CN101800151A - Asymmetric field reflection type flight time mass spectrometer - Google Patents
Asymmetric field reflection type flight time mass spectrometer Download PDFInfo
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Abstract
The invention relates to an asymmetric field reflection type flight time mass spectrometer, relating to the chemical component analysis and analyzing technology. The asymmetric field reflection type flight time mass spectrometer is provided with an ion accelerating area, an ion field-free flight area and an ion reflecting area which consists of several parallel electrodes, wherein the ion reflecting area is an ion reflecting electrode system of an asymmetric ion reflecting mirror; the ion reflecting mirror consists of four groups of opposite and adjacent electrodes; the four groups of electrodes are relatively independent in the four directions, and surround into the ion reflecting area; the ion working voltage is applied to the four groups of electrodes, i.e. the working voltage applied to each group of electrodes can be independently adjusted; the electric field generated in the ion reflecting area is not a uniform field, but an electric field which can be freely adjusted according to requirements; and the ions of different energy can be focused. The invention can carry out proper compensation on the energy of the ions to realize high-resolution mass spectrometric analysis, and can properly adjust the motion direction of the ions to realize high-sensitivity mass spectrometric analysis.
Description
Technical field
Asymmetric field reflection type flight time mass spectrometer of the present invention is relevant with chemical composition analysis and analytical technology.Specifically, relate to the reflection type flight time mass spectrometer that a kind of usefulness comprises asymmetric field ion reflecting electrode and carry out the mass analyzer that mass of ion is analyzed.
Technical background
In the scientific instrument of being useful on chemical composition analysis; mass spectrometer has very high sensitivity and accuracy; this makes mass spectrometer become one of present most widely used analytical technology; be widely used in chemistry, life science, food security; environmental protection, numerous areas such as medical treatment, pharmacy industry.According to the difference of operation principle etc., the commercial mass spectrometers device of many types is arranged at present, comprise magnetic mass spectrometer, time-of-flight mass spectrometer, level Four bar mass spectrometer, ion trap mass spectrometer, Fourier synchrometer, track ion trap mass spectrometer etc.The continuous research and development of new mass spectrometer have not only greatly been promoted the development of mass-spectrometric technique, also made major contribution for other scientific domain.
In numerous mass spectrometers, time-of-flight mass spectrometer is to use at present more a kind ofly, and it has, and mass range is big, mass resolution is high, analysis speed is fast, detection sensitivity is high, structure is comparatively simple, to characteristics such as instrument processing and maintenance requirement are lower and easy to use.
According to the difference of geometry, time-of-flight mass spectrometer is divided into orthoscopic and reflective two kinds again.In reflection type flight time mass spectrometer, owing to used the ion mirror field and proofread and correct the kinetic energy difference with identical mass-to-charge ratio ion, so it has higher mass resolution ability, also is current application time-of-flight mass spectrometer the most widely.Fig. 1 has provided the structure and the schematic diagram of a traditional reflection type flight time mass spectrometer.Among Fig. 1, comprise: mass spectrometric ion source region 11, ion accelerating region voltage electrode 12, sample ions 13 constitute the ion accelerating region, sample ions 13 is accelerated to certain kinetic energy in this zone, and sample ion 13 flies until entering ion echo area 15 through ion field-free flight district 14 always.The ion echo area is made up of one group of ion mirror field electrode 16.Ion be subjected in the echo area one almost with the rightabout electric field action of ion accelerating field, and to slow down until movement velocity be zero.Then, these speed are that zero ion is further oppositely quickened by the electric field of ion echo area again, and the echo area that flies out reenters ion field-free flight district 14 and do oppositely flight, until being detected by ion monitoring device 17.Obviously, for ion beam with identical mass-to-charge ratio, its initial kinetic energy, or the bigger ion 18 of initial velocity slows down in ion echo area process, when quickening overall process again, will be littler than initial kinetic energy, or the little ion 19 of initial velocity is spent more time in the ion echo area.Certainly, kinetic energy is big, and fireballing ion is in that to leave the speed that is obtained behind the ion echo area also still bigger, and its flight time also can be shorter.Like this, kinetic energy is big, also with regard to the big ion of speed in field-free flight district 14 ion that specific rate is slow spend the short time, but in the echo area again the slow ion of specific rate spend the time of growing.For a reflection type flight time mass spectrometer that design is good, the setting of its each several part geometry, use with ion acceleration and reflected voltage, should guarantee to have the ion of fast speed, with than the ion of jogging speed in the thru-flight process, it is the same as far as possible promptly to be included in used total time of ion accelerating region, field-free flight district and ion echo area, realizes that promptly so-called ion energy focuses on.The biggest quality that can obtain reflection type flight time mass spectrometer is so the most at last differentiated.
