CN107356663A - Explosion-proof helium chromatography with discharge ionization detector - Google Patents

Explosion-proof helium chromatography with discharge ionization detector Download PDF

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Publication number
CN107356663A
CN107356663A CN201710765245.7A CN201710765245A CN107356663A CN 107356663 A CN107356663 A CN 107356663A CN 201710765245 A CN201710765245 A CN 201710765245A CN 107356663 A CN107356663 A CN 107356663A
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China
Prior art keywords
explosion
proof
cartridge
detector
helium
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Pending
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CN201710765245.7A
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Chinese (zh)
Inventor
王斌
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Chengdu Kai Sheng Jie Technology Co Ltd
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Chengdu Kai Sheng Jie Technology Co Ltd
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Priority to CN201710765245.7A priority Critical patent/CN107356663A/en
Publication of CN107356663A publication Critical patent/CN107356663A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
    • G01N27/68Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using electric discharge to ionise a gas
    • G01N27/70Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using electric discharge to ionise a gas and measuring current or voltage
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/62Detectors specially adapted therefor
    • G01N30/64Electrical detectors

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  • Chemical & Material Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

The present invention realizes the explosion-proof helium discharge detector in research and development in explosion-proof and non-explosion-proof industry, experiment, production, the instrument of quality inspection, instrument, with inert gas helium in detector quartz chamber body or in high temperature resistant, high pressure, the high ionized region to insulate, DC high-voltage is in high pressure cartridge and intensifies and forms region of discharge in the presence of cartridge, rapidly enter constant discharge, produce ion, form pulse direct current electric discharge, form electric arc, shwoot photon is stable into argon.Ion produces shock under the intensifying of high voltage power supply, forms the physical change process that energy obtains curtage signal, turns into the important evidence of other gas composition content sizes of the quantitative analysis in addition to helium element.This detector reaches national explosion-proof criteria or international explosion-proof criteria, has explosion-proof, flame proof, back-fire relief, the function of malleation purging integration.

