CN110690100A - Inductively coupled plasma mass spectrometry interface device - Google Patents
Inductively coupled plasma mass spectrometry interface device Download PDFInfo
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- CN110690100A CN110690100A CN201911049521.5A CN201911049521A CN110690100A CN 110690100 A CN110690100 A CN 110690100A CN 201911049521 A CN201911049521 A CN 201911049521A CN 110690100 A CN110690100 A CN 110690100A
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- hole
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- diameter
- inclined plane
- inductively coupled
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- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 title claims abstract description 17
- 238000005070 sampling Methods 0.000 claims abstract description 20
- 150000001450 anions Chemical class 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims description 3
- 238000001819 mass spectrum Methods 0.000 claims description 2
- 230000001939 inductive effect Effects 0.000 claims 1
- 150000002500 ions Chemical class 0.000 abstract description 14
- 238000013461 design Methods 0.000 abstract description 7
- 238000010884 ion-beam technique Methods 0.000 abstract description 5
- 238000000605 extraction Methods 0.000 abstract description 4
- 230000035945 sensitivity Effects 0.000 abstract description 4
- 238000009825 accumulation Methods 0.000 abstract description 3
- 239000011159 matrix material Substances 0.000 abstract description 3
- 230000002401 inhibitory effect Effects 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N argon Substances [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- -1 argon ion Chemical class 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
- H01J49/0409—Sample holders or containers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/06—Electron- or ion-optical arrangements
- H01J49/062—Ion guides
- H01J49/065—Ion guides having stacked electrodes, e.g. ring stack, plate stack
- H01J49/066—Ion funnels
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/06—Electron- or ion-optical arrangements
- H01J49/067—Ion lenses, apertures, skimmers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/26—Mass spectrometers or separator tubes
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Electron Tubes For Measurement (AREA)
Abstract
The invention discloses an inductively coupled plasma mass spectrometry interface device which comprises a sampling cone, an intercepting cone, an anion lens and a shell, wherein the sampling cone, the intercepting cone and the anion lens are sequentially arranged in the shell, a first through hole is formed in the center of the sampling cone, a second through hole, a third through hole and a fourth through hole are sequentially arranged in the intercepting cone, the length of the second through hole is smaller than that of the third through hole and that of the fourth through hole, and a diameter changing device is arranged in the third through hole and used for changing the inner diameter of the third through hole. The invention has the advantages that: 1, the design of the intercepting cone accelerates the extraction speed of ions, can reduce the accumulation of high-matrix and high-salt samples at the mouth of the intercepting cone, and improves the phenomenon of signal drift; 2, the interception cone reduces the voltage for the second time and the first inclined plane and the second inclined plane, thereby inhibiting the divergence of the ion beam behind the interception cone and greatly improving the sensitivity of the instrument.
Description
Technical Field
The invention relates to the field of laboratory analytical instruments, in particular to an interface device of an inductively coupled plasma mass spectrometer.
Background
ICP-MS is now a conventional analysis method for trace and ultra-trace elements in aqueous solution in an analysis and test laboratory, and is widely applied to the fields of environment, semiconductors, medical treatment, food and the like. In the development of ICP-MS, the extraction interface has been one of the focuses of researchers, and its transmission characteristics directly affect the analytical performance of the ICP-MS instrument. Foreign instrument manufacturers have different designs for interfaces and advantages. Such as a sampling cone with a copper base plate, which is mainly related to heat dissipation; for example, the truncated cone opening of the embedded sheet with the side hole influences the transmission path of aerosol and improves the salt accumulation characteristic of the cone opening; for example, the design of different thicknesses is adopted for the central channel of the embedded sheet, so that the convergence of ions is directly influenced, the transmission of the ions is improved, and the sensitivity of an instrument is improved; according to the designed three-cone interface, one intercepting cone is added to be called as a super intercepting cone, ion interception is carried out through two steps of pressure reduction and two steps of acute angles, the third cone angle is smaller, the divergence of ion beams behind the cone is effectively reduced, and the pollution of a mass spectrum system behind the cone is reduced; for example, a sampling cone and an intercepting cone mouth which adopt a slit are specially designed cone mouths, and the slit is used for inputting collision/reaction gas.