For common reflection type flight time mass spectrometer, its employed ion mirror is made of one group of electrode 21 with rectangular configuration, as shown in Figure 2.Several parallel poles 201,202,203,204,205 and 206 of forming ion mirror among Fig. 2, when they are loaded operating voltage, to 22 generations be similar to uniform electric field in the ion echo area, this electric field can carry out energy focusing to ion 23, to realize high-resolution purpose.
Obviously, for a traditional reflection type flight time mass spectrometer, because its ion echo area reflecting electrode, or be referred to as the structure of ion mirror, as shown in Figure 2.The electric field that it produced will be similar to uniform electric field, and it can only be focused on particle energy, but can't carry out " energy compensating " to the ion of different-energy, can not proofread and correct the ion with different motion direction more.In addition, because the desired uniform field of conventional ion speculum distributes, feasible machining and assembling to ion mirror also has very high requirement.The most important thing is that the advanced key technology of relevant reflection type flight time mass spectrometer and intellectual property thereof are all grasped abroad in company's hand, our country can't use substantially in scale.Therefore, the new core reflection time-of-flight mass technology with independent intellectual property right of exploitation is of great significance and value.
Summary of the invention
The object of the invention is: a kind of asymmetric field reflection type flight time mass spectrometer is provided, it is made up of four groups of ion reflecting electrodes relatively independent on four direction, the ion operating voltage that is applied on these four groups of electrodes can independent regulation, make ion in this ion mirror, can be decelerated, quicken and change the direction of motion, with the purpose of the focusing of realization ion energy, energy adjustment and space-focusing, thereby obtain better mass resolution and mass spectrometer detection efficiency.
The object of the invention is achieved through the following technical solutions: a kind of asymmetric field reflection type flight time mass spectrometer, has the ion accelerating region, the ion echo area that ion field-free flight district and several parallel pole constitute, described ion echo area is the ion reflecting electrode system of asymmetric ion mirror, described ion mirror opposes by four groups but adjacent electrode is formed, every group of electrode combines by the parallel electrodes of minor structure more, four groups of electrodes are relatively independent on four direction, surround the ion mirror district by them, on described four groups of electrodes, apply the ion operating voltage respectively, but be the operating voltage independent regulation that applies on every group of electrode, the electric field that produces in the ion echo area no longer is a uniform field, but the electric field of regulating arbitrarily as required, with the focusing of ion beam of different-energy.
Use asymmetrical ion reflection technology and device to replace traditional ion reflecting electrode system, realize that ion can be decelerated, quickens and change the direction of motion in this ion mirror, to realize ion energy focusing, energy adjustment and space-focusing.The purpose of energy focusing is in order to improve mass spectrometric mass resolution ability, and energy adjustment is in order to regulate ion energy more subtly, to obtain higher mass resolution; The purpose of space-focusing be reduce ion in flight course because the loss that dispersion of velocities caused realizes ion high efficiency of transmission and mass spectrometric high-sensitivity detection.The novel asymmetric reflection type flight time mass spectrometer that the present invention provides no longer is a uniform field by above-mentioned four groups of electric fields that voltage produced, but can carry out electric field adjusting as required arbitrarily.Compare with existing reflection type flight time mass spectrometer, have the following advantages: the first, except ion energy function, can also carry out suitable compensation, with the purpose that realizes that high resolution mass spec is analyzed to energy of ions with conventional ion speculum.The second, except the linear reflective function of ion motion direction, can also carry out suitable adjustment, to realize the purpose of high sensitivity mass spectral analysis to the direction of motion of ion with conventional ion speculum.
