CN103115956A - Low-pressure high-temperature pyrolysis furnace applicable to mass spectrographic analysis and application thereof - Google Patents
Low-pressure high-temperature pyrolysis furnace applicable to mass spectrographic analysis and application thereof Download PDFInfo
- Publication number
- CN103115956A CN103115956A CN2013100217447A CN201310021744A CN103115956A CN 103115956 A CN103115956 A CN 103115956A CN 2013100217447 A CN2013100217447 A CN 2013100217447A CN 201310021744 A CN201310021744 A CN 201310021744A CN 103115956 A CN103115956 A CN 103115956A
- Authority
- CN
- China
- Prior art keywords
- pyrolysis
- sample
- low
- temperature
- pyrolysis oven
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention relates to a low-pressure high-temperature pyrolysis furnace applicable to mass spectrographic analysis and an application thereof. The pyrolysis furnace consists of a furnace body, a bracket, a pyrolysis chamber, a sample introduction pipe and a differential hole. According to the low-pressure high-temperature pyrolysis furnace applicable to the mass spectrographic analysis and the application of the low-pressure high-temperature pyrolysis furnace, the pyrolysis chamber is directly connected with a mass spectrum electrolysis chamber so as to control the temperature of the pyrolysis furnace, and then, a sample is enabled to be subjected to pyrolysis at different temperatures; and an ionization chamber is in a vacuum state, and the interior of the pyrolysis furnace is in a low-pressure state, so that pyrolysis products can diffuse to the electrolysis chamber under the action of pressure, the pyrolysis products of the sample are enabled to enter the electrolysis chamber at first time so as to be ionized, and the problem that free radicals and unstable intermediates are difficultly subjected to in-situ detection during low-pressure pyrolysis reaction is solved.
Description
Technical field
The present invention relates to a kind of pyrolysis oven, be specifically related to a kind of low-voltage high-temperature pyrolysis oven and application thereof of suitable mass spectrophotometry.
Background technology
The pyrolysis of coal is an important process technology in the coal utilization process, to the research of pyrolysis of coal process and product help the to promote mutual understanding structure and composition of coal, can help to analyze the pyrolysis behavior to the impact of whole gasification, therefore, the pyrolytic process of fully realizing coal can further be illustrated the molecular structure of coal.
Mass-spectrometric technique is a kind of analytical approach of measuring the ion specific charge, and its principle is to make that in sample, each component ionizes in ion gun, generates the positively charged ion of different specific charges, through the effect of accelerating field, forms ion beam, enters mass analyzer.In mass analyzer, the recycling Electric and magnetic fields makes opposite velocity dispersion occurs, and they are focused on respectively and obtains mass spectrogram, thereby determine its quality.Mass-spectrometric technique commonly used has level Four bar mass spectrum, ion trap mass spectrometry, flight time mass spectrum etc. at present.Wherein level Four bar mass spectrum is the ion that utilizes different quality, and the difference of movement locus is analyzed by measured ion in radio-frequency field; Ion trap mass spectrometry is to distinguish the quality of ion by different ions restraint conditions difference in ion trap; Flight time mass spectrum is by after giving identical energy, and fast these characteristics of the ion flight that ion flight speed is slow, quality is little that quality is large are measured the quality of ion.
Mostly present research for pyrolysis product is to adopt first collects pyrolysis product, recycle mass spectrophotometry after ion gun ionization, this method that detects afterwards of first collecting may be because of the reaction between component before detecting, and can't obtain the real information of pyrolysis product Changing Pattern in pyrolytic process.The research that also has directly is connected pyrolysis oven with mass spectrum by conduit, but the free radical that produces in pyrolytic process or reaction intermediate are extremely unstable, has reduced the real-time of analyzing.The ion of some specific moleculars is also unsettled simultaneously, and cancellation also easily occurs in the ion transfer process, the integrality that impact detects.
Summary of the invention
The defective that exists in order to overcome prior art the purpose of this invention is to provide a kind of low-voltage high-temperature pyrolysis oven and application thereof of suitable mass spectrophotometry, the free radical and the intermediate that produce in pyrolytic process for detection of sample.Its design philosophy is pyrolysis oven to be directly fixed on the front end of mass spectrum ionization chamber, by controlling the pyrolysis oven temperature, make sample pyrolysis under different temperatures, because ionization chamber is in vacuum state, and be low pressure in pyrolysis oven, therefore pyrolysis product can make the pyrolysis of coal product very first time enter tank room and be ionized because pressure-acting spreads to tank room, reduces losses of ions.
