CN103972020A - Analytical method for ion mobility spectrometry - Google Patents
Analytical method for ion mobility spectrometry Download PDFInfo
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- CN103972020A CN103972020A CN201310039444.1A CN201310039444A CN103972020A CN 103972020 A CN103972020 A CN 103972020A CN 201310039444 A CN201310039444 A CN 201310039444A CN 103972020 A CN103972020 A CN 103972020A
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Abstract
The invention discloses an analytical method for an ion mobility spectrometry. The analytical method includes arranging an ion consumption area between an ionization reaction area and a mobility area of an ion mobility tube. Special organic reagent molecules in the ion consumption area are capable of selectively eliminating interfering ions, so that resolution degree of target ions is increased, and influence on the ionization reaction area and the mobility area is avoided. The invention further provides application of the analytical method in detecting sulfur.
Description
Technical field
The present invention relates to a kind of ion mobility spectrometry analytical method.Taking ion mobility spectrometry as technical support, between the ionization reaction district of transference tube and migration area, an ion consumption location is set, for optionally eliminating interfering ion, when improving separating degree, do not affect the molecule-ionic reaction in ionization reaction district.
Background technology
Ion mobility spectrometry (Ion Mobility Spectrometry, IMS) technology is that the one that 20 century 70s occur separates detection technique, compared with the conventional art such as mass spectrum, chromatogram, it has the features such as simple in structure, highly sensitive, analysis speed is fast, is suitable for on-the-spot use.Ionic migration spectrometer is mainly made up of ionization source, ion gate, migration area and detector.Ion source makes sample molecule, N
2, O
2with steam ionization, the ion of generation is easy to and molecule generation ion molecule reaction, obtains multi-products ion.The ion gate that ion is opened by periodicity under the ordering about of electric field enters migration area, floating gas molecule with the neutrality of adverse current constantly collides, because these ions have different migration rates in electric field, different ions is separated, successively arrive detector.
But the resolution of IMS is lower, the more difficult separation of ion that mobility is approaching, in spectrogram time and occur the phenomenon of overlap of peaks.The organic reagent that optionally adulterates in carrier gas or in floating gas is one of means that address this problem.G.A.Eiceman etc. (G.A.Eiceman et al., Anal.Chim.Acta, 1995,306,21-33), using acetone as dopant, have improved the selectivity that detects 19 kinds of organic phosphorus compounds significantly; (the R.Fern á ndez-Maestre et al. such as R.Fern á ndez-Maestre, RapidCommun.Mass Spectrom., 2012,26,2211 – 2223) by carry out the doping of organic solvent to floating gas, change the product ion structure of analyte, thereby improved peak-peak separating degree.But in the time that organic reagent is doped in carrier gas, it also may suppress the ionization of target compound in eliminating interfering ion; When organic reagent is added on while floating in gas, due to ion in migration area with the intermolecular continuous collision of organic reagent, can impel the broadening of quasi-molecular ions.
The problem of bringing in order to solve the organic reagent place of doping, the present invention arranges ion consumption location between the ionization reaction district of transference tube and migration area, in ion consumption location, add organic reagent molecule, not only can improve selectivity and the peak-peak separating degree of analytical method, and ionization reaction district and migration area not impacted.
Summary of the invention
The invention discloses a kind of ion mobility spectrometry analytical method, between the ionization reaction district of transference tube and migration area, an ion consumption location is set; The generation of ion consumption location is to realize by pass into the gas that contains organic reagent molecule between ionization reaction district and migration area.
Ion mobility spectrometry comprises the transference tube with receiving pole, be provided with near transference tube one end of receiving pole and float gas entrance, be provided with carrier gas inlet away from transference tube one end of receiving pole, be provided with total gas outlet in the transference tube floating between gas entrance and carrier gas inlet;
On the sidewall of transference tube, be provided with the air inlet of the gas that contains organic reagent molecule, air inlet floats between gas entrance and total gas outlet transference tube, in the transference tube at air inlet place, form ion consumption location, the gas that contains organic reagent molecule enters in ion consumption location by this air inlet.
