CN102034668A - Cylindrical ion trap mass spectrometer - Google Patents
Cylindrical ion trap mass spectrometer Download PDFInfo
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- CN102034668A CN102034668A CN201010506093.7A CN201010506093A CN102034668A CN 102034668 A CN102034668 A CN 102034668A CN 201010506093 A CN201010506093 A CN 201010506093A CN 102034668 A CN102034668 A CN 102034668A
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Abstract
The invention relates to a cylindrical ion trap mass spectrometer, which is characterized by comprising an ion source, a cylindrical ion trap, a charge detector and an electromagnetic shielding cover for shielding interference of a radio frequency electric field in the charge detector, wherein the charge detector is arranged at the bottom in a cavity of the electromagnetic shielding cover; a through hole is formed at the central position of the top of the electromagnetic shielding cover; and the ion source pumps a detected sample into the cylindrical ion trap through a sample inlet of the cylindrical ion trap, and the detected sample passes through the through hole of the electromagnetic shielding cover, which is formed below the cylindrical ion trap, and is thrown into the charge detector to be detected. The cylindrical ion trap has small volume and is easy to process, so the structure of the mass spectrometer comprising the ion source, the cylindrical ion trap, the charge detector and the electromagnetic shielding cover is simplified, and the cost is reduced. The mass spectrometer can be widely applied to the quality measurement of various micron-sized particles.
Description
Technical field
The present invention relates to a kind of mass spectrometer, particularly about a kind of cylindrical ion trap mass spectrometer that is used to measure the micron dimension particle.
Background technology
At present, micron and nano particle more and more receive the concern of association areas such as physics, chemistry and biology owing to have special electricity, optics, thermokinetics, chemistry and biological characteristics.Common particulate matter, for example dust, big aerosol, virus, cell etc. all play an important role in the Nature, and therefore the sign to size, quality and the chemical composition of these particulate matters has great importance.
Mass spectrum is a kind of material to be carried out quality determination and analytical method qualitatively, and this method has sensitivity, reaches advantages such as accurate fast, is playing the part of crucial role in the life science in modern age.The material size of modern mass spectrometer energy measurement approximates 100 ten thousand atomic units below 10nm.And the modern head and shoulders above mass spectrometric measuring range of micron particles can not be carried out quality determination to it with traditional mass spectrometer.Extensively be present in the environment owing to the micron particles material simultaneously, and its distributional difference is big, need carries out on-the-spot and real-time analysis.Therefore, need design and have new ionization and ion detection means, and small-sized, portable mass spectrometer is realized the analysis to particulate matter.
In recent years, the determination techniques of micron particles quality is in continuous development.Calendar year 2001 Fuerstenau people such as (Fuerstenau) utilizes electron spray-flight time-electric charge induction pipe mass spectrometer system successfully to measure the virus of some known quality (paddy rice macula lutea virus and the listless virus of tobacco) first, this method rapid and convenient, the mensuration of thousands of virion quality can be finished in half an hour.But because the restriction of faradic detection and ion required time when passing induction tube, its measured quality error is bigger, about about 15%; And the volume ratio of flight time mass spectrum is bigger, is unfavorable for realizing miniaturization.2002 and Cai in 2003 etc. adopt electron spray-quadrupole ion trap-light scattering detector and substance assistant laser desorpted-two quadrupole ion trap-fluorescence detectors that the quality of 0.91 μ m and 1.10 μ m polystyrene spheres is measured respectively, the mass-to-charge ratio that records has surpassed 109, and error is less than 1%.But need to utilize electron gun to change the quantity of electric charge of trapped ion in the experimentation, operate and calculate loaded down with trivial details time-consuming accordingly, also limited the application of this method.Subsequently, Peng etc. have been developed the induced with laser sound wave desorption ionization method of particulate matter again in 2005, the method only need be with the drips of solution of