And domestic manufacturers rarely have own design to the taper, mainly adopt former import interface arrangement, consequently two problems appear: (1) the running cost of the ICP-MS instrument is greatly improved, and the social service of the domestic instrument is hindered; (2) the design key parameters of the cone are aperture and shape, which are related to the design of the ion lens and the configuration of the vacuum system. The original imported interface has the problem of mismatching with the domestic instrument, so that the sensitivity of the instrument is greatly reduced, and the development of the domestic instrument to the application market is limited.
Disclosure of Invention
The invention aims to provide an inductively coupled plasma mass spectrometry interface device.
In order to solve the technical problems, the invention is realized by the following technical scheme: the utility model provides an inductively coupled plasma mass spectrometry interface device, includes sampling awl, intercepting awl, anion lens and casing, be equipped with sampling awl, intercepting awl and anion lens in the casing in proper order, sampling awl center is equipped with first through-hole, be equipped with second through-hole, third through-hole and fourth through-hole in the intercepting awl in proper order, the length of second through-hole is less than the third through-hole with the length of fourth through-hole, be equipped with the internal diameter that reducing device is used for changing the third through-hole in the third through-hole.
Preferably, the first through hole is a cylindrical through hole with the aperture of 1.0mm to 1.1 mm.
Preferably, the second through hole is a tapered hole, and the distance between the second through hole and the air inlet end of the first through hole isWhere δ is the mean free path of the collected particles, D0To sample the aperture of the cone, P0At atmospheric pressure, P1For low pressure after passing through the sampling cone, the aperture of one end of the conical hole is 0.45mm to 0.75mm, and the aperture of the other end is 2.50mm to 3.50 mm.
Preferably, the aperture of the second through hole is the same as the maximum aperture of the first through hole, and the aperture of the third through hole is larger than the aperture of the second through hole.
Preferably, the diameter changing device is of a circular ring structure, a diameter changing through hole is formed in the diameter changing device, and a first inclined plane and a second inclined plane are respectively arranged at two ends of the diameter changing through hole.
Preferably, the diameter changing device is arranged in the third through hole, and the distance between the diameter changing device and the air inlet end of the second through hole is d1*tan(a)*k1，d1Is the minimum value of the aperture of the second through hole, a is half of the taper of the second through hole, k1Are coefficients.
Preferably, the included angle between the first inclined plane and the inner surface of the diameter changing device is 30-60 degrees, the included angle between the second inclined plane and the inner surface of the diameter changing device is 30-60 degrees, the lengths of the first inclined plane and the second inclined plane are 0.15m to 0.5m, and the length and the height of the first inclined plane and the second inclined plane are d1*tan(a)*k2，k2Are coefficients.
Preferably, the length of the third through hole is equal to the length of the fourth through hole.
Compared with the prior art, the invention has the advantages that:
1, the design of the intercepting cone accelerates the extraction speed of ions, can reduce the accumulation of high-matrix and high-salt samples at the mouth of the intercepting cone, and improves the phenomenon of signal drift;
2, the secondary voltage reduction of the interception cone is related to the second inclined plane of the first inclined plane, so that the divergence of the ion beam after the interception cone is inhibited, and the sensitivity of the instrument is greatly improved;
and 3, the extraction speed of the interception cone is accelerated, the deposition of plasma airflow at the cone opening is reduced, and the phenomenon of signal drift caused by high matrix and high salt samples is improved.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic view of a reducing device according to the present invention;
FIG. 3 is a closed boundary region of the MATLAB simulation of the present invention;
FIG. 4 is a charge density distribution after a second via of the present invention;
FIG. 5 is a spatial charge field distribution in the yz plane of the present invention;
fig. 6 is a space charge field distribution everywhere on the xy section of the present invention.
1-sampling cone, 11-first through hole, 2-intercepting cone, 21-first through hole, 22-second through hole, 23-third through hole, 3-negative ion lens, 4-diameter changing device, 41-first inclined plane, 42-diameter changing through hole and 43-second inclined plane.
Detailed Description
Embodiments of the invention are further described below with reference to the accompanying drawings:
as shown in fig. 1 and 2: the utility model provides an inductively coupled plasma mass spectrometry interface arrangement, includes sampling awl, intercepting awl, anion lens and casing, is equipped with sampling awl, intercepting awl and anion lens in proper order in the casing.