Migration area is consistent with airflow direction in ion consumption location, contrary with airflow direction in ionization reaction district;
All gas in transference tube leaves migration tube by total gas outlet.
When ion mobility spectrometry is positive ion mode, organic reagent is one or two or more kinds in ammonia, acetone;
When ion mobility spectrometry is negative ion mode, organic reagent is one or two or more kinds in carrene, carbon tetrachloride.
The gas that carries organic reagent molecule is one or two or more kinds in air, nitrogen.
In the gas that contains organic reagent molecule, the molar concentration of organic reagent molecule is 0.02-5mol/L.Advantage of the present invention:
The present invention arranges ion consumption location between the ionization reaction district of transference tube and migration area, in ion consumption location, add organic reagent molecule, not only can improve the selectivity of analytical method and the separating degree of peak-peak, and ionization reaction district and migration area not impacted.
Brief description of the drawings
Fig. 1 is one of part-structure schematic diagram of the transference tube that relates in the method;
Fig. 2 be the transference tube that relates in the method part-structure schematic diagram two;
Fig. 3 be the transference tube that relates in the method part-structure schematic diagram three;
Fig. 4 be the transference tube that relates in the method part-structure schematic diagram four;
Fig. 5 be the transference tube that relates in the method part-structure schematic diagram five;
Fig. 6 a is the sulphur IMS collection of illustrative plates of cleaned air while doing carrier gas, and Fig. 6 b is the sulphur IMS collection of illustrative plates while adding carrene in carrier gas;
Fig. 7 is the sulphur IMS figure adding methylene chloride in ion consumption location.
Embodiment
The invention discloses a kind of ion mobility spectrometry analytical method, between the ionization reaction district of transference tube and migration area, an ion consumption location is set; The generation of ion consumption location is to realize by pass into the gas that contains organic reagent molecule between ionization reaction district and migration area.
Ion mobility spectrometry comprises the transference tube with receiving pole, be provided with near transference tube one end of receiving pole and float gas entrance, be provided with carrier gas inlet away from transference tube one end of receiving pole, be provided with total gas outlet in the transference tube floating between gas entrance and carrier gas inlet;
On the sidewall of transference tube, be provided with the air inlet of the gas that contains organic reagent molecule, air inlet floats between gas entrance and total gas outlet transference tube, in the transference tube at air inlet place, form ion consumption location, the gas that contains organic reagent molecule enters in ion consumption location by this air inlet.
Migration area is consistent with airflow direction in ion consumption location, contrary with airflow direction in ionization reaction district;
All gas in transference tube leaves migration tube by total gas outlet.
When ion mobility spectrometry is positive ion mode, organic reagent is one or two or more kinds in ammonia, acetone;
When ion mobility spectrometry is negative ion mode, organic reagent is one or two or more kinds in carrene, carbon tetrachloride.
The gas that carries organic reagent molecule is one or two or more kinds in air, nitrogen.
In the gas that contains organic reagent molecule, the molar concentration of organic reagent molecule is 0.02-5mol/L.
The part-structure schematic diagram of the transference tube relating in the method as Figure 1-5,1 is carrier gas, and 2 is ionization reaction district, and 3 is conducting ring, 4 is dead ring, and 5 is total gas outlet, and 6 is organic reagent gas inlet, 7 is ion gate, and 8 for floating gas, and 9 is ion consumption location.
In Fig. 1, the gas inlet that contains organic reagent molecule is 1, and air inlet airflow direction is 180 degree with the airflow direction of total gas outlet;
In Fig. 2, the gas inlet that contains organic reagent molecule is 1, and air inlet airflow direction is 0 degree with the airflow direction of total gas outlet;
In Fig. 3, the gas inlet that contains organic reagent molecule is 2, and one of them air inlet airflow direction is 180 degree with the airflow direction of total gas outlet, and another air inlet airflow direction is 0 degree with the airflow direction of total gas outlet;
In Fig. 4, the gas inlet that contains organic reagent molecule is 4, and 4 air inlets carry out equal angular circle distribution according to the center line of transference tube.
