CN102192948A - Method and device for sampling mass spectrum for in-situ nondestructive analysis - Google Patents
Method and device for sampling mass spectrum for in-situ nondestructive analysis Download PDFInfo
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- CN102192948A CN102192948A CN201010129119.0A CN201010129119A CN102192948A CN 102192948 A CN102192948 A CN 102192948A CN 201010129119 A CN201010129119 A CN 201010129119A CN 102192948 A CN102192948 A CN 102192948A
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Abstract
The invention belongs to the field of sample analysis and relates to a method and device for sampling a mass spectrum for in-situ nondestructive analysis. According to the method, an organic matter is volatilized by electric heating, the sample is not damaged, and the volatile matter is taken into the mass spectrum by using inert gas. The device is characterized in that a mass spectrum probe is made of metal; a heater and a temperature sensor arranged on the probe are respectively used as a heating device and a temperature feedback device; two holes are arranged on the probe; two pipelines are arranged and connected to a power supply and a temperature control module through wires; and the temperature of probe is set by a computer, thereby being accurate in temperature control. The device is simple and is convenient to take and install.
Description
Technical field
The invention belongs to the sample analysis field, relate to and be used for mass spectral sample injection method and sampling device thereof, relate in particular to a kind of mass spectrum sample injection method and device thereof of original position nondestructive analysis.
Background technology
Mass spectrometer is the important tool of carrying out molecular weight determination and compound structure parsing, continuous development along with science and technology, the information that mass spectrum provides for relevant research is more and more, has become the main analytical approach of popular domains such as life science, Homeland Security, food security, clinical medicine detection and space technology gradually.In the prior art, common mass spectral sample introduction mainly adopts dual mode: application of gas chromatorgraphy/mass and direct inlet probe.Application of gas chromatorgraphy/mass is to utilize gas chromatography or liquid chromatography that sample is introduced mass spectrum analysis, to complex compound compartment analysis accurately, all can measure to the very big albumen of molecular weight from the gas that molecular weight is very little, good sensitivity and stability are arranged, but for gas chromatography or liquid chromatography, all can not can't harm the analysis of original position to sample.The direct inlet probe sampling technique is the monkey that sample is placed the sample feeding rod top, import sample by the mode that heats near the vacuum environment ion gun, perhaps can by in chamber with sample desorb from the tinsel that can heat rapidly, smash by mass spectral ion gun then and analyze, be generally used for analyzing solid and liquid.Direct inlet probe in the market has two kinds, one is direct inlet probe (DIP), uses electrical heating, 1000 milliamperes of maximum currents, 1000 milliamperes/minute of flank speeds, another is directly to resolve sample feeding rod (DEP), and this sample feeding rod can be carried out three rank level Four temperature programmes, the highest 〉=450 ℃, 150 ℃/minute of the highest heating rates, which kind of sample feeding rod no matter all needs sample is put into the monkey of sample feeding rod, can not carry out the harmless analysis of original position to sample.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of mass spectrum sample injection method and device thereof of original position nondestructive analysis is provided
The present invention is used for the in situ detection volatile organism, does not need to use gas chromatography or direct inlet probe, uses electrical heating to make the organism volatilization, can control temperature accurately, does not injure sample, utilizes inert gas that volatile matter is brought in the mass spectrum.
Particularly, mass spectral sample injection method of the present invention is characterized in that, it comprises and utilizes electrical heating, uses assist gas that sample is brought in the mass spectrum.
Among the present invention, the assist gas of use is an inert gas, as nitrogen.
Among the present invention, adopt sampling pump to collect sample.
Among the present invention, adopt mass spectrum directly sample to be collected detection.
The invention provides a kind of sampling device, this sampling device is made electrical heating mass spectrum probe by metal as shown in Figure 1.
