CN202486056U - Sulfur detector based on dielectric barrier discharge mode atomic emission spectroscopy - Google Patents

Sulfur detector based on dielectric barrier discharge mode atomic emission spectroscopy Download PDF

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Publication number
CN202486056U
CN202486056U CN2012200113379U CN201220011337U CN202486056U CN 202486056 U CN202486056 U CN 202486056U CN 2012200113379 U CN2012200113379 U CN 2012200113379U CN 201220011337 U CN201220011337 U CN 201220011337U CN 202486056 U CN202486056 U CN 202486056U
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China
Prior art keywords
discharge
atomic emission
dielectric barrier
electrode
emission spectrum
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Expired - Fee Related
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CN2012200113379U
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Chinese (zh)
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黄军维
刘霁欣
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BEIJING JITIAN INSTRUMENT Co Ltd
Beijing Titan Instruments Co Ltd
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BEIJING JITIAN INSTRUMENT Co Ltd
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Abstract

The utility model discloses a sulfur detector based on dielectric barrier discharge mode atomic emission spectroscopy. The sulfur detector comprises a power supply, a discharge camber, electrodes, and a detector, wherein the discharge chamber is made of a dielectric layer, the front end of the discharge chamber is provided with a sample inlet, the discharge chamber is internally provided with a discharge channel, the discharge channel is in a straight line shape, the external surfaces of the left side wall and the right side wall of the discharge chamber are respectively fixed with a left electrode and a right electrode, the power supply is connected with the left electrode and the right electrode in series, and the detector is arranged at the rear side of an outlet end of the discharge chamber. According to the sulfur detector disclosed by the sulfur detector, a sample flows through a dielectric barrier discharge field at normal pressure, the compound of the sample is decomposed, sulfur in the sample is combined again to form exited state S2 molecules, and characteristic spectrum lines are sent out, so that the content of the sulfur in the sample can be detected. The sulfur detector has the advantages of compactness in structure, small dead volume, convenience for carrying, low energy consumption, low operating temperature and high sensitivity. The sulfur detector can be used in the chromatographic detection of the sulfur and sulfide, and the atomic emission detection, and is the premise and powerful guarantee for realizing the onsite operation, the miniaturization and the portability of a chromatography analyzer.