In Fig. 5, the gas inlet that contains organic reagent molecule is 1, is provided with in the dead ring of this air inlet and is provided with cavity, and this cavity communicates with air inlet, and communicates with ion consumption location by a series of apertures.
Sample is carried and is entered ionization reaction district and be ionized by carrier gas, and all ions are through ion consumption location under the effect of electric field, and interfering ion is eliminated under the effect of organic reagent molecule.Subsequently, the ion gate that ion is opened by periodicity enters migration area, successively arrives receiving pole according to the difference of mobility.
Embodiment 1
Adopt IMS to detect S, carrier gas is periodically switched between the air of cleaned air and doping carrene, and over time as shown in Figure 6 a, the IMS collection of illustrative plates of S as shown in Figure 6 b for the signal strength signal intensity of S.Result shows: in the time that carrene is not adulterated in carrier gas, the reactive ion of IMS is that (in figure, the existence at chloride ion peak is because carrier gas switches to after cleaned air to oxonium ion, migration tube inside still remains carrene), after sulphur molecule and oxonium ion reaction, can generate sulphion, but the transit time of two kinds of ions is very approaching, has occurred overlap peak; In the time adulterating carrene in carrier gas, the reactive ion major part of IMS is chloride ion, and sulphur molecule can not react with chloride ion and generate sulphion, can't detect the signal of S.
As shown in Figure 7, in carrene makes an addition to ion consumption location time, the reactive ion of IMS is oxonium ion, sulfur molecule and oxonium ion react in ionization reaction district, after generating sulphion, enter ion consumption location together with remaining oxonium ion, in this region, oxonium ion can be reacted totally by carrene, and finally only surplus sulphion and chloride ion enter migration area, and therefore on IMS figure, the separating degree of peak-peak is significantly improved.
Ion of the present invention consumption location contains specific organic reagent molecule, can optionally eliminate interfering ion, has not only improved the separating degree of object ion, and has avoided the impact on ionization reaction district and migration area.
Claims (6)
1. an analytical method for ion mobility spectrometry, is characterized in that: between the ionization reaction district of transference tube and migration area, an ion consumption location is set;
The generation of ion consumption location is to realize by pass into the gas that contains organic reagent molecule between ionization reaction district and migration area.
2. analytical method according to claim 1, is characterized in that:
Ion mobility spectrometry comprises the transference tube with receiving pole, be provided with near transference tube one end of receiving pole and float gas entrance, be provided with carrier gas inlet away from transference tube one end of receiving pole, be provided with total gas outlet in the transference tube floating between gas entrance and carrier gas inlet;
On the sidewall of transference tube, be provided with the air inlet of the gas that contains organic reagent molecule, air inlet floats between gas entrance and total gas outlet transference tube, in the transference tube at air inlet place, form ion consumption location, the gas that contains organic reagent molecule enters in ion consumption location by this air inlet.
3. analytical method according to claim 1, is characterized in that:
Migration area is consistent with airflow direction in ion consumption location, contrary with airflow direction in ionization reaction district;
All gas in transference tube leaves migration tube by total gas outlet.
4. analytical method according to claim 1, is characterized in that:
When ion mobility spectrometry is positive ion mode, organic reagent is one or two or more kinds in ammonia, acetone;
When ion mobility spectrometry is negative ion mode, organic reagent is one or two or more kinds in carrene, carbon tetrachloride.
5. according to the analytical method described in claim 1,3 or 4, it is characterized in that: the gas that carries organic reagent molecule is one or two or more kinds in air, nitrogen.
6. according to the analytical method described in claim 1,3 or 4, it is characterized in that: in the gas that contains organic reagent molecule, the molar concentration of organic reagent molecule is 0.02-5mol/L.