particulate matter on silicon chip, allow solvent volatilize, go to shine silicon chip back with laser then, the sound wave of induced with laser is resolved sample, though the efficient of this parsing/ioning method is lower, only needs when utilizing optical means to analyze quality for individual particle enough.Than substance assistant laser desorpted, the desorb of induced with laser sound wave can realize that virus, cell etc. do not have the ionization of the biologic grain of rigid shell, than electron spray, it is safer that the desorb of induced with laser sound wave makes that bacterium, virus etc. have an analysis of communicable biologic grain in the aqueous solution.Nie etc. utilize the method for induced with laser sound wave desorb-cylindrical ion trap-light scattering to realize analysis to human adenovirus, rainbow virus and vaccinia virus.In 2007, Peng etc. have been developed the quick mensuration that induced with laser sound wave parsing-charge detection mass spectrography is used for cell and microparticle quality again, can obtain the mass-to-charge ratio of particulate matter by frequency scanning, by electric charge detector can directly obtain its with the quantity of electric charge, the quality of particulate matter just can be calculated acquisition easily like this.On this basis, Nie waits the method for utilizing induced with laser sound wave desorb-quadrupole ion trap-charge detection to measure a series of animals and normal person and anaemia patient's erythrocytic quality.These researchs all focus on the ionization that particulate matter is new and the foundation and the improvement of method for quick, have realized the quick mensuration of granular mass.For the further scene of particulate matter and the needs that original position is analyzed of adapting to, develop a kind of miniaturization particle mass spectrometer that can realize that granular mass is measured fast and be very important.
Summary of the invention
At the problems referred to above, the purpose of this invention is to provide a kind of simple in structure, volume is little, and can realize measuring fast the cylindrical ion trap mass spectrometer of granular mass.
For achieving the above object, the present invention takes following technical scheme: a kind of cylinder ion trap mass spectrometer, it is characterized in that: it comprises that an ion source, a cylindrical ion trap, an electric charge detector and are used for the electro-magnetic shielding cover that the shielded radio frequency electric field disturbs described electric charge detector, described electric charge detector is arranged on described electro-magnetic shielding cover cavity inner bottom part, and the center position at described electro-magnetic shielding cover top is provided with a through hole; Described ion source is squeezed into sample in the described cylindrical ion trap through the sample inlet of described cylindrical ion trap, behind the through hole of the described electro-magnetic shielding cover by being arranged on described cylindrical ion trap below, be thrown on the described electric charge detector and detect.
Described cylindrical ion trap comprises a upper end electrode, a ring electrode and a lower end electrode, and described upper end electrode, ring electrode and lower end electrode surround the electric field of a cylindrical region; Apply the radio-frequency voltage that is used to imprison the sample ion on described ring electrode, described upper end electrode and lower end electrode adopt ground connection, connect one of them connected mode of direct current and Opposed crossing; Described upper end electrode and lower end electrode center position offer a circular hole respectively, at described upper end electrode and described ring electrode, and being respectively arranged with an insulating ceramics ring that has an opening between described ring electrode and the described lower end electrode, described opening is described sample inlet.
Described ion source adopts induced with laser sound wave maldi ion source, and it comprises a sample target and a laser.
The through hole at described electro-magnetic shielding cover top is set with an aperture plate that allows the particle ion to pass.
The trap radius r of described cylindrical ion trap
0Between 1mm～5mm, described upper end electrode is to trap centre distance z
0, and described lower end electrode to trap centre distance z
0Between 1mm～5mm; Distance between described aperture plate and the described lower end electrode is between 5mm～15mm.
The peripheral shape of described ring electrode adopts square and circular one of them shape, and described upper end electrode and lower end electrode adopt one of them shape of rectangle and circle.
