Ion source is radioactivity63Ni, radioactivity235Am, radioactivity3H, corona discharge ion source, introduce ketone dopant Any one in photoion source.
The ion gate is any one of Bradbury-Neilson type and Tyndall-Powell type ion gate.
Floating gas to be includes O2、N2、CO2、H2, any gas including the gases such as Ar or two kinds or more admixture of gas.
It is an advantage of the invention that
The present invention is conducive to eliminate the influence that complex matrices accurately identify ion mobility spectrometry and detect target compound, mentions The selectivity and sensitivity of macroion migration spectrum.
Detailed description of the invention
Fig. 1, a kind of transference tube for complex sample separation analysis.
Wherein: 1 --- ion source;2 --- ionized region;3 --- ion gate;4 --- migration area;5 --- ion receiving pole; 6 --- sample air inlet;7 --- two-way valve;8 --- drift gas air inlet;9 --- air inlet.
Specific embodiment
The invention will now be described in further detail with reference to the accompanying drawings.
Embodiment 1
A kind of transference tube for complex sample separation analysis is as shown in fig. 1.Transference tube is one hollow Cylindrical cavity, the axial direction along transference tube are ion source 1, ionized region 2, ion gate 3,4 and of migration area from left to right Ion receiving pole 5;Sample air inlet 6 is arranged close to 1 one end of ion source in ionized region 2, and air inlet 6 is through airflow channel and a two-way valve Door 7 is connected;Drift gas air inlet 8 is arranged close to 5 one end of ion receiving pole in migration area 4, in migration area 4 close to 3 one end of ion gate Gas outlet 9 is set.
Ion source 1 uses radioactivity63Ni generates (H in the positive-ion mode2O)nH+Ion;Ion gate 3 is Tyndall- Powell type ion gate, 3 aperture plate spacing of ion gate are 1mm, and aperture plate voltage difference is 100V when enabling, and shutdown voltage is 150V;Electricity Internal diameter from area 2 is 20mm, and 2 length 20mm of ionized region, 2 internal electric intensity of ionized region is 60V/mm;The internal diameter of migration area 4 is 30mm, 4 length 60mm of migration area, 4 internal electric intensity of migration area are 60V/mm.
When transference tube works, at time zero (t=0s), two-way valve 7 is opened, and sample to be tested gas is through two-way valve Door 7 enters in ionized region 2, sample gas flow velocity 60mL/min;After timing 10s, two-way valve 7 is closed.
The difference of height of the respective proton affinity of compounds not of the same race contained in sample to be tested gas in ionized region 2 (H that is different, successively being generated with ion source 12O)nH+Proton-Transfer Reactions occurs and forms product ion, ion gate 3 is opened according to every 15ms Product in ionized region 2 is discharged into migration area 4 by the timing for opening 200us, and in migration area, 4 internal electric field driving ion successively reaches Ion receiving pole 5, and be converted into current strength and the spectrogram information of time is exported.
While the above process carries out, the air inlet 8 that gas is arranged from migration area 4 is floated all the way and is entered inside migration area 2, And transference tube is flowed out in the gas outlet 9 along the direction contrary with ion flight through being arranged on migration area 4.
Float gas be by silica gel, active carbon, molecular sieve filtration pure air.

Claims (5)