The center of the sampling cone is provided with a first through hole which is a cylindrical through hole and is a Debye length formula:
in the formula of0Dielectric constant in vacuum, TeIs the electron temperature, kBIs Boltzmann constant, neIs the electron density. When the DE length is much smaller than the space size, the plasma is quasi-neutral. It can be seen that the Debye length of the plasma gas flow at the sampling cone is about 10-5mm, in order to ensure quasi-neutrality, it is required to ensure that the debye length is far smaller than the aperture of the sampling cone, and the aperture of the first through hole is 1.0mm to 1.1mm in general.
And a second through hole, a third through hole and a fourth through hole are sequentially arranged in the intercepting cone, the length of the second through hole is smaller than that of the third through hole and that of the fourth through hole, and a diameter changing device is arranged in the third through hole and used for changing the inner diameter of the third through hole. Since the position of the mach disk affects the optimum position of the test result, the optimum ion response can be obtained when the second through hole is located from the first through hole to two thirds of the mach disk. The second through hole position Xs can be calculated by the following formula:
where δ is the mean free path of the collected particles, D0To sample the aperture of the cone, P0At atmospheric pressure, P1Low pressure after passing through the sampling cone. The position of the skimmer cone is calculated to be in the range of about 10mm to 11 mm. The second through hole is a tapered hole, the aperture of one end of the tapered hole is 0.45mm to 0.75mm, and the aperture of the other end of the tapered hole is 2.5mm to 3.5 mm.
After the plasma gas flow passes through the interception cone, the Debye length is increased along with the reduction of the electron density, the quasi-neutral state is destroyed, and the space charge effect is obvious. The space charge effect was simulated using a closed boundary region of a MATLAB construction as shown in fig. 3. This model assumes that the ion beam is not lost, moving in the trapezoidal region in fig. 3. Since the ion content of the sample is much smaller than that of the argon ion, and only the argon ion flow is considered here, the relationship between the charge density ρ and the distance z behind the skimmer cone can be calculated from the charge continuity and the ion movement velocity as shown in fig. 4. MeterThe calculation shows that the electric field equipotential line distribution formed by the space charge is shown in FIG. 5: the space charge field distribution on the cross section was obtained from (z-250), and the result is shown in fig. 6. The region with serious space charge effect is mainly concentrated in the region where the ion beam is just formed, the electric field intensity formed by the space charge is outward along the radial direction, the sample ions with small mass are more easily pushed to the outer side, the sample ions with large mass are not easily repelled, and the result can cause the serious loss of the heavier ions of the light ions, namely the light discrimination phenomenon. In summary, the distance between the third through hole and the air inlet end of the second through hole is d1*tan(a)*k2，d1Is the hole length of the second through hole, a is half of the taper of the second through hole, k2Are coefficients. K is obtained through tests2In the range of 14 to 20, the device is excellent.
A diameter changing device is arranged in the third through hole, the diameter changing device is of a circular ring-shaped structure, a diameter changing through hole is formed in the diameter changing device, and a first inclined plane and a second inclined plane are arranged at two ends of the diameter changing through hole respectively. The distance between the reducing device and the air inlet end of the second through hole is d1*tan(a)*k1，d1Is the hole length of the second through hole, a is half of the taper of the second through hole, k1Is a distance coefficient. K is obtained through tests2Taking the range of 25 to 40, the device works well. The diameter-variable through hole is 10 to 18 times of the second through hole. The included angle between the first inclined plane and the inner surface of the diameter changing device is 30-60 degrees, the included angle between the second inclined plane and the inner surface of the diameter changing device is 30-60 degrees, the lengths of the first inclined plane and the second inclined plane are 0.15m to 0.5m, and the length sum height of the first inclined plane and the second inclined plane is d1*tan(a)*k3，k3Are coefficients. Through experiments, k3The device effect is good when the range of 0.45 to 1.85 is taken.
The above description is only an embodiment of the present invention, but the technical features of the present invention are not limited thereto, and any changes or modifications within the technical field of the present invention by those skilled in the art are covered by the claims of the present invention.
Claims (8)
1. The utility model provides an inductively coupled plasma mass spectrometry interface arrangement, includes sampling awl, intercepting awl, anion lens and casing, its characterized in that, be equipped with sampling awl, intercepting awl and anion lens in the casing in proper order, sampling awl center is equipped with first through-hole, be equipped with second through-hole, third through-hole and fourth through-hole in the intercepting awl in proper order, the length of second through-hole is less than the third through-hole with the length of fourth through-hole, the internal diameter that reducing device is used for changing the third through-hole is equipped with in the third through-hole.