The present invention is owing to take above technical scheme, it has the following advantages: 1, the present invention is owing to adopt the mass spectrometer that comprises ion source, cylindrical ion trap, electric charge detector and electro-magnetic shielding cover, cylindrical ion trap surrounds a cylindrical electric field region by ring electrode and upper end electrode, lower end electrode, the sample ions of dishing out strikes on the electric charge detector detected, and cylindrical ion trap has smaller volume and be easy to processing, therefore simplify structure of the present invention, reduced cost.2, the present invention is because employing is provided with electric charge detector in the bottom of electro-magnetic shielding cover cavity, the sample particle ion of dishing out through cylindrical ion trap is detected by electric charge detector, can obtain the mass-to-charge ratio and the charge number of particle ion simultaneously, therefore, realized quick mensuration to granular mass.3, the present invention is because the cylindrical ion trap that adopts has less size, therefore make that the required radio-frequency voltage that applies is also smaller on ring electrode, thereby reduced vacuum requirements, can under more rough vacuum condition, work, required vacuum condition only needs mechanical pump just can provide, for the mass spectral further simplification of particle provides advantageous conditions.4, the present invention is owing to adopt this soft ionization method of induced with laser sound wave desorb, therefore can further cylindrical ion trap mass spectrometer of the present invention be extended to the mensuration of multiple biologic grains such as pair cell, virus, and help the foundation of the methods such as Rapid identification of virus.The present invention can be widely used in the mensuration to various micron particles quality.
Description of drawings
Fig. 1 is an overall structure schematic diagram of the present invention;
Fig. 2 is a cylindrical ion trap structural representation of the present invention;
Fig. 3 is the profile of Fig. 2;
Fig. 4 is the mass spectrogram that the present invention is obtained when utilizing electric charge detector that ion is detected;
Fig. 5 is the mass distribution block diagram that the present invention measures 3 μ m polystyrene spheres.
Embodiment
Below in conjunction with drawings and Examples the present invention is described in detail.
Ion trap mass spectrometer has structure and relatively simply and to vacuum degree requires characteristics such as low, is to make the mass spectrometric first-selection of miniaturization.And the present invention adopts the wherein the simplest cylindrical ion trap structure of structure, hyperboloid structure with respect to traditional quadrupole ion trap, the easier processing of the cylindrical structural of cylindrical ion trap and realization miniaturization and diversification, so cylindrical ion trap is suitable for making up on-the-spot hand-held analyzer device very much.Although just as the store tools of ion, the cylindrical ion trap with appropriate structure and size also can be used as mass analyzer to cylindrical ion trap, and can obtain good resolution and sensitivity at first.Because the simple structure of cylindrical ion trap, it can also be processed to array structure or micron-sized ion trap chip is realized high-throughout mass spectral analysis.In addition, the size that cylindrical ion trap is littler makes required radio-frequency voltage also smaller, thereby has reduced instrument itself to vacuum requirements.
As Fig. 1～shown in Figure 3, the present invention includes an ion source 1, a cylindrical ion trap 2, an electric charge detector 3 and and be used for the electro-magnetic shielding cover 4 that the shielded radio frequency electric field disturbs electric charge detector 3, electric charge detector 3 is arranged on the bottom in electro-magnetic shielding cover 4 cavitys, and the center position at electro-magnetic shielding cover 4 tops is provided with a through hole 5.Ion source 1 is squeezed into sample in the cylindrical ion trap 2 through the sample inlet of cylindrical ion trap 2, and behind the through hole 5 of the electro-magnetic shielding cover 4 by being arranged on cylindrical ion trap 2 belows, is thrown on the electric charge detector 3, realizes the detection to sample.
As Fig. 2, shown in Figure 3, cylindrical ion trap 2 comprises a upper end electrode 6, a ring electrode 7 and a lower end electrode 8, and upper end electrode 6, ring electrode 7 and lower end electrode 8 surround the electric field of a cylindrical region.Wherein, apply the radio-frequency voltage that is used to imprison the sample ion on ring electrode 7, upper end electrode 6 and lower end electrode 8 can adopt ground connection, connect connected modes such as direct current or Opposed crossing.Upper end electrode 6 and lower end electrode 8 center positions in cylindrical ion trap 2 offer a circular hole 9 respectively, and the sample ion is dished out from circular hole 9 outside the cylindrical ion trap 2, and are detected by electric charge detector 3.At upper end electrode 6 and ring electrode 7, and be respectively arranged with an insulating ceramics ring 11 that has an opening 10 between ring electrode 7 and the lower end electrode 8, ring electrode 7 and upper end electrode 6, lower end electrode 8 are kept apart, avoid it to be in contact with one another and the phenomenon that is short-circuited.Wherein, opening 10 is the sample inlet of cylindrical ion trap 2.