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| CN201310039444.1A CN103972020A (en) | 2013-01-31 | 2013-01-31 | Analytical method for ion mobility spectrometry |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106770608A (en) * | 2016-11-30 | 2017-05-31 | 云南无线电有限公司 | Improve the method and its process circuit of transference tube interference free performance |
| CN110632164A (en) * | 2019-10-31 | 2019-12-31 | 大连大学 | Method for simultaneously detecting phthalate compounds in food |
| CN110646501A (en) * | 2019-10-31 | 2020-01-03 | 大连大学 | Method for detecting environmental hormone dimethyl phthalate |
| CN111089895A (en) * | 2019-11-29 | 2020-05-01 | 大连大学 | Application of ion mobility spectrometry in rapid detection of phthalate compounds in plastics |
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| US4950893A (en) * | 1989-04-27 | 1990-08-21 | Environmental Technologies Group, Inc. | Method and apparatus for enhanced ion spectra generation and detection in ion mobility spectrometry |
| US5283199A (en) * | 1990-06-01 | 1994-02-01 | Environmental Technologies Group, Inc. | Chlorine dioxide monitor based on ion mobility spectrometry with selective dopant chemistry |
| US20080277575A1 (en) * | 2007-05-08 | 2008-11-13 | Hitachi, Ltd. | Ion mobility spectrometer and ion-mobility-spectrometry/mass-spectrometry hybrid spectrometer |
| CN101382521A (en) * | 2007-09-04 | 2009-03-11 | 中国科学院大连化学物理研究所 | Method for enhancing sensitivity of ionic migration spectrum |
| CN201935894U (en) * | 2010-12-31 | 2011-08-17 | 同方威视技术股份有限公司 | Ion mobility spectrometry and sample injection device used for same |
| CN102318035A (en) * | 2007-07-30 | 2012-01-11 | 粒子监测系统有限公司 | Detection of analytes using ion mobility spectrometry |
| CN102479663A (en) * | 2010-11-30 | 2012-05-30 | 中国科学院大连化学物理研究所 | Ion mobility tube and applications thereof |
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2013
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Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US4950893A (en) * | 1989-04-27 | 1990-08-21 | Environmental Technologies Group, Inc. | Method and apparatus for enhanced ion spectra generation and detection in ion mobility spectrometry |
| US5283199A (en) * | 1990-06-01 | 1994-02-01 | Environmental Technologies Group, Inc. | Chlorine dioxide monitor based on ion mobility spectrometry with selective dopant chemistry |
| US20080277575A1 (en) * | 2007-05-08 | 2008-11-13 | Hitachi, Ltd. | Ion mobility spectrometer and ion-mobility-spectrometry/mass-spectrometry hybrid spectrometer |
| CN102318035A (en) * | 2007-07-30 | 2012-01-11 | 粒子监测系统有限公司 | Detection of analytes using ion mobility spectrometry |
| CN101382521A (en) * | 2007-09-04 | 2009-03-11 | 中国科学院大连化学物理研究所 | Method for enhancing sensitivity of ionic migration spectrum |
| CN102479663A (en) * | 2010-11-30 | 2012-05-30 | 中国科学院大连化学物理研究所 | Ion mobility tube and applications thereof |
| CN201935894U (en) * | 2010-12-31 | 2011-08-17 | 同方威视技术股份有限公司 | Ion mobility spectrometry and sample injection device used for same |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106770608A (en) * | 2016-11-30 | 2017-05-31 | 云南无线电有限公司 | Improve the method and its process circuit of transference tube interference free performance |
| CN110632164A (en) * | 2019-10-31 | 2019-12-31 | 大连大学 | Method for simultaneously detecting phthalate compounds in food |
| CN110646501A (en) * | 2019-10-31 | 2020-01-03 | 大连大学 | Method for detecting environmental hormone dimethyl phthalate |
| CN111089895A (en) * | 2019-11-29 | 2020-05-01 | 大连大学 | Application of ion mobility spectrometry in rapid detection of phthalate compounds in plastics |
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Application publication date: 20140806 |