CN203351552U - Organic matter detection apparatus of negative ion proton reverse transfer reaction mass spectrum - Google Patents
Organic matter detection apparatus of negative ion proton reverse transfer reaction mass spectrum Download PDFInfo
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- CN203351552U CN203351552U CN 201320345776 CN201320345776U CN203351552U CN 203351552 U CN203351552 U CN 203351552U CN 201320345776 CN201320345776 CN 201320345776 CN 201320345776 U CN201320345776 U CN 201320345776U CN 203351552 U CN203351552 U CN 203351552U
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Abstract
An organic matter detection apparatus of a negative ion proton reverse transfer reaction mass spectrum comprises a gas discharge negative ion source, a reaction tube, a negative ion mass spectrum detection system, a discharge power supply, an ion extraction power supply and an ion drift power supply. The reaction tube is located between the gas discharge negative ion source and the negative ion mass spectrum detection system. The gas discharge negative ion source is composed of a discharge cathode, a discharge anode, a discharge pad and an extraction pad. The discharge cathode is located on the top of the gas discharge negative ion source. The discharge pad is located between the discharge cathode and the discharge anode. The extraction pad is located between the discharge anode and the reaction tube. A discharge gas inlet is arranged on the discharge cathode. A discharge gas extraction opening is arranged on the extraction pad. The reaction tube is composed of a sample introduction pole, a tail pole, multiple annular electrodes and annular pads, wherein, the annular electrodes and the annular pads are arranged in an alternate way. The cathode of the discharge power supply is serially connected with a resistor and further connected with the discharge cathode. The anode of the discharge power supply is connected with the discharge anode. By extracting and guiding electric fields of negative reaction ions such as OH-, the negative ion proton reverse transfer reaction mass spectrum for organic matter detection is successfully realized.
Description
Technical field
The utility model belongs to the analyzing and testing field, is specifically related to a kind of anion proton reversion and moves the mass spectral:mass spectrographic organic substance checkout gear of reaction.
Background technology
Flowing afterglow mass spectrometer research shows: H
3o
+the positive reaction ion can with organic substance generation Proton-Transfer Reactions, provide proton to organic substance, by the organic substance ionization; OH
-anion also can be used as reactive ion, move and react with the reversion of organic substance generation proton, capture proton from organic substance to be measured, by organic substance ionization (Patrik Spanel, International Journal of Mass Spectrometry and Ion Processes, 145 (1995) 177-186).H
3o
+or OH
-ion reacts with organic substance and all has higher speed constant, in the trace detection field, has broad application prospects, especially OH
-context of detection in anion at the electronegativity material more has superiority, and is expected to be applied to public safety field.
The flowing afterglow mass spectrometer technology is, by modes such as electric discharge, radiation, reagent gas is become to plasma, but what extract ion is not electric field but high velocity carrier gas, the ion be extracted out is by the organic substance ionization in flow duct, and organic substance just can finally be detected by mass spectrum like this.Also extracted upper state neutral molecule/atom when due to high velocity carrier gas, extracting ion and entered flow duct, these upper state neutral molecule/atoms can cause unnecessary chemical reaction, thereby cause product ion complicated; The expensive carrier gas such as helium are also given to detect to study and are brought financial burden; High velocity carrier gas is to realize by the high pumping rate lobe pump of flow duct afterbody, the large volume of lobe pump and the restriction certain further developing of detection field of high noisy flow twilight sunset device.
The Proton transfer reaction mass spectrometry technology that developed recently gets up has solved the problems referred to above that in the flowing afterglow mass spectrometer technology, carrier gas brings well.It becomes steam or ammonia into plasma by modes such as electric discharge, radiation equally, but adopts Electric Field Mode to extract cation H
3o
+or NH
4 +as reactive ion, and the guiding ion has been avoided the use of carrier gas in reaction chamber migration and reaction.The Proton transfer reaction mass spectrometry technology with highly sensitive, response is fast, soft ionization, do not need the advantage such as calibration obtaining great achievement aspect the trace organic substance detection research in the fields such as environment, food.Yet electric field extracts OH
-the proton reversion of negative reaction ion moves the reaction mass spectrum and but has no the open report of successfully realizing.