As shown in Figure 1, ion source 1 adopts induced with laser sound wave desorb (LIAD) ion source, it comprises a sample target 12 and a laser 13, sample drips on sample target 12, beat at the back side of sample target 12 by the laser that laser 13 sends, and then the particle ion of sample is parsed.The particle ion enters in the cylindrical ion trap 2 by the opening 10 of insulating ceramics ring 11, by modes such as frequency scanning of the prior art or voltage scanning with the particle ion outside the circular hole 9 of lower end electrode 8 is dished out trap, and strike on the electric charge detector 3, and then realize detection to the particle ion by the through hole 5 at electro-magnetic shielding cover 4 tops.
Through hole 5 places at electro-magnetic shielding cover 4 tops also are set with an aperture plate 14 that allows the particle ion to pass, and aperture plate 14 also can the shielded radio frequency electric field to the interference of electric charge detector 3.
Different shapes such as in the foregoing description, that the peripheral shape of ring electrode 7 can be processed into is square, circle, upper end electrode 6 and lower end electrode 8 also can adopt rectangle or circle etc., so that assembling for convenience.
In the various embodiments described above, as shown in Figure 3, the trap radius r of cylindrical ion trap 2 of the present invention
0Between 1mm～5mm; Upper end electrode 6 to trap centre distance z
0, and lower end electrode 8 to trap centre distance z
0Also between 1mm～5mm.
In the various embodiments described above, the distance between aperture plate 14 and the lower end electrode 8 is between 5mm～15mm.
Below in conjunction with a specific embodiment effect of the present invention is described.Utilize the present invention that the quality of the standard particle 3 μ m polystyrene spheres bought from American National Standard and technological associations (NIST) has been carried out measuring fast, obtained the mass distribution block diagram of 3 μ m polystyrene spheres.
At first, the polystyrene spheres standard items suspension of buying is cleaned with deionized water, with the centrifugal removal of sodium azide in the solution.Then prepared hanging drop is added on the silicon chip of prior well cutting.Treat behind the aqueous solution evaporate to dryness silicon chip to be fixed on the sample target 12.And then open vacuum pump of the prior art, laser, function generator, radio frequency amplifier, electric charge detector power supply and data handling system successively, and utilize helium that the pressure of vacuum systems is regulated, set the parameter of pertinent instruments simultaneously.
For the mensuration of 3 μ m polystyrene spheres quality, the actual conditions of setting is: the air pressure in the cylindrical ion trap 2 is 4Pa, is applied to the radio-frequency voltage V on the ring electrode 7
Ac(0～p value) is 1000V, upper end electrode 6 and lower end electrode 8 ground connection, and the frequency scanning scope is 900Hz～300Hz, and the linear scan time is 5s, and the energy of laser 13 (532nm, pulse duration is 7ns) is the 30mJ/ pulse.
The laser that sends with laser 13 during experiment goes to bombard silicon chip back, sample is hunted down after entering cylindrical ion trap 2, and then the ion instability is dished out outside the cylindrical ion trap 2 by the frequency scanning mode, and utilize 3 pairs of ions of electric charge detector to detect, and then obtain a mass spectrogram (as shown in Figure 4), a polystyrene ball particle is all represented at each peak wherein, ordinate be each polystyrene spheres surface with charge number z, abscissa is the m/z value of each polystyrene spheres, and both products are the quality m of single polystyrene spheres.
To the mass distribution block diagram (as shown in Figure 5) that obtains after nearly the m value of 200 polystyrene spheres is added up, its average quality is 8.81 * 10
12Da, the standard deviation of mass distribution are 18%.The deviate that records be slightly larger than reported by the measured value 16% of quadrupole ion trap, this mainly is because cylindrical ion trap has littler volume, the bigger reason of corresponding enclosed pasture effect.But experimental result shows that the resolution of quadrupole ion trap and cylindrical ion trap does not have significant difference in the mensuration to micron particles, and then explanation utilizes cylindrical ion trap can realize quality determination and analysis to particulate matter well.