The invention provides a kind of low-voltage high-temperature pyrolysis oven of suitable mass spectrophotometry, this pyrolysis oven comprises body of heater, support, pyrolysis chamber, sample feeding pipe and difference hole; Described pyrolysis oven directly is connected with the mass spectrum tank room by the pyrolysis chamber; When sample during pyrolysis, makes sample under different temperatures, pyrolysis occur by the temperature in regulating stove in pyrolysis oven, pyrolysis product due to pressure-acting to the diffusion of mass spectrum tank room, when entering the mass spectrum tank room through forming molecular beam behind the difference hole.
The low-voltage high-temperature pyrolysis oven of suitable mass spectrophotometry provided by the invention, described sample feeding pipe are the beautiful pipes of 99 shaped steel, and external diameter is 4mm, and internal diameter is 2mm.The aperture in described difference hole is 0.5mm, and material is copper.
The low-voltage high-temperature pyrolysis oven of suitable mass spectrophotometry provided by the invention, temperature and the pressure of described pyrolysis oven are controlled by the pyrolysis chamber; It is 1200 ℃ that the pyrolysis chamber controls temperature; It is 1 ~ 300Pa that the pyrolysis chamber controls pressure by molecular pump.
The present invention also provides the application of the low-voltage high-temperature pyrolysis oven of described suitable mass spectrophotometry, and this pyrolysis oven is applied to the pyrolysis of solid, liquid, gas three-phase sample; Wherein, gaseous sample adopts the mass flowmeter sample introduction, and solid sample adopts direct application of sample, and fluid sample adopts the bubbling input mode.
The invention has the beneficial effects as follows: the present invention utilizes pyrolysis oven directly to be connected with the mass spectrum ionization chamber, makes the pyrolysis product very first time enter tank room ionization, reduces the free radical of sample pyrolysis generation and the loss of intermediate product.
Description of drawings
Fig. 1 is the structural representation of the low-voltage high-temperature pyrolysis oven of a kind of suitable mass spectrophotometry of the present invention; Wherein (1) is body of heater, and (2) are support, and (3) are the pyrolysis chamber, and (4) are sample feeding pipe, and (5) are the difference hole;
Fig. 2 is take flight time mass spectrum as example, low-voltage high-temperature pyrolysis oven and flight time mass spectrum connection diagram; Wherein (6) are the low-voltage high-temperature pyrolysis oven, and (7) are flight time mass spectrum;
Fig. 3 is the pyrolysis mass spectrogram with the temperature rising of coal model compound methyl phenyl ethers anisole.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in further details.
As shown in Figure 1, the low-voltage high-temperature pyrolysis oven of a kind of suitable mass spectrophotometry of the present invention comprises body of heater, support, pyrolysis chamber, sample feeding pipe and difference hole.When sample during pyrolysis, makes sample under different temperatures, pyrolysis occur by the temperature in regulating stove in pyrolysis oven, pyrolysis product is because pressure-acting spreads to tank room, when entering the flight time mass spectrum tank room through forming molecular beam behind the difference hole.
Fig. 3 is the pyrolysis mass spectrogram with the temperature rising of coal model compound methyl phenyl ethers anisole.673K, 973K, 1073K, 1173K and five representative temperature spots of 1373K have been chosen respectively.Can find out clearly the variation tendency of parent ion and fragmention from spectrogram, thereby analyze pyrolytic process.
The present invention can be applied to the analysis of sample pyrolysis product free radical and intermediate, utilizes pyrolysis oven directly to be connected with the mass spectrum ionization chamber, makes the pyrolysis product very first time enter tank room ionization, reduces the free radical of sample pyrolysis generation and the loss of intermediate product.
Claims (7)
1. the low-voltage high-temperature pyrolysis oven of a suitable mass spectrophotometry is characterized in that: this pyrolysis oven comprises body of heater, support, pyrolysis chamber, sample feeding pipe and difference hole;
The pyrolysis chamber is fixed on body of heater by support at the body of heater center, and pyrolysis chamber's front end is connected with sample feeding pipe, be used for to add response sample, and there is a protruding difference hole to the pyrolysis chamber body of heater rear end, and sample feeding pipe, pyrolysis chamber and the maintenance of center, difference hole are in the same horizontal line.