The utility model content
Technology of the present utility model is dealt with problems: provide a kind of anion proton reversion to move the mass spectral:mass spectrographic organic substance checkout gear of reaction, by simple charging method, prepare OH
-, CH
3 -or NH
2 -, realize organic substance is carried out to high-effect ionic in conjunction with drift-tube technique, and realize online highly sensitive detection as reactive ion in anion.
The utility model technical solution: a kind of anion proton reversion moves the mass spectral:mass spectrographic organic substance checkout gear of reaction, comprises gas discharge anion source 1, reaction tube 2, negative ion mass spectrum detection system 3, discharge power supply 4, the ion extraction power supply 5 and ion drift power supply 6; Described reaction tube 2 is between gas discharge anion source 1 and negative ion mass spectrum detection system 3; Described gas discharge anion source 1 consists of electric discharge negative electrode 7, discharge anode 8, electric discharge pad 9 and extraction pad 10, the electric discharge negative electrode is positioned at gas discharge anion source 1 top, electric discharge pad 9, between electric discharge negative electrode 7 and discharge anode 8, extracts pad 10 between discharge anode 8 and reaction tube 2; Electric discharge negative electrode 7 is provided with discharge gas entrance 11, extracts pad 10 and is provided with discharge gas bleeding point 12; Described reaction tube 2 by the sample introduction utmost point 13, the tail utmost point 14, multi-disc annular electrode 15 is alternate with annular gasket 16 forms, the sample introduction utmost point 13 centers are provided with ion entrance 17, side is provided with treats test sample gas entrance 18, tail Ji14 center is provided with ion outlet 19; Described discharge power supply 4 negative poles connect a resistance with the electric discharge negative electrode 7 be connected, the positive pole of discharge power supply 4 is connected with discharge anode 8; Described ion drift power supply 6 negative poles are connected with the sample introduction utmost point 13 on reaction tube 2 tops and the tail utmost point 14 of afterbody respectively with anodal, between reaction tube 2 adjacent electrodes, by resistance, are connected; The negative pole of described the ion extraction power supply 5 is connected with discharge power supply 4 is anodal, and the positive pole of the ion extraction power supply 5 is connected with the negative pole of ion drift power supply 6.
Described discharge gas can be steam, methane gas or ammonia, and gas flow is 0.5ml/min～40ml/min.
Described gas discharge anion source (1) internal gas pressure is at 5Pa～200Pa.
Described reaction tube (2) internal gas pressure scope is 60Pa～500Pa, and described reaction tube (2) internal electric field scope is 10V/cm～700V/cm.
Described ion entrance (17) diameter is 0.1mm～20mm.
Described ion outlet (19) diameter is 0.1mm～5mm.
Described negative ion mass spectrum detection system (3) can be the mass spectrum detection systems such as quadrupole rod mass spectrum with anion detecting function, flight time mass spectrum, ion trap mass spectrometry.
The utility model difference and advantage compared with prior art is:
(1) that Proton transfer reaction mass spectrometry preparation electric field extract is H
3o
+in the positive reaction ion, by Proton-Transfer Reactions, by organic substance ionization to be measured, and the utility model preparation is extracted, be negative reaction ion OH
-deng, reverse and move reaction by the determinand ionization by proton.The utility model is contrary with directions of an electric field such as Proton transfer reaction mass spectrometry intermediate ion source, drift tubes, and the mass spectrum detection system is that anion is surveyed mass spectrum.Can prepare by the flow duct mass-spectrometric technique extracts OH
-in the negative reaction ion, but it adopts high velocity carrier gas to extract wherein anion, and ion reacts with determinand in flow process, and its high velocity carrier gas is to realize extracting by the lobe pump of flow duct afterbody.In the utility model, only adopt electric field simply to extract, and by the reversed electric field effect, allowing anion move and to react with determinand in drift tube, the ion source structure in the utility model, the ion extraction mode and ion migration pattern are different from the flow duct technology.In addition, the utility model is without high velocity carrier gas, so without lobe pump.