On the such scheme basis, described ion mirror is made of four groups of rectangular electrodes, four groups of circular arc, four groups of ellipse arc electrodes or hyperboloid shape electrode group, and wherein, described four groups of electrodes are identical, perhaps, adjacent electrode difference but comparative electrode is identical in four groups of electrodes.
Produce and use cost for reducing, on the such scheme basis, each group electrode of described speculum is made of the rectangular electrode plate that printed substrate processes, four electrode plate surround the ion echo area, each electrode plate is processed to a plurality of more small electrodes with rectangular shape again, or is referred to as conductive strips, can load different operating voltages on each conductive strips, and independent regulation arbitrarily, the electric field that they produce in the ion echo area is regulated arbitrarily as required.Owing to adopt new ion reflecting electrode process technology, simplify the manufacturing process of reflection type flight time mass spectrometer, reduce manufacturing cost, lowering apparatus production significantly and use cost.
The invention provides a kind of method of operation of described asymmetric field reflection type flight time mass spectrometer: keep the operating voltage of the opposed two groups of electrodes of vertical direction identical, the operating voltage of two groups of opposed electrodes by regulating horizontal direction is finished focusing of ion beam in the horizontal direction; Keep the operating voltage of the opposed two groups of electrodes of horizontal direction identical,, realize focusing of ion beam in vertical direction by regulating the operating voltage of two groups of opposed electrodes of vertical direction; By the operating voltage of adjusting level and vertical direction electrode, realize that ion beam is in three-dimensional focusing.
Superiority of the present invention is: can carry out suitable compensation to energy of ions, to realize the high resolution mass spec analysis; Can carry out suitable adjustment to the direction of motion of ion, to realize the high sensitivity mass spectral analysis.
Description of drawings
Fig. 1. the structural representation of traditional reflection type flight time mass spectrometer.
Fig. 2. the structural representation of traditional reflection type flight time mass spectrometer ion mirror.
Fig. 3. the ion mirror structural representation of asymmetric field reflection type flight time mass spectrometer of the present invention.
Ion motion situation map in Fig. 4, ion ion echo area in the present invention.
Fig. 5, the present invention propose by printed substrate processing and manufacturing ion mirror structural representation.
The ion mirror electrode structure schematic diagram that constitutes by four arc-shaped electrode groups that Fig. 6, the present invention propose.
Fig. 7, ion be operation principle and process schematic diagram in the asymmetric field reflection type flight time mass spectrometer.