Well heater and temperature sensor are housed as heating arrangement and Temperature Feedback device on the described probe, link to each other with temperature control modules with power supply by electric wire, can set the temperature of probe by computing machine, on probe, have two holes, be added with the two-way pipeline, as shown in Figure 1, first via pipeline uses inert gas, as nitrogen usually for the pipeline of auxiliary gas, the second the tunnel is kapillary, is connected in mutually with sampling pump and inserts mass spectrum or directly insert mass spectrum.After all power supply of instrument and gas supply system are opened, can detect, the temperature that can bear according to the material that will detect and sample itself is set the temperature of probe, probe stays for some time at sample surfaces during detection, and probe heated sample surface produces volatile matter, assist gas by certain flow rate is taken in the mass spectrum, by observation and search to mass spectrogram, just can determine the composition of volatile matter, can also carry out semi-quantitative analysis to interested material.
Sampling device provided by the invention is simple, and installation is easy to carry.
Sampling device of the present invention does not need gas phase or liquid chromatography that sample is carried out pre-treatment, does not need the sample removal is put in the direct inlet probe yet, can accomplish the original position nondestructive analysis.
For the ease of understanding, below will the present invention be described in detail by concrete drawings and Examples.It needs to be noted, instantiation and accompanying drawing only are in order to illustrate, obviously those of ordinary skill in the art can illustrate according to this paper, within the scope of the invention the present invention is made various corrections and change, and these corrections and change are also included in the scope of the present utility model.
Description of drawings
Fig. 1 is the synoptic diagram of sampling device electrical heating mass spectrum probe.
Embodiment
Embodiment 1
Adopt copper billet to make probe, well heater and temperature sensor are set as heating arrangement and temperature sensor in the probe, link to each other with temperature conditioning unit with power supply by electric wire, power supply and temperature control unit are integrated on the circuit board and are installed on the mass spectrum.On copper billet probe, have two holes, the nitrogen steel cylinder is inserted respectively in two holes through the gas circuit pipeline of relief outlet and the quartz capillary that external diameter 375um, internal diameter are 250um, and with epoxide-resin glue good seal (as shown in Figure 1).The flow velocity of nitrogen is 0.5-1l/min, has both protected volatile matter to avoid being exposed in the air, can guarantee the sampling of sampling pump again, and the other end of quartz capillary is connected in the sampling pump that sample frequency is 0.5l/min, and sampling pump links to each other with mass spectrum.As utilize the remained on surface of electrical heating Mass Spectrometer Method yarn fabric, instrument power source and source of the gas are all opened, owing to be to detect textile, can not destroy yarn fabric itself, so can set the temperature of probe is 50 degree, stop a bit of time as long as will pop one's head in during detection in textile surfaces, the volatilization of will being heated of the residue of textile surfaces, carry it in the kapillary by assist gas nitrogen, enter mass spectrum analysis then, by to the observation of mass spectrum chromatogram characteristic quasi-molecular ions and in database, search and plainly just can judge the composition that textile surfaces is residual, if any further needs, can carry out semiquantitative analysis, in testing process because sample does not sustain damage, so can carry out in situ detection to some other valuables or the sample that can't sample, convenient and practical.
Claims (9)
1. the mass spectrum sample injection method of an original position nondestructive analysis is characterized in that, it comprises and utilizes electrical heating, uses assist gas that sample is brought in the mass spectrum.
2. by the described method of claim 1, it is characterized in that described assist gas is an inert gas.
3. by the described method of claim 2, it is characterized in that described assist gas is that inert gas is a nitrogen.
4. by the described method of claim 1, it is characterized in that described sample is collected by sampling pump.
5. by the described method of claim 1, it is characterized in that, adopt mass spectrum directly sample to be collected detection.
6. the mass spectrum sampling device of an original position nondestructive analysis, it is characterized in that making electrical heating mass spectrum probe by metal, well heater and temperature sensor are set as heating arrangement and temperature sensor in the probe, link to each other with temperature conditioning unit with power supply by electric wire, power supply and temperature control unit are integrated on the circuit board and are installed on the mass spectrum.
7. by the described device of claim 6, it is characterized in that described probe is provided with two holes, be added with the two-way pipeline, wherein one the tunnel is the pipeline of assist gas, and another road is a kapillary.
8. by the described device of claim 6, it is characterized in that the heating arrangement electrical heating sample of described probe, after the sample volatilization, use assist gas that sample is brought in the mass spectrum.