Described pyrolysis oven directly is connected with the mass spectrum tank room by the pyrolysis chamber;
When sample during pyrolysis, makes sample under different temperatures, pyrolysis occur by the temperature in regulating stove in pyrolysis oven, pyrolysis product due to pressure-acting to the diffusion of mass spectrum tank room, when entering the mass spectrum tank room through forming molecular beam behind the difference hole.
2. according to the low-voltage high-temperature pyrolysis oven of the described suitable mass spectrophotometry of claim 1, it is characterized in that: described sample feeding pipe is the beautiful pipes of 99 shaped steel, and external diameter is 4mm, and internal diameter is 2mm.
3. according to the low-voltage high-temperature pyrolysis oven of the described suitable mass spectrophotometry of claim 1, it is characterized in that: the aperture in described difference hole is 0.5mm, and material is copper.
4. according to the low-voltage high-temperature pyrolysis oven of the described suitable mass spectrophotometry of claim 1, it is characterized in that: temperature and the pressure of described pyrolysis oven are controlled by the pyrolysis chamber.
5. according to the low-voltage high-temperature pyrolysis oven of the described suitable mass spectrophotometry of claim 4, it is characterized in that: it is 1200 ℃ that described pyrolysis chamber controls temperature.
6. according to the low-voltage high-temperature pyrolysis oven of the described suitable mass spectrophotometry of claim 4, it is characterized in that: it is 1 ~ 300Pa that described pyrolysis chamber controls pressure by molecular pump.
7. the application of the low-voltage high-temperature pyrolysis oven of the described suitable mass spectrophotometry of claim 1 is characterized in that: this pyrolysis oven is applied to the pyrolysis of solid, liquid, gas three-phase sample; Wherein, gaseous sample adopts the mass flowmeter sample introduction, and solid sample adopts direct application of sample, and fluid sample adopts the bubbling input mode.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013100217447A CN103115956A (en) | 2013-01-22 | 2013-01-22 | Low-pressure high-temperature pyrolysis furnace applicable to mass spectrographic analysis and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013100217447A CN103115956A (en) | 2013-01-22 | 2013-01-22 | Low-pressure high-temperature pyrolysis furnace applicable to mass spectrographic analysis and application thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103115956A true CN103115956A (en) | 2013-05-22 |
Family
ID=48414382
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2013100217447A Pending CN103115956A (en) | 2013-01-22 | 2013-01-22 | Low-pressure high-temperature pyrolysis furnace applicable to mass spectrographic analysis and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103115956A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104122322A (en) * | 2014-07-15 | 2014-10-29 | 江西中烟工业有限责任公司 | Method and device for detecting whole process of compound cracking |
| CN105784917A (en) * | 2014-12-26 | 2016-07-20 | 中国科学院大连化学物理研究所 | Application of mass spectrometer to detection process of ionized intermediates in catalytic reaction |
| CN107576717A (en) * | 2017-10-24 | 2018-01-12 | 中国科学技术大学 | A kind of in-situ detector for different diffusion length catalytic reaction gas phase intermediate products |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4626412A (en) * | 1984-12-14 | 1986-12-02 | Monsanto Company | Method and apparatus for carrying out catalyzed chemical reactions and for studying catalysts |
| EP1724574A1 (en) * | 2004-02-27 | 2006-11-22 | Japan Science and Technology Agency | Analytical method and analyzer capable of substantially simultaneously analyzing absorption/emission/scattering spectrum and mass spectrum, and analytical method and mass spectroscope utilizing electrospray ionization technique |
| CN101634651A (en) * | 2008-07-25 | 2010-01-27 | 中国科学院大连化学物理研究所 | Multiphase catalytic reaction device for testing in situ solid-state nuclear magnetic resonance |
| CN201876386U (en) * | 2010-11-23 | 2011-06-22 | 北京汇丰隆经济技术开发有限公司 | Device for cracking bioaerosol mass spectrum at high temperature |
| CN102359986A (en) * | 2011-07-05 | 2012-02-22 | 中国科学院过程工程研究所 | In-situ detection device and detection method for heat conversion reaction process of solid fuel |
-
2013
- 2013-01-22 CN CN2013100217447A patent/CN103115956A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4626412A (en) * | 1984-12-14 | 1986-12-02 | Monsanto Company | Method and apparatus for carrying out catalyzed chemical reactions and for studying catalysts |