Number in the figure:
Among Fig. 1:
The mass spectrometric ion of 11--source region 12--ion accelerating region voltage electrode 13--sample ions
14--ion field-free flight district 15--ion echo area
One group of ion mirror field of 16--electrode 17--ion monitoring device
The little ion of ion 19--initial velocity that the 18--initial velocity is bigger
Among Fig. 2:
One group of electrode with rectangular configuration of 21--constitutes
201,202,203,204,205,206--forms the parallel pole of ion mirror
22--ion echo area 23--ion beam
Among Fig. 3:
31,32,33,34--ion mirror electrode
35--ion mirror interval
311,321,331, the ion mirror operating voltage that is applied on four groups of electrodes of 341--
Among Fig. 4:
Loaded different operating voltages on four groups of electrodes of V1, V2, V3, V4--composition ion mirror
41,42,43 for having the ion beam of different kinetic energy
Among Fig. 5:
51,52,53, the rectangular electrode plate made by printed substrate of 54-
511,512,513,514,515-conductive strips
Between 55--ion echo area
Among Fig. 6:
61,62,64, four groups of arc-shaped electrodes of 64--
65--ion echo area
Among Fig. 7:
70--ion source 71--ion beam
72--the is field-free asymmetric ion of 73--echo area, ion flight district
74,75,76,77--electrode group
741,742,743,744--forms the single electrode of electrode 74
The 78--ion detector
Embodiment
Embodiment 1
A kind of asymmetric field reflection type flight time mass spectrometer, has the ion accelerating region, the ion echo area that ion field-free flight district and several parallel pole constitute, described ion echo area is the ion reflecting electrode system of asymmetric ion mirror, described ion mirror opposes by four groups but adjacent electrode is formed, four groups of electrodes are relatively independent on four direction, surround the ion mirror district by them, on described four groups of electrodes, apply the ion operating voltage respectively, but be the operating voltage independent regulation that applies on every group of electrode, the electric field that produces in the ion echo area no longer is a uniform field, but the electric field of regulating arbitrarily as required, with the focusing of ion beam of different-energy.Shown in the ion mirror structural representation of Fig. 3 asymmetric field reflection type flight time mass spectrometer of the present invention, surrounding the ion mirror operating voltage 311,321,331,341 that is applied on 35, the four groups of electrodes in ion mirror interval by four groups of ion mirror electrodes 31,32,33,34 can regulate arbitrarily as required.
As shown in the figure, ion mirror 31,32,33,34 mainly opposes by four groups but adjacent electrode is formed, and on four direction (be assumed to X1 here, X2, and Y1, Y2) relatively independent, surround ion mirror interval 35 by them.The ion operating voltage 311,321,331,341 that is applied on described four groups of electrodes can independent regulation, therefore, the electric field that is produced in the ion mirror interval by these four groups of voltages also no longer is a uniform field, but can carry out electric field adjusting as required arbitrarily.The purpose of its adjusting is in order to make ion can be decelerated in this ion mirror, to quicken and the change direction of motion, focusing on the purpose of energy adjustment and space-focusing to realize ion energy.
Shown in ion motion situation map in Fig. 4 ion ion echo area in the present invention, different operating voltage V1, V2, V3, V4 have been loaded on four groups of electrodes of composition ion mirror, make that the electric field that is produced no longer is parallel uniform electric field in the ion echo area, this electric field can make ion beam 41,42,43 slow down on the one hand, and the ion echo area of quickening again to fly out arrives ion detector; On the other hand, because the distribution situation of electric field, as V4＞V2, after having the ion beam 43 process decelerations and deflection of big kinetic energy, because it will be subjected to more approaching the effect than highfield that formed by high voltage V4, it will be than the bigger angle of ion beam 41 deflections than highfield away from high voltage V4 formation.And the deflection angle of energy ion beam 42 placed in the middle will be between 41 and 43.Its result will cause ion beam 41,42,43 concentrated relatively, promptly be equivalent to the focusing of ion beam of different-energy.This focussing force will improve the detection efficient of ion, or has been referred to as to improve the detection sensitivity of mass spectrometer.The technology of the present invention that Here it is can also change the ion motion direction, realizes the principle of ion focusing function.
As a same reason, can realize ion beam in vertical direction by the size that changes operating voltage V1 and V3, promptly with respect to the ion deflecting situation on V1, the V3 direction.In a word, by the size of suitable adjusting operating voltage V1, V2, V3, V4, can realize that ion beam is in three-dimensional focusing situation.
With Fig. 7 structure of the present invention and operation principle are described below.The present invention is made up of the ion echo area 73 of the ion source region 70 of reflection type flight time mass spectrometer, field-free ion flight district 72 and asymmetric ion mirror, sample ions is accelerated the back 70 and forms ion beam 71 and enter by four electrode groups 74,75,76,77 through field-free ion flight district 72 and surround asymmetric ion echo area 73, with electrode group 74 is example, it is made up of four parallel single electrodes 741,742,743,744.In addition, electrode group 75,76,77 is made up of littler electrode too.When on this four electrodes group 74,75,76,77, loading identical or different direct voltage respectively, will in ion echo area 73, produce electric field, i.e. the ion mirror applied electric field.Make the ion that enters in the asymmetric ion echo area 73 slow down, deflection, processes such as acceleration, and focusing again.