1. a kind of application method of the transference tube for complex sample separation analysis, it is characterised in that:
The transference tube be a hollow tube-shape cavity, along the axial direction of transference tube be disposed with from left to right from Component, ionized region, ion gate, migration area and ion receiving pole;
Air inlet is provided in the side wall surface of ion source one end in ionized region, air inlet is through airflow channel and a two-way valve phase Connection;
Ion receiving pole one end is provided with drift gas air inlet in migration area, outlet is set close to ion gate one end in migration area Mouthful;
Ion source is that any ion source of protonated ion can be generated;
When transference tube works, the drift gas air inlet that gas is arranged from migration area is floated all the way and is entered inside migration area, and along Flow out transference tube in gas outlet of the direction contrary with ion flight through being arranged on migration area;A preset period of time when Between in length, two-way valve is opened, and sample to be tested gas enters in ionized region through two-way valve;After preset period of time, two Port valve door is closed;
The height difference of the respective proton affinity of compounds not of the same race contained in sample to be tested gas in ionized region, successively Proton-Transfer Reactions occurs with the protonated ion that ion source generates and forms product ion, the ion that product ion is opened through the period Door enters migration area, ion receiving pole is successively reached under the driving of migration area internal electric field, and be converted into current strength clock synchronization Between spectrogram information output.
2. application method according to claim 1, it is characterised in that: the time span of the preset period of time be 0.001~ Between 5ms.
3. application method according to claim 1, it is characterised in that: ion source is radioactivity63Ni, radioactivity235Am, it puts Penetrating property3H, corona discharge ion source, be introduced into the photoion source of ketone dopant any one.
4. application method according to claim 1, it is characterised in that: the ion gate is Bradbury-Neilson type With Tyndall-Powell type ion gate any one.
5. application method according to claim 1, it is characterised in that: the drift gas be include O2、N2、CO2、H2, Ar etc. Any gas including gas or two kinds or more admixture of gas.
CN201811412003.0A 2018-11-25 2018-11-25 Use method of ion migration tube for complex sample separation and analysis Active CN110487884B (en)

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CN110487884B CN110487884B (en) 2022-01-04

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112485321A (en) * 2020-11-24 2021-03-12 中国科学院大连化学物理研究所 Ion mobility spectrometry determination method for content of ammonia gas in ammonia-containing gas

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19805569C1 (en) * 1998-02-12 1999-10-07 Bruker Saxonia Analytik Gmbh Method for the detection of substance traces with solvent-assisted dosing and ion mobility spectrometer to carry out the method
CN104713940A (en) * 2013-12-13 2015-06-17 中国科学院大连化学物理研究所 Novel on-fingerprint prohibited good spectrum detection device and method and application thereof
CN105632874A (en) * 2014-11-07 2016-06-01 中国科学院大连化学物理研究所 DC non-uniform electric field ion migration tube
CN106841367A (en) * 2015-12-07 2017-06-13 中国科学院大连化学物理研究所 A kind of Ion transfer spectrum detection method of time resolution Dynamic Thermal parsing
CN106872553A (en) * 2015-12-14 2017-06-20 中国科学院大连化学物理研究所 A kind of Propofol detection method for eliminating sevoflurane interference
CN108072694A (en) * 2016-11-17 2018-05-25 中国科学院大连化学物理研究所 A kind of blood concentration assay instrument detecting system
CN108091537A (en) * 2016-11-21 2018-05-29 中国科学院大连化学物理研究所 A kind of ladder Field ion mobility pipe

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19805569C1 (en) * 1998-02-12 1999-10-07 Bruker Saxonia Analytik Gmbh Method for the detection of substance traces with solvent-assisted dosing and ion mobility spectrometer to carry out the method
CN104713940A (en) * 2013-12-13 2015-06-17 中国科学院大连化学物理研究所 Novel on-fingerprint prohibited good spectrum detection device and method and application thereof
CN105632874A (en) * 2014-11-07 2016-06-01 中国科学院大连化学物理研究所 DC non-uniform electric field ion migration tube
CN106841367A (en) * 2015-12-07 2017-06-13 中国科学院大连化学物理研究所 A kind of Ion transfer spectrum detection method of time resolution Dynamic Thermal parsing
CN106872553A (en) * 2015-12-14 2017-06-20 中国科学院大连化学物理研究所 A kind of Propofol detection method for eliminating sevoflurane interference
CN108072694A (en) * 2016-11-17 2018-05-25 中国科学院大连化学物理研究所 A kind of blood concentration assay instrument detecting system
CN108091537A (en) * 2016-11-21 2018-05-29 中国科学院大连化学物理研究所 A kind of ladder Field ion mobility pipe

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112485321A (en) * 2020-11-24 2021-03-12 中国科学院大连化学物理研究所 Ion mobility spectrometry determination method for content of ammonia gas in ammonia-containing gas

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