| EP1724574A1 (en) * | 2004-02-27 | 2006-11-22 | Japan Science and Technology Agency | Analytical method and analyzer capable of substantially simultaneously analyzing absorption/emission/scattering spectrum and mass spectrum, and analytical method and mass spectroscope utilizing electrospray ionization technique |
| CN101634651A (en) * | 2008-07-25 | 2010-01-27 | 中国科学院大连化学物理研究所 | Multiphase catalytic reaction device for testing in situ solid-state nuclear magnetic resonance |
| CN201876386U (en) * | 2010-11-23 | 2011-06-22 | 北京汇丰隆经济技术开发有限公司 | Device for cracking bioaerosol mass spectrum at high temperature |
| CN102359986A (en) * | 2011-07-05 | 2012-02-22 | 中国科学院过程工程研究所 | In-situ detection device and detection method for heat conversion reaction process of solid fuel |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104122322A (en) * | 2014-07-15 | 2014-10-29 | 江西中烟工业有限责任公司 | Method and device for detecting whole process of compound cracking |
| CN105784917A (en) * | 2014-12-26 | 2016-07-20 | 中国科学院大连化学物理研究所 | Application of mass spectrometer to detection process of ionized intermediates in catalytic reaction |
| CN105784917B (en) * | 2014-12-26 | 2018-06-29 | 中国科学院大连化学物理研究所 | Application of the mass spectrograph during detection is catalyzed reactive ion intermediate |
| CN107576717A (en) * | 2017-10-24 | 2018-01-12 | 中国科学技术大学 | A kind of in-situ detector for different diffusion length catalytic reaction gas phase intermediate products |
| CN107576717B (en) * | 2017-10-24 | 2019-10-25 | 中国科学技术大学 | A kind of in-situ detector being catalyzed reaction gas phase intermediate product for different diffusion lengths |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| WO2010121518A1 (en) | Method and apparatus for atmospheric pressure desorption ionization | |
| JP2015076338A (en) | Tandem quadrupole mass spectrometer | |
| Nakatani et al. | An analytical system for single-cell metabolomics of typical mammalian cells based on highly sensitive nano-liquid chromatography tandem mass spectrometry | |
| CN103115956A (en) | Low-pressure high-temperature pyrolysis furnace applicable to mass spectrographic analysis and application thereof | |
| CN106290210B (en) | A kind of method and detection system of atmospheric pressure glow discharge detection metal ion | |
| US11087966B1 (en) | Mass spectrum resolution device for measuring laser ablation ion species with improved time of flight mass spectrometry | |
| MX2012003626A (en) | Method for detecting molecules through mass spectrometry. | |
| CN102903596B (en) | A kind of ion source temperature control heating device | |
| CN105829880B (en) | Mass spectrometer and mass spectrometric analysis method | |
| CN104882352A (en) | Mass spectrum apparatus for gas-phase molecule-ion reaction and analysis method | |
| CN103084127A (en) | High-temperature normal-pressure catalytic reactor suitable for mass spectrometry and application thereof | |
| CN104966657A (en) | Sample introduction interface device for ionization source, mass spectrometry and liquid phase gas chromatograph-mass spectrometer | |
| CN111739785A (en) | Dual ion source slow electron speed imaging device | |
| CN103380371A (en) | Method and apparatus for detecting and identifying gases by means of ion mobility spectrometry | |
| CN103134878A (en) | Trapping and releasing method for improving gas chromatogram center cutting technique performance | |
| CN105301088A (en) | Accelerator mass spectrometer with simultaneous isotope measurement function | |
| CN104813162A (en) | Tandem quadrupole mass spectrometer | |
| WO2019000699A1 (en) | Novel chlorine/bromine isotope mass spectrometer and analysis method therefor | |
| CN108499499B (en) | Temperature-controllable micro continuous flow tube reactor | |
| CN104237371A (en) | Simple device for realizing real-time direct injection analysis of mass spectrometer and application of simple device | |
| CN108717010B (en) | Device for generating and screening atomized aerosol | |
| CN104377108A (en) | In-situ pyrolytic ion source for detecting free radicals and reaction intermediates | |
| US20180031529A1 (en) | Mass spectrometry method, chromatograph mass spectrometer, and program for mass spectrometry | |
| Santamaria-Fernandez et al. | Precise and traceable 13C/12C isotope amount ratios by multicollector ICPMS | |
| CN102683152B (en) | A kind of proton translocation mass ion source |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20130522 |