Obviously, if when all loading identical direct voltage on four groups of electrodes, be equal to the ion mirror in the conventional reflective time-of-flight mass spectrometer this moment, and its effect is also identical.
Consider to load on the different electrode groups situation of different direct voltages below, equate for simplifying the discussion situation, suppose the voltage that is carried on electrode group 74 and 76, so no-voltage be poor between them that also potential-free is poor.But be carried in direct voltage on the electrode group 75 and be higher than voltage on the electrode group 77, then form an electric-force gradient between electrode group 75 and electrode group 77, all ions in asymmetric ion echo area 73 will be subjected to by the electric field force effect of electrode group 75 on electrode group 77 directions this moment.Theoretically, the time that ion moves in electric field is long more, and its suffered electric field action is big more.That is to say that it is bigger that the ion ratio that run duration is long in electric field short ion of run duration in electric field is subjected to effect of electric field.For the present invention, the first, for the identical ion of mass-to-charge ratio, the time that the ion that kinetic energy is big more moves in ion mirror is long more, and in other words, the time that the little ion of ion ratio kinetic energy that kinetic energy is big more moves in ion mirror is longer; The second, for the identical ion of mass-to-charge ratio, because the time that the big more little ion of ion ratio kinetic energy of kinetic energy moves in ion mirror is longer, so the active force that it is subjected to is also bigger.So, in asymmetric ion mirror field, the little ion of the ion ratio kinetic energy that kinetic energy is big in ion mirror also big more with respect to the deflection between electrode group 75 and 77.We know.In time-of-flight mass spectrometer, owing to the initial space distribution of ion and dispersing of initial motion direction, ion beam all can have certain spatial distribution, and this distribution meeting becomes big along with the increasing of flight time and distance.But after the asymmetric ion mirror effect that process the present invention provides, because the deflection situation of the ion that the big ion of kinetic energy and kinetic energy are little is different, if the operating voltage that loads is suitable, then can be so that through after the asymmetric ion mirror, the ion that ion that kinetic energy is big and kinetic energy are little will be in a certain point focusing.This is the desired ion focusing effect that reaches of the present invention just also.In the practical application, should regulate the size of operating voltage, feasible focusing of ion beam after asymmetric ion mirror focuses on is near ion detector, to realize improving the purpose of mass spectrometer ion detection efficient and sensitivity.In this example, ion will be focused near the ion detector 78.
Embodiment 2
Basic identical with embodiment 1 structure, it is ion mirror structure difference, as Fig. 5 the present invention propose by shown in the printed substrate processing and manufacturing ion mirror structural representation, each group electrode of forming speculum all is to be processed by a bar printing wiring board, in Fig. 5, between the ion echo area that surrounds by four blocks of rectangular electrode plates 51,52,53,54 55.For each piece in these four blocks of rectangular electrode plates 51,52,53,54 is processed to have the more small electrode of rectangular shape again, or be referred to as conductive strips.Conductive strips 511,512,513,514,515 as shown in rectangular electrode plate 51.Their effect is the same with ion mirror electrode in the conventional reflective time-of-flight mass spectrometer, is in order to be loaded different operating voltages, so that 55 produce the ion reflected field in the ion echo area.Obviously, owing to can load different operating voltages on each conductive strips of each group electrode, and independent regulation arbitrarily, the electric field that they produce in ion echo area 55 also can be regulated arbitrarily as required.In the present invention, the purpose of regulating electric field is can slow down to sample ions in order to produce in ion echo area 55, quicken and the change direction of motion, realizing the purpose of ion energy focusing, energy adjustment and space-focusing, and finally improve the mass resolution ability and the detection sensitivity of time-of-flight mass spectrometer.