The various embodiments described above only are used to illustrate the present invention; the structure of voltage application mode, each parts, size, the position is set and shape all can change to some extent; on the basis of technical solution of the present invention; all improvement and equivalents of individual component being carried out according to the principle of the invention all should not got rid of outside protection scope of the present invention.
Claims (10)
1. cylinder ion trap mass spectrometer, it is characterized in that: it comprises that an ion source, a cylindrical ion trap, an electric charge detector and are used for the electro-magnetic shielding cover that the shielded radio frequency electric field disturbs described electric charge detector, described electric charge detector is arranged on described electro-magnetic shielding cover cavity inner bottom part, and the center position at described electro-magnetic shielding cover top is provided with a through hole; Described ion source is squeezed into sample in the described cylindrical ion trap through the sample inlet of described cylindrical ion trap, behind the through hole of the described electro-magnetic shielding cover by being arranged on described cylindrical ion trap below, be thrown on the described electric charge detector and detect.
2. a kind of cylinder ion trap mass spectrometer as claimed in claim 1, it is characterized in that: described cylindrical ion trap comprises a upper end electrode, a ring electrode and a lower end electrode, and described upper end electrode, ring electrode and lower end electrode surround the electric field of a cylindrical region; Apply the radio-frequency voltage that is used to imprison the sample ion on described ring electrode, described upper end electrode and lower end electrode adopt ground connection, connect one of them connected mode of direct current and Opposed crossing; Described upper end electrode and lower end electrode center position offer a circular hole respectively, at described upper end electrode and described ring electrode, and being respectively arranged with an insulating ceramics ring that has an opening between described ring electrode and the described lower end electrode, described opening is described sample inlet.
3. a kind of cylinder ion trap mass spectrometer as claimed in claim 1 is characterized in that: described ion source adopts induced with laser sound wave maldi ion source, and it comprises a sample target and a laser.
4. a kind of cylinder ion trap mass spectrometer as claimed in claim 2 is characterized in that: described ion source adopts induced with laser sound wave maldi ion source, and it comprises a sample target and a laser.
5. as claim 1 or 2 or 3 or 4 described a kind of cylinder ion trap mass spectrometers, it is characterized in that: the through hole at described electro-magnetic shielding cover top is set with an aperture plate that allows the particle ion to pass.
6. as claim 1 or 2 or 3 or 4 described a kind of cylinder ion trap mass spectrometers, it is characterized in that: the trap radius r of described cylindrical ion trap
0Between 1mm～5mm, described upper end electrode is to trap centre distance z
0, and described lower end electrode to trap centre distance z
0Between 1mm～5mm; Distance between described aperture plate and the described lower end electrode is between 5mm～15mm.
7. a kind of cylinder ion trap mass spectrometer as claimed in claim 5 is characterized in that: the trap radius r of described cylindrical ion trap
0Between 1mm～5mm, described upper end electrode is to trap centre distance z
0, and described lower end electrode to trap centre distance z
0Between 1mm～5mm; Distance between described aperture plate and the described lower end electrode is between 5mm～15mm.
8. as claim 1 or 2 or 3 or 4 or 7 described a kind of cylinder ion trap mass spectrometers, it is characterized in that: the peripheral shape of described ring electrode adopts square and circular one of them shape, and described upper end electrode and lower end electrode adopt one of them shape of rectangle and circle.
9. a kind of cylinder ion trap mass spectrometer as claimed in claim 5 is characterized in that: the peripheral shape of described ring electrode adopts square and circular one of them shape, and described upper end electrode and lower end electrode adopt one of them shape of rectangle and circle.