(2) innovation of the present utility model is: successfully by electric field, extract OH
-in anion, as reactive ion, avoided in the flowing afterglow technology adopting high velocity carrier gas to extract ion and the deficiency such as the reaction system that causes is complicated, carrier gas is expensive and the lobe pump volume is large, noise is large.In addition, by extracting OH
-in the negative reaction ion, in conjunction with the reversed electric field drift-tube technique, and be equipped with the negative ion mass spectrum detection system, form the reversion of anion proton and move the reaction substance spectral apparatus, the selectivity that is more suitable for partial organic substances detects.
The accompanying drawing explanation
Fig. 1 is that a kind of anion proton reversion of the present utility model moves the mass spectral:mass spectrographic organic substance checkout gear schematic diagram of reaction;
Fig. 2 is OH prepared by the utility model device
-anion detects the mass spectrogram of acetone.
Embodiment
As shown in Figure 1, a kind of anion proton reversion of the present utility model moves the mass spectral:mass spectrographic organic substance checkout gear embodiment of reaction and comprises: comprise gas discharge anion source 1, reaction tube 2, negative ion mass spectrum detection system 3, discharge power supply 4, the ion extraction power supply 5 and ion drift power supply 6; Described reaction tube 2 is between gas discharge anion source 1 and negative ion mass spectrum detection system 3; Described gas discharge anion source 1 consists of electric discharge negative electrode 7, discharge anode 8, electric discharge pad 9 and extraction pad 10, the electric discharge negative electrode is positioned at gas discharge anion source 1 top, electric discharge pad 9, between electric discharge negative electrode 7 and discharge anode 8, extracts pad 10 between discharge anode 8 and reaction tube 2; Electric discharge negative electrode 7 is provided with discharge gas entrance 11, extracts pad 10 and is provided with discharge gas bleeding point 12; Described reaction tube 2 by the sample introduction utmost point 13, the tail utmost point 14, multi-disc annular electrode 15 is alternate with annular gasket 16 forms, the sample introduction utmost point 13 centers are provided with ion entrance 17, side is provided with treats test sample gas entrance 18, tail Ji14 center is provided with ion outlet 19; Described discharge power supply 4 negative poles connect a resistance with the electric discharge negative electrode 7 be connected, the positive pole of discharge power supply 4 is connected with discharge anode 8; Described ion drift power supply 6 negative poles are connected with the sample introduction utmost point 13 on reaction tube 2 tops and the tail utmost point 14 of afterbody respectively with anodal, between reaction tube 2 adjacent electrodes, by resistance, are connected; The negative pole of described the ion extraction power supply 5 is connected with discharge power supply 4 is anodal, and the positive pole of the ion extraction power supply 5 is connected with the negative pole of ion drift power supply 6.
The utility model work is: discharge gas (steam, methane gas or ammonia), by discharge gas entrance 11, passes into the interior electric discharge of gas discharge anion source 1, can prepare the negative reaction ion A
-(as: OH
-, CH
3 -or NH
2 -), the voltage provided through the ion extraction power supply 5 is extracted into reactive ion in reaction tube 2, by treating that the organic substance M that test sample gas entrance 18 enters moves and reacts with the reversion of reactive ion generation proton: A
-+ M → [M-H]
-+ AH, proton is transferred to reactive ion from organic substance, thereby, by organic substance ionization to be measured, the organic substance anion after the loss proton is under reaction tube 2 electric field actions, drift to negative ion mass spectrum detection system 3 detected, obtain mass-to-charge ratio and the corresponding ionic strength of ion.As shown in Figure 2, be the mass spectrogram of steam electric discharge preparation negative reaction ion OH-detection acetone, ordinate is relative ionic strength, abscissa is mass-to-charge ratio.The quasi-molecular ions that mass-to-charge ratio is 17 is reactive ion OH
-, the molecular weight of acetone is 58, molecular formula is CH
3c (O) CH
3, the product ion after the loss proton is CH
3c (O) CH
2 -, the quasi-molecular ions that is 57 places in mass-to-charge ratio is the product ion peak of acetone.