9. by the described device of claim 6, it is characterized in that the sample that described probe maybe can't be sampled to valuables carries out in situ detection.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010129119.0A CN102192948B (en) | 2010-03-18 | 2010-03-18 | Method and device for sampling mass spectrum for in-situ nondestructive analysis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010129119.0A CN102192948B (en) | 2010-03-18 | 2010-03-18 | Method and device for sampling mass spectrum for in-situ nondestructive analysis |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102192948A true CN102192948A (en) | 2011-09-21 |
| CN102192948B CN102192948B (en) | 2014-06-11 |
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| CN201010129119.0A Expired - Fee Related CN102192948B (en) | 2010-03-18 | 2010-03-18 | Method and device for sampling mass spectrum for in-situ nondestructive analysis |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109065436A (en) * | 2018-10-12 | 2018-12-21 | 中国科学院上海有机化学研究所 | A kind of carbon fiber ionization apparatus that heat assists and the method for realizing ionization using the device |
| CN109473336A (en) * | 2018-12-19 | 2019-03-15 | 中国科学院长春应用化学研究所 | Efficient ionization probe electrospray ionization mass spectrum ion source device and the probe suitable for the ion source device |
| CN111208190A (en) * | 2020-01-10 | 2020-05-29 | 中国科学院深圳先进技术研究院 | Sampling head, sampling system, mass spectrum imaging device and sampling method |
| CN111208191A (en) * | 2020-01-10 | 2020-05-29 | 中国科学院深圳先进技术研究院 | Sampling head, sampling system, mass spectrum imaging device and sampling method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2388602Y (en) * | 1999-08-27 | 2000-07-19 | 中国科学院兰州化学物理研究所 | Continuous sample-feeding device for mass spectrographic detection in situ |
| CN1437013A (en) * | 2002-02-04 | 2003-08-20 | 李学璧 | Sample entering method for atomic spectrometer |
-
2010
- 2010-03-18 CN CN201010129119.0A patent/CN102192948B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2388602Y (en) * | 1999-08-27 | 2000-07-19 | 中国科学院兰州化学物理研究所 | Continuous sample-feeding device for mass spectrographic detection in situ |
| CN1437013A (en) * | 2002-02-04 | 2003-08-20 | 李学璧 | Sample entering method for atomic spectrometer |
Non-Patent Citations (2)
| Title |
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| 《JEOL News》 20051231 Robert B.Cody,et al Direct Analysis in Real Time (DARTtm)Mass Spectrometry 第8-12页 1-9 第40卷, 第1期 * |
| 《分析测试学报》 20080430 郭长娟等 加热毛细管作为飞行时间质谱仪真空接口的研究 第339-343页 1-9 第27卷, 第4期 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109065436A (en) * | 2018-10-12 | 2018-12-21 | 中国科学院上海有机化学研究所 | A kind of carbon fiber ionization apparatus that heat assists and the method for realizing ionization using the device |
| CN109473336A (en) * | 2018-12-19 | 2019-03-15 | 中国科学院长春应用化学研究所 | Efficient ionization probe electrospray ionization mass spectrum ion source device and the probe suitable for the ion source device |
| CN109473336B (en) * | 2018-12-19 | 2024-03-12 | 中国科学院长春应用化学研究所 | High-efficiency ionization probe electrospray mass spectrum ion source device and probe suitable for same |
| CN111208190A (en) * | 2020-01-10 | 2020-05-29 | 中国科学院深圳先进技术研究院 | Sampling head, sampling system, mass spectrum imaging device and sampling method |
| CN111208191A (en) * | 2020-01-10 | 2020-05-29 | 中国科学院深圳先进技术研究院 | Sampling head, sampling system, mass spectrum imaging device and sampling method |
| CN111208190B (en) * | 2020-01-10 | 2021-05-18 | 中国科学院深圳先进技术研究院 | Sampling head, sampling system, mass spectrum imaging device and sampling method |
| CN111208191B (en) * | 2020-01-10 | 2021-05-18 | 中国科学院深圳先进技术研究院 | Sampling head, sampling system, mass spectrum imaging device and sampling method |
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| Publication number | Publication date |
|---|---|
| CN102192948B (en) | 2014-06-11 |
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