Description

Sulphur detecting device based on dielectric barrier discharge pattern atomic emission spectrum
Technical field
The utility model relates to sulphur and sulfide detection technique field in the analytical instrument, particularly relates to a kind of sulphur detecting device based on dielectric barrier discharge pattern atomic emission spectrum.
Background technology
The sulphur detecting device is one of important detecting device of chromatogram and Atomic Emission Spectral Analysis instrument, and the height of detection sensitivity is directly connected to the performance of instrument, the analysis detection limit of it and instrument, and precision, stability is directly related.In the analytical instrument there be sulphur detection method commonly used at present: based on the AAS of chemical colour reaction reaction, and the potentiometric titration of potential change during based on sulphuric dioxide and the interaction of IKI battery, four kinds of ICP atomic emission spectrometry and sulphur P detectors.The main now sulphur P detector that adopts of chromatogram and Atomic Emission Spectral Analysis instrument.
AAS only is applicable to the analysis of fluid sample, in system, add complicated developer, and chromogenic reaction receives temperature, the influence of acidity, and color speed is slow, can not continuous detecting, be not suitable for the requirement of chromatographic apparatus.Potentiometric titration can be measured the sulphur in the air sample, but can not distinguish sulphur and chemical homolog selenium in the sample, can not be used for stratographic analysis.Inductively coupled plasma (ICP), its working temperature is high, and the atomic excitation ability is strong, and matrix disturbs little, is multielement composite property detecting device, but the bulky operating cost of ICP is high, has limited its range of application.The sulphur P detector is existing usefulness sulphur detecting device the most widely, and is simple in structure, highly sensitive, but dead volume is bigger than normal, and thermal value is high, and baseline wander can take place long-term the use, needs correction of timing when measuring for a long time.Dielectric barrier discharge is a gas discharge under a kind of atmospheric pressure of electrode surface overwrite media, and apparent is the gas discharge that evenly fills the air, and it is worked under normal pressure, and volume is little, and working temperature is low, and energy consumption is low.Still unexposed report is based on the sulphur detecting device of dielectric barrier discharge pattern atomic emission spectrum at present.
The utility model content
The technical matters that the utility model will solve provides a kind of compact conformation, volume is little, working temperature is low, energy consumption is low, the highly sensitive sulphur detecting device based on dielectric barrier discharge pattern atomic emission spectrum.
For solving the problems of the technologies described above, the utility model adopts following technical scheme:
A kind of sulphur detecting device based on dielectric barrier discharge pattern atomic emission spectrum comprises power supply, discharge cavity, electrode, detector, and discharge cavity is processed by dielectric layer; The inside of discharge cavity is discharge channel, and discharge channel is a linear pattern, the fixing respectively left and right electrode of the outside surface of the left and right sidewall of discharge cavity; Power supply is connected with left and right electrode; The front end of discharge cavity is provided with sample inlet, and detector is arranged on the rear side of discharge cavity endpiece, the outer setting insulation course of discharge cavity.
The utility model is based on the sulphur detecting device of dielectric barrier discharge pattern atomic emission spectrum, and wherein said left and right electrode is symmetrical with the center line of discharge cavity, and left and right electric discharge between electrodes spacing is 0.5mm-5mm.
The utility model is based on the sulphur detecting device of dielectric barrier discharge pattern atomic emission spectrum, and the thickness of dielectric layers of wherein said discharge cavity is: 0.1mm to 5mm.
The utility model is based on the sulphur detecting device of dielectric barrier discharge pattern atomic emission spectrum, and wherein said detector is optical filter and photomultiplier, and optical filter is arranged on the exit of discharge cavity, and the rear end of optical filter is provided with photomultiplier.
The utility model is based on the sulphur detecting device of dielectric barrier discharge pattern atomic emission spectrum, and wherein said detector is a spectrometer.
The utility model is based on the sulphur detecting device of dielectric barrier discharge pattern atomic emission spectrum, and wherein said dielectric layer adopts aluminium oxide ceramics, zirconia ceramics, and boron nitride ceramics, aluminium nitride ceramics, quartz or glass are processed.
The utility model is based on the sulphur detecting device of dielectric barrier discharge pattern atomic emission spectrum, and wherein said left and right electrode is silk ribbon shape electrode or coat film electrode.
The utility model is based on the sulphur detecting device of dielectric barrier discharge pattern atomic emission spectrum, and wherein said silk ribbon shape electrode is aluminium foil or copper foil electrode, on the left and right sidewall that is adhesive in discharge cavity.
The utility model is based on the sulphur detecting device of dielectric barrier discharge pattern atomic emission spectrum, and wherein said coat film electrodes use Jinsui River or silver-colored water are coated on the discharge cavity sidewall, forms electrode through behind the high temperature sintering.
The utility model is based on the sulphur detecting device of dielectric barrier discharge pattern atomic emission spectrum, and the xsect of wherein said discharge cavity is a square or rectangular, and the outside surface of insulation course is cylindrical.