10. a kind of cylinder ion trap mass spectrometer as claimed in claim 6 is characterized in that: the peripheral shape of described ring electrode adopts square and circular one of them shape, and described upper end electrode and lower end electrode adopt one of them shape of rectangle and circle.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102339720A (en) * | 2011-09-26 | 2012-02-01 | 中国科学院化学研究所 | Ion source device for injecting sample under atmospheric pressure |
| CN102945785A (en) * | 2012-11-12 | 2013-02-27 | 武汉矽感科技有限公司 | Pulse type glow discharge ion source with ion trap |
| CN103745905A (en) * | 2014-01-06 | 2014-04-23 | 中国科学院化学研究所 | Particulate ion trap mass spectrometer with low-temperature charge detector |
| CN104637776A (en) * | 2015-01-21 | 2015-05-20 | 中国科学院上海微系统与信息技术研究所 | Sandwich-structured MEMS (Micro-Electro-Mechanical Systems) column-shaped ion well, manufacturing method and application |
| CN107449648A (en) * | 2017-06-30 | 2017-12-08 | 中国科学院广州地球化学研究所 | A kind of preparation method of the sample target of ore mineral suitable for ion microprobe analysis |
| CN108470672A (en) * | 2018-03-19 | 2018-08-31 | 塔里木大学 | A kind of ion implanting component and its control and data processing method |
| CN111856165A (en) * | 2020-08-21 | 2020-10-30 | 中国科学院精密测量科学与技术创新研究院 | Device and method for rapidly measuring electric field noise of metal surface |
| CN116047114A (en) * | 2023-01-05 | 2023-05-02 | 北京量子信息科学研究院 | Measuring method and measuring device for surface ion trap trapping electric field distribution |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102339720B (en) * | 2011-09-26 | 2014-04-02 | 中国科学院化学研究所 | Ion source device for injecting sample under atmospheric pressure |
| CN102339720A (en) * | 2011-09-26 | 2012-02-01 | 中国科学院化学研究所 | Ion source device for injecting sample under atmospheric pressure |
| CN102945785A (en) * | 2012-11-12 | 2013-02-27 | 武汉矽感科技有限公司 | Pulse type glow discharge ion source with ion trap |
| CN103745905B (en) * | 2014-01-06 | 2016-03-16 | 中国科学院化学研究所 | A kind of particulate ion trap mass spectrometer with low-temperature charge detector |
| CN103745905A (en) * | 2014-01-06 | 2014-04-23 | 中国科学院化学研究所 | Particulate ion trap mass spectrometer with low-temperature charge detector |
| CN104637776B (en) * | 2015-01-21 | 2017-06-20 | 中国科学院上海微系统与信息技术研究所 | A kind of sandwich structure MEMS cylindrical ion traps, preparation method and application |
| CN104637776A (en) * | 2015-01-21 | 2015-05-20 | 中国科学院上海微系统与信息技术研究所 | Sandwich-structured MEMS (Micro-Electro-Mechanical Systems) column-shaped ion well, manufacturing method and application |
| CN107449648A (en) * | 2017-06-30 | 2017-12-08 | 中国科学院广州地球化学研究所 | A kind of preparation method of the sample target of ore mineral suitable for ion microprobe analysis |
| CN107449648B (en) * | 2017-06-30 | 2019-09-27 | 中国科学院广州地球化学研究所 | A kind of preparation method of the sample target of the ore mineral suitable for ion microprobe analysis |
| CN108470672A (en) * | 2018-03-19 | 2018-08-31 | 塔里木大学 | A kind of ion implanting component and its control and data processing method |
| CN108470672B (en) * | 2018-03-19 | 2020-02-14 | 塔里木大学 | Ion implantation assembly and control and data processing method thereof |
| CN111856165A (en) * | 2020-08-21 | 2020-10-30 | 中国科学院精密测量科学与技术创新研究院 | Device and method for rapidly measuring electric field noise of metal surface |
| CN111856165B (en) * | 2020-08-21 | 2022-05-03 | 中国科学院精密测量科学与技术创新研究院 | Device and method for rapidly measuring electric field noise of metal surface |
| CN116047114A (en) * | 2023-01-05 | 2023-05-02 | 北京量子信息科学研究院 | Measuring method and measuring device for surface ion trap trapping electric field distribution |
| CN116047114B (en) * | 2023-01-05 | 2024-07-02 | 北京量子信息科学研究院 | Measuring method and measuring device for surface ion trap trapping electric field distribution |
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