Prepare effect in order to obtain different ions, discharge gas can be steam, methane gas or ammonia, and gas flow is 0.5ml/min～40ml/min, and gas discharge anion source 1 internal gas pressure is at 5Pa～200Pa.In order to obtain different reaction effects and to maintain certain vacuum condition, described reaction tube 2 internal gas pressure scopes are 60Pa～500Pa, described reaction tube 2 internal electric field scopes are 10V/cm～700V/cm, and ion entrance 17 diameters are 0.1mm～20mm, and ion outlet 19 diameters are 0.1mm～5mm.Different Mass Spectrometer Method systems has ion detection characteristics separately, so, according to actual negative ion detection needs, negative ion mass spectrum detection system 3 can be the mass spectrum detection systems such as quadrupole rod mass spectrum with anion detecting function, flight time mass spectrum, ion trap mass spectrometry.
The utility model specification does not elaborate part and belongs to techniques well known.
The above; it is only the utility model part embodiment; but protection range of the present utility model is not limited to this; in the technical scope that any those skilled in the art disclose at the utility model; the variation that can expect easily or replacement, within all should being encompassed in protection range of the present utility model.
Claims (7)
1. an anion proton reversion moves the mass spectral:mass spectrographic organic substance checkout gear of reaction, it is characterized in that: comprise gas discharge anion source (1), reaction tube (2), negative ion mass spectrum detection system (3), discharge power supply (4), the ion extraction power supply (5) and ion drift power supply (6); Described reaction tube (2) is positioned between gas discharge anion source (1) and negative ion mass spectrum detection system (3); Described gas discharge anion source (1) is by electric discharge negative electrode (7), discharge anode (8), electric discharge pad (9) and extract pad (10) formation, the electric discharge negative electrode is positioned at gas discharge anion source (1) top, electric discharge pad (9) is positioned between electric discharge negative electrode (7) and discharge anode (8), extracts pad (10) and is positioned between discharge anode (8) and reaction tube (2); Electric discharge negative electrode (7) is provided with discharge gas entrance (11), extracts pad (10) and is provided with discharge gas bleeding point (12); Described reaction tube (2) is by the sample introduction utmost point (13), the tail utmost point (14), multi-disc annular electrode (15) and annular gasket (16) alternate composition, the sample introduction utmost point (13) center is provided with ion entrance (17), side is provided with treats test sample gas entrance (18), and the center of the tail utmost point (14) is provided with ion outlet (19); Described discharge power supply (4) negative pole connect a resistance with the electric discharge negative electrode (7) be connected, the positive pole of discharge power supply (4) is connected with discharge anode (8); Described ion drift power supply (6) negative pole is connected with the sample introduction utmost point (13) on reaction tube (2) top and the tail utmost point (14) of afterbody respectively with positive pole, between reaction tube (2) adjacent electrode, by resistance, is connected; The negative pole of described the ion extraction power supply (5) is connected with discharge power supply (4) is anodal, and the positive pole of the ion extraction power supply (5) is connected with the negative pole of ion drift power supply (6).
2. according to claims 1, described a kind of anion proton reversion moves the mass spectral:mass spectrographic organic substance checkout gear of reaction, and it is characterized in that: described discharge gas is steam, methane gas or ammonia, and gas flow is 0.5ml/min～40ml/min.
3. according to claims 1, described a kind of anion proton reversion moves the mass spectral:mass spectrographic organic substance checkout gear of reaction, and it is characterized in that: described gas discharge anion source (1) internal gas pressure is at 5Pa～200Pa.