When coming the processing ion mirror electrodes with printed substrate, its biggest advantage is to use material cheap, and processing and assembling are simple, therefore, can reduce manufacturing, the operation and maintenance cost of the reflection type flight time mass spectrometer of asymmetric ion mirror.
Embodiment 3
Present embodiment improves the ion mirror structure, shown in the ion mirror electrode structure schematic diagram that constitutes by four arc-shaped electrode groups that Fig. 6 the present invention proposes, surround ion echo area 65 by four groups of arc-shaped electrodes 61,62,64,64, these four groups of arc-shaped electrodes 61,62,64,64 can be equal to fully, also can be relative two groups identical, and adjacent two groups inequality.Similarly, when being carried in the voltage of each group on electrode 61,62,64,64 not simultaneously, its electric field that produces in ion echo area 65 also changes thereupon, the purpose of regulating electric field is can slow down, quicken and change the direction of motion to sample ions in order to produce in ion echo area 65, to realize the purpose of ion energy focusing, energy adjustment and space-focusing, improve the mass resolution ability and the detection sensitivity of time-of-flight mass spectrometer.
Except that rectangle and arc-shaped electrode, oval-shaped electrode, the electrode of other geometries such as hyperboloid shape electrode may be used to the foundation of the given asymmetric ion mirror of the present invention.
Claims (4)
1. asymmetric field reflection type flight time mass spectrometer, has the ion accelerating region, the ion echo area that ion field-free flight district and several parallel pole constitute, it is characterized in that: described ion echo area is the ion reflecting electrode system of asymmetric ion mirror, described ion mirror opposes by four groups but adjacent electrode is formed, four groups of electrodes are relatively independent on four direction, surround the ion mirror district by them, on described four groups of electrodes, apply the ion operating voltage respectively, but be the operating voltage independent regulation that applies on every group of electrode, the electric field that produces in the ion echo area no longer is a uniform field, but the electric field of regulating arbitrarily as required, with the focusing of ion beam of different-energy.
2. according to the described asymmetric field reflection type flight time mass spectrometer of claim 1, it is characterized in that: described ion mirror is made of four groups of rectangular electrodes, four groups of circular arc, four groups of ellipse arc electrodes or hyperboloid shape electrode group, wherein, described four groups of electrodes are identical, perhaps, adjacent electrode difference but comparative electrode is identical in four groups of electrodes.
3. according to claim 1 or 2 described asymmetric field reflection type flight time mass spectrometers, it is characterized in that: each group electrode of described speculum is made of the rectangular electrode plate that printed substrate processes, four electrode plate surround the ion echo area, each electrode plate is processed to a plurality of more small electrodes with rectangular shape again, or be referred to as conductive strips, can load different operating voltages on each conductive strips, and independent regulation arbitrarily, the electric field that they produce in the ion echo area is regulated arbitrarily as required.
4. method of operation at the described asymmetric field reflection type flight time mass spectrometer of one of claim 1 to 3, it is characterized in that: keep the operating voltage of the opposed two groups of electrodes of vertical direction identical, the operating voltage of two groups of opposed electrodes by regulating horizontal direction is finished focusing of ion beam in the horizontal direction; Keep the operating voltage of the opposed two groups of electrodes of horizontal direction identical,, realize focusing of ion beam in vertical direction by regulating the operating voltage of two groups of opposed electrodes of vertical direction; By the operating voltage of adjusting level and vertical direction electrode, realize that ion beam is in three-dimensional focusing.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103201821A (en) * | 2010-09-08 | 2013-07-10 | 株式会社岛津制作所 | Time-of-flight mass spectrometer |
| CN112420481A (en) * | 2020-11-26 | 2021-02-26 | 中国科学技术大学 | Mass spectrometer and ion lens device thereof |
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| CN112420481B (en) * | 2020-11-26 | 2022-04-19 | 中国科学技术大学 | Mass spectrometer and ion lens device thereof |
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Application publication date: 20100811 |