The utility model is often depressed the dielectric barrier discharge field based on the sulphur detecting device sample flow of dielectric barrier discharge pattern atomic emission spectrum, and sample compound decomposes, and sulphur wherein reconfigures, and forms excited state S 2Molecule, and send characteristic spectral line, thus record sulfur content in the sample; This detecting device has compact conformation, and dead volume is little, and is easy to carry; Energy consumption is low; Low and the highly sensitive advantage of working temperature, the chromatogram that can be used for sulphur and sulfide detects, atomic emissions detects, and is the prerequisite and the strong guarantee of chromatogram alanysis instrument scene, miniaturization, portability.Compare with the sulphur P detector, the discharge channel volume of the utility model sulphur detecting device is little, and the launch spot of generation is concentrated, and spectral intensity is high, and is highly sensitive.
Be described further below in conjunction with the sulphur detecting device based on dielectric barrier discharge pattern atomic emission spectrum of accompanying drawing the utility model.
Description of drawings
Fig. 1 is the structural representation of the utility model based on the sulphur detecting device of dielectric barrier discharge pattern atomic emission spectrum;
Fig. 2 is the A-A sectional view of Fig. 1.
Embodiment
Like Fig. 1, shown in 2; The utility model comprises power supply 1, discharge cavity 2, left and right electrode 31,32, optical filter 4, photomultiplier 5 based on the sulphur detecting device of dielectric barrier discharge pattern atomic emission spectrum; But power supply 1 is the AC power of voltage regulation and frequency modulation; Discharge cavity 2 forms by dielectric layer is bonding, and its xsect is a square or rectangular.Thickness of dielectric layers is: 0.1mm to 5mm, and dielectric layer adopts aluminium oxide ceramics, zirconia ceramics, boron nitride ceramics, aluminium nitride ceramics, quartz or glass are processed, its purity from 50.00% to 99.99%.The front end of discharge cavity 2 is provided with sample inlet 21, and inside is discharge channel 22, and discharge channel 22 is a linear pattern.The fixing respectively left and right electrode 31,32 of the outside surface of the left and right sidewall of discharge cavity 2, left and right electrode 31,32 is symmetrical with the center line of discharge cavity 2, and left and right electrode 31,32 can be silk ribbon shape electrode or coat film electrode.Silk ribbon shape electrode can be aluminium foil or copper foil electrode, on the left and right sidewall that is adhesive in discharge cavity 2.The coat film electrode can adopt Jinsui River or silver-colored water or other molten metals to be coated on discharge cavity 2 sidewalls, behind high temperature sintering, forms electrode.Power supply 1 links to each other with 31,32 series connection of left and right electrode, and left and right electrode 31, the discharge spacing between 32 are 0.5mm-5mm.
The outer setting insulation course 6 of discharge cavity 2, the outside surface of insulation course 6 are cylindrical.
Optical filter 4 is arranged on the exit of discharge cavity 2, and the rear end of optical filter 4 is provided with photomultiplier 5.
In the utility model, also can spectrometer be set, replace optical filter and photomultiplier to detect at the endpiece of discharge cavity.
The utility model based on the testing process of the sulphur detecting device of dielectric barrier discharge pattern atomic emission spectrum is: the sulphur detecting device is installed on the sulfide analysis appearance; Feed discharge gas at sample inlet 21, energized 1, the adjusting electric power output voltage is: 5000 volts to 20000 volts; Discharge frequency is 10KHz to 200KHz; Gather air sample with the atmospheric sampling machine and feed in the carrier gas, the sulfide molecules region of discharge of flowing through is broken down into sulphur atom, is combined into excited state S again 2Molecule; And send characteristic spectral line, and the parasitic light of optical filter 2 other wavelength of filtering, optical signals photomultiplier 5 detects; Thereby measure airborne sulphuric dioxide; This detecting device has very high sensitivity to sulphur, and signal is quafric curve response with sample concentration, to the measurement range of sulphur is: 0.001%-0.1% (v/v).
In the above-mentioned testing process, discharge gas flow 1 milliliters/second to 1000 milliliters/second, discharge gas adopts argon gas, helium, nitrogen, the air behind the high-purity gas of hydrogen or the combination gas of different proportion or process filtration and the purifying.
The utility model can be through regulating sparking voltage based on the sulphur detecting device of dielectric barrier discharge pattern atomic emission spectrum; Discharge frequency; Spacing between discharge cavity two electrodes changes region of discharge electric field intensity; Change discharge condition and discharge power and can produce dissimilar sulphur emission spectrum, be convenient in analyzing practice, select the high spectral line of signal to noise ratio (S/N ratio).
The utility model sulphur detector volume is little, and core texture only is equivalent to the size of adult's thumb, and is simple in structure; Energy consumption is low, only needs 5-30 watt power input to get final product operate as normal, working temperature low (<50 ℃); Instrument component influence to adjacent is little, is convenient to the integrated and miniaturization of instrument.
Above-described embodiment describes the preferred implementation of the utility model; Be not that scope to the utility model limits; Under the prerequisite that does not break away from the utility model design spirit; Various distortion and improvement that those of ordinary skills make the technical scheme of the utility model all should fall in the definite protection domain of the utility model claims.