4. according to claims 1, described a kind of anion proton reversion moves the mass spectral:mass spectrographic organic substance checkout gear of reaction, it is characterized in that: described reaction tube (2) internal gas pressure scope is 60Pa～500Pa, and described reaction tube (2) internal electric field scope is 10V/cm～700V/cm.
5. according to claims 1, described a kind of anion proton reversion moves the mass spectral:mass spectrographic organic substance checkout gear of reaction, and it is characterized in that: described ion entrance (17) diameter is 0.1mm～20mm.
6. according to claims 1, described a kind of anion proton reversion moves the mass spectral:mass spectrographic organic substance checkout gear of reaction, and it is characterized in that: described ion outlet (19) diameter is 0.1mm～5mm.
7. according to claims 1, described a kind of anion proton reversion moves the mass spectral:mass spectrographic organic substance checkout gear of reaction, and it is characterized in that: described negative ion mass spectrum detection system (3) is quadrupole rod mass spectrum detection system, flight time mass spectrum detection system or the ion trap mass spectrometry detection system with anion detecting function.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201320345776 CN203351552U (en) | 2013-06-15 | 2013-06-15 | Organic matter detection apparatus of negative ion proton reverse transfer reaction mass spectrum |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201320345776 CN203351552U (en) | 2013-06-15 | 2013-06-15 | Organic matter detection apparatus of negative ion proton reverse transfer reaction mass spectrum |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103337445A (en) * | 2013-06-15 | 2013-10-02 | 中国科学院合肥物质科学研究院 | Organic matter detection device and method for anion proton counter-transference reaction mass spectrometry |
| CN104183454A (en) * | 2014-08-26 | 2014-12-03 | 昆山禾信质谱技术有限公司 | Proton transfer reaction mass spectrum ion transmission device |
| CN108447762A (en) * | 2018-05-15 | 2018-08-24 | 中国科学技术大学 | A kind of Proton transfer reaction mass spectrometry instrument and its detection method |
| CN108538700A (en) * | 2018-05-15 | 2018-09-14 | 中国科学技术大学 | A kind of Proton-Transfer Reactions ion source, mass spectrograph and its detection method |
-
2013
- 2013-06-15 CN CN 201320345776 patent/CN203351552U/en not_active Withdrawn - After Issue
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103337445A (en) * | 2013-06-15 | 2013-10-02 | 中国科学院合肥物质科学研究院 | Organic matter detection device and method for anion proton counter-transference reaction mass spectrometry |
| CN103337445B (en) * | 2013-06-15 | 2015-10-28 | 中国科学院合肥物质科学研究院 | A kind of anion proton reversion moves the mass spectrographic organic substance checkout gear of reaction and detection method |
| CN104183454A (en) * | 2014-08-26 | 2014-12-03 | 昆山禾信质谱技术有限公司 | Proton transfer reaction mass spectrum ion transmission device |
| CN104183454B (en) * | 2014-08-26 | 2017-02-15 | 昆山禾信质谱技术有限公司 | Proton transfer reaction mass spectrum ion transmission device |
| CN108447762A (en) * | 2018-05-15 | 2018-08-24 | 中国科学技术大学 | A kind of Proton transfer reaction mass spectrometry instrument and its detection method |
| CN108538700A (en) * | 2018-05-15 | 2018-09-14 | 中国科学技术大学 | A kind of Proton-Transfer Reactions ion source, mass spectrograph and its detection method |
| CN108538700B (en) * | 2018-05-15 | 2024-02-23 | 中国科学技术大学 | Proton transfer reaction ion source, mass spectrometer and detection method thereof |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| AV01 | Patent right actively abandoned |
Granted publication date: 20131218 Effective date of abandoning: 20151028 |
|
| AV01 | Patent right actively abandoned |
Granted publication date: 20131218 Effective date of abandoning: 20151028 |
|
| C25 | Abandonment of patent right or utility model to avoid double patenting |