2. The inductively coupled plasma mass spectrometry interface device of claim 1, wherein the first through-hole is a cylindrical through-hole with a diameter of 1.0mm to 1.1 mm.
3. The inductively coupled plasma mass spectrometry interface device of claim 1, wherein the second through hole is a tapered hole, and the second through hole is spaced from the inlet end of the first through hole by a distance of
Where δ is the mean free path of the collected particles, D0To sample the aperture of the cone, P0At atmospheric pressure, P1For low pressure after passing through the sampling cone, the aperture of one end of the conical hole is 0.45mm to 0.75mm, and the aperture of the other end is 2.50mm to 3.50 mm.
4. The inductively coupled plasma mass spectrometry interface device of claim 1, wherein the third through hole has a diameter equal to the maximum diameter of the second through hole, and the fourth through hole has a diameter larger than the third through hole.
5. The inductively coupled plasma mass spectrometry interface device of claim 1, wherein the diameter-varying device is a circular ring structure, and has a diameter-varying through hole inside, and the diameter-varying through hole has a first inclined surface and a second inclined surface at two ends thereof.
6. An inductive coupler as claimed in claim 5The plasma-combining mass spectrum interface device is characterized in that the diameter-changing device is arranged in the third through hole, and the distance between the diameter-changing device and the air inlet end of the second through hole is d1*tan(a)*k1，d1Is the minimum value of the aperture of the second through hole, a is half of the taper of the second through hole, k1Are coefficients.
7. The inductively coupled plasma mass spectrometry interface device of claim 5, wherein the first inclined plane has an angle of 30-60 degrees with the inner surface of the reducing device, the second inclined plane has an angle of 30-60 degrees with the inner surface of the reducing device, the first inclined plane and the second inclined plane have a length of 0.15m to 0.5m, and the first inclined plane and the second inclined plane have a length and a height d1*tan(a)*k3，k3Are coefficients.
8. The inductively coupled plasma mass spectrometry interface device of claim 1, wherein the length of the third via is equal to the length of the fourth via.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911049521.5A CN110690100A (en) | 2019-10-31 | 2019-10-31 | Inductively coupled plasma mass spectrometry interface device |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911049521.5A CN110690100A (en) | 2019-10-31 | 2019-10-31 | Inductively coupled plasma mass spectrometry interface device |
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| CN110690100A true CN110690100A (en) | 2020-01-14 |
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| CN201911049521.5A Pending CN110690100A (en) | 2019-10-31 | 2019-10-31 | Inductively coupled plasma mass spectrometry interface device |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2510862Y (en) * | 2001-12-27 | 2002-09-11 | 北京有色金属研究总院 | Inductive-coupling plasma spectrum interface unit |
| US20090039251A1 (en) * | 2007-08-09 | 2009-02-12 | Agilent Technologies, Inc. | Mass spectrometer |
| CN102439683A (en) * | 2009-04-03 | 2012-05-02 | 瓦里安半导体设备公司 | Ion source |
| CN107068534A (en) * | 2011-12-12 | 2017-08-18 | 塞莫费雪科学（不来梅）有限公司 | Mass spectrometer vacuum interface method and equipment |
| CN210607180U (en) * | 2019-10-31 | 2020-05-22 | 杭州谱育科技发展有限公司 | Inductively coupled plasma mass spectrometry interface device |
-
2019
- 2019-10-31 CN CN201911049521.5A patent/CN110690100A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2510862Y (en) * | 2001-12-27 | 2002-09-11 | 北京有色金属研究总院 | Inductive-coupling plasma spectrum interface unit |
| US20090039251A1 (en) * | 2007-08-09 | 2009-02-12 | Agilent Technologies, Inc. | Mass spectrometer |
| CN102439683A (en) * | 2009-04-03 | 2012-05-02 | 瓦里安半导体设备公司 | Ion source |
| CN107068534A (en) * | 2011-12-12 | 2017-08-18 | 塞莫费雪科学（不来梅）有限公司 | Mass spectrometer vacuum interface method and equipment |
| CN210607180U (en) * | 2019-10-31 | 2020-05-22 | 杭州谱育科技发展有限公司 | Inductively coupled plasma mass spectrometry interface device |
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