Claims (10)

1. sulphur detecting device based on dielectric barrier discharge pattern atomic emission spectrum, it is characterized in that: comprise power supply, discharge cavity, electrode, detector, discharge cavity is processed by dielectric layer; The inside of discharge cavity is discharge channel, and discharge channel is a linear pattern, the fixing respectively left and right electrode of the outside surface of the left and right sidewall of discharge cavity; Power supply is connected with left and right electrode; The front end of discharge cavity is provided with sample inlet, and detector is arranged on the rear side of discharge cavity endpiece, the outer setting insulation course of discharge cavity.
2. the sulphur detecting device based on dielectric barrier discharge pattern atomic emission spectrum according to claim 1 is characterized in that: said left and right electrode is symmetrical with the center line of discharge cavity, and left and right electric discharge between electrodes spacing is 0.5mm-5mm.
3. the sulphur detecting device based on dielectric barrier discharge pattern atomic emission spectrum according to claim 2, it is characterized in that: the thickness of dielectric layers of said discharge cavity is: 0.1mm to 5mm.
4. the sulphur detecting device based on dielectric barrier discharge pattern atomic emission spectrum according to claim 3; It is characterized in that: said detector is optical filter and photomultiplier; Optical filter is arranged on the exit of discharge cavity, and the rear end of optical filter is provided with photomultiplier.
5. the sulphur detecting device based on dielectric barrier discharge pattern atomic emission spectrum according to claim 3 is characterized in that: said detector is a spectrometer.
6. according to claim 4 or 5 described sulphur detecting devices based on dielectric barrier discharge pattern atomic emission spectrum, it is characterized in that: said dielectric layer adopts aluminium oxide ceramics, zirconia ceramics, and boron nitride ceramics, aluminium nitride ceramics, quartz or glass are processed.
7. the sulphur detecting device based on dielectric barrier discharge pattern atomic emission spectrum according to claim 6 is characterized in that: said left and right electrode is silk ribbon shape electrode or coat film electrode.
8. the sulphur detecting device based on dielectric barrier discharge pattern atomic emission spectrum according to claim 7 is characterized in that: said silk ribbon shape electrode is aluminium foil or copper foil electrode, on the left and right sidewall that is adhesive in discharge cavity.
9. the sulphur detecting device based on dielectric barrier discharge pattern atomic emission spectrum according to claim 7 is characterized in that: said coat film electrodes use Jinsui River or silver-colored water are coated on the discharge cavity sidewall, form electrode through behind the high temperature sintering.
10. according to Claim 8 or 9 described sulphur detecting devices based on dielectric barrier discharge pattern atomic emission spectrum, it is characterized in that: the xsect of said discharge cavity is a square or rectangular, and the outside surface of insulation course is cylindrical.
CN2012200113379U 2012-01-11 2012-01-11 Sulfur detector based on dielectric barrier discharge mode atomic emission spectroscopy Expired - Fee Related CN202486056U (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103091303A (en) * 2013-02-05 2013-05-08 大连海事大学 Method for detecting alkali metal elements in drinking water
CN103149195A (en) * 2013-03-06 2013-06-12 河海大学 Spectrum detection method and device for dielectric barrier discharge
CN103760138A (en) * 2014-02-17 2014-04-30 哈尔滨工业大学(威海) Portable DBD (dielectric barrier discharge) plasma spectrometer
CN106872417A (en) * 2017-03-06 2017-06-20 大连理工大学 Using SDBD and the experimental provision and method of emission spectrum detection OH concentration
CN104502330B (en) * 2014-12-12 2017-06-27 大连理工大学 A kind of LIBS detection means for detecting fluid sample
CN112782174A (en) * 2020-12-25 2021-05-11 西南化工研究设计院有限公司 High-frequency electrodeless argon discharge ionization detector and method for analyzing sulfur and phosphorus compounds in gas

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103091303A (en) * 2013-02-05 2013-05-08 大连海事大学 Method for detecting alkali metal elements in drinking water
CN103091303B (en) * 2013-02-05 2015-04-15 大连海事大学 Method for detecting alkali metal elements in drinking water
CN103149195A (en) * 2013-03-06 2013-06-12 河海大学 Spectrum detection method and device for dielectric barrier discharge
CN103760138A (en) * 2014-02-17 2014-04-30 哈尔滨工业大学(威海) Portable DBD (dielectric barrier discharge) plasma spectrometer
CN104502330B (en) * 2014-12-12 2017-06-27 大连理工大学 A kind of LIBS detection means for detecting fluid sample
CN106872417A (en) * 2017-03-06 2017-06-20 大连理工大学 Using SDBD and the experimental provision and method of emission spectrum detection OH concentration
CN106872417B (en) * 2017-03-06 2019-10-11 大连理工大学 Utilize the experimental provision and method of SDBD and emission spectrum detection OH concentration
CN112782174A (en) * 2020-12-25 2021-05-11 西南化工研究设计院有限公司 High-frequency electrodeless argon discharge ionization detector and method for analyzing sulfur and phosphorus compounds in gas

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