Description

Explosion-proof helium chromatography with discharge ionization detector
Technical field
The present invention is the another core component in analytical instrument, instrument, applies to national defence, oil, chemical industry, gas, coke oven Coal gas, drilling well, mining, environmental protection, quality inspection, colliery, refinery, nuclear energy, space flight, medical, biogas, smelt, oxygen processed, semiconductor, Quality analysis, the process analysis fields such as printing and dyeing, welding.
Technical background
The currently detector in many analysis industry instruments, instrument, using non-explosion-proof casing, does not add spark arrester, Check-valves, without explosion prevention function, in the case that detector is in work, high pressure cartridge produces arc light, if in inflammable-explosive In fried gas or scene, is very easy to light fuel gas.Current many detector sensitivity for analysis all in ppm levels, analyze gas The body component excessively limit, far from the analysis for meeting gaseous impurity.This detector overcomes this difficulty, and test limit is as little as 0.1ppb poles, meet industry, national defence, the technical demand of scientific research.
The content of the invention
The present invention realizes the flexible design of multi-scheme multi-method, used;It is researching and developing, being real for explosion-proof and non-explosion-proof industry Test, produce, quality inspection, instrument, the explosion-proof helium discharge detector in instrument.This detector is the another core in analytical instrument, instrument Heart technology, it is widely used in the sensor of chromatographic field.National explosion-proof criteria and international explosion-proof criteria is fully achieved in one kind, can be Various explosion-proof occasion work.Detector housing has the function of flame proof.Detector entrance has check-valves, and purpose is exactly detector chamber When the air pressure of body uprises the pressure more than gas access suddenly, check-valves blocks air-flow by the way that material is thus formed can only immediately The function that air inlet will not flow backwards is realized explosion-proof.Analyze gas or purge gas helium enters detector quartz chamber body and powered high pressure Under cartridge collective effect, ionized region is produced, the collision of ion and ion produces a branch of corona shwoot arc light and forms ion, photon, Ion, photon produce energy, the motion process of ion and ion high-speed impact under the physical phenomenon high speed motion of high potential Middle generation electric current sends electric wave, and the collector through collecting region, which is collected, produces current signal or voltage signal.
Helium has inflow detector, just there is a reason of outflow, helium and the tested gas with impurity ionized region by from Spark arrester is flowed into after change, after ionized shock and loses energy, and by flow sensor, the flow passed through to air-flow carries out real-time Monitoring, under can so ensureing whether gas flow is maintained at identical conditions during analysis, this time analysis result reaches more Add accurate impression, more science.Small volume of the cavity of detector itself, purge gass all the way are devised in scheme, accelerate quartz The dead angle purging of cavity, purpose are exactly that pressure-fired is formed in detector cavity and produces more ions, are thus had just Pressure purging function, also cavity form more stable electron ion.
This detector is under conditions of closed, and in 400 DEG C of high temperature, under 10Mpa air pressure, leakage is less than 0.001mL Daily, 100 working days are without deformation;This detector canonical reference:《Chemical industry on-line gas chromatography》HG/T4095-2009、 GB 3836.1-2000/GB 3836.1-2010 explosion gas environment electrical installation Part I:General Requirement, GB 3836.5-2004 explosion gas environment electrical installation Part V:Ex "p" enclosure " P ", GB 9669.1-1998 industry Product description general provisions.The analytical instrument test methods of GB/T 11606 and design.
Technical principle
Its principle of this detector is exactly to be insulated in the case of completely closed, while in height in high resistance detector body, by(1) Purge gass helium passes through(2)Check-valves is through entering either(17)Analysis gas is directly entered quartz cavity arrival(30)After region of discharge.When (24)High pressure cartridge with(11)Intensify cartridge all carry high-tension electricity in the case of, discharge electrode(Cartridge or pole pipe)Voltage be greater than 400 volts of high pressures, intensify pole tension and can not be equal to 0 volt, while on the premise of the concentration Reinheitszahl of helium is greater than certain value, now Region of discharge two-stage can just produce(30)Ionized region.Under being acted at high-tension the two poles of the earth, the corona for producing a branch of high-energy forms arc Light, aura produce photon, electronics, ion simultaneously.Move and produce in high-tension electric field high speed(20)Ionized region is tightly attached to In quartz chamber body.
When helium is intensified by a large amount of helium atoms of ionized region, the helium atom being intensified and electron collision generation helium ion are steady Fixed DC pulse turns into metastable state.It is positive and negative that the helium that collector spout sprays or the gas with impurity are intensified generation again Electric charge, it is ionized in ionized region and produces high-speed motion, hits generation energy, produced by during this releases energy Curtage turns into signal.
When analyzed drive of the gaseous impurity through helium, into the ionization of detector ionized region, it is intensified, pure helium Caused helium atom has high-energy, if impurity molecule or atom with separation bring into ionized region occur inelastic collision or Accelerate collision so that the energy dropoff of helium atom or enhancing, now add an appropriate voltage on extremely in intensifying for region of discharge, be ionized Atom formed charge order entrance(31)Collecting region quilt(14)Nozzle collector passes out.By(28)Collector, record Instrument or miscellaneous equipment are recorded to form electric wave signal.Foreign atom, the molecule being ionized, it can obtain with standard specimen concentration into just Than or the electric current, the voltage signal that are inversely proportional.The complete electric wave signal of a width is obtained after processing of circuit, this just becomes tested miscellaneous The Wave crest and wave trough spectrogram of matter content value.
Electric wave signal caused by the content of this detector analysing impurity is directly proportional to standard sample gas or inverse ratio, detector The sensitivity of linear wider detection is higher, and test limit is lower.High voltage power supply, intensify power supply in the case where condition is certain, The purity of helium is to determine that detector appraises and decides quantitative basis, is to provide the Main Basiss of 1 boundary's point of analysing impurity content.
The sensitivity of detector and high voltage power supply, intensify supply voltage, jet size, cavity volume, insulaion resistance, cartridge Or pole pipe material spaced position, helium purity are relevant, voltage more High Linear is wider, and frequency is faster, and sensitivity is higher.
Embodiment.
Brief description of the drawings
Fig. 1:Summary figure
Fig. 2:Theory structure scheme one
Fig. 3:Theory structure scheme two
Fig. 4:Theory structure scheme three
Fig. 5:Theory structure scheme four
Fig. 6:Theory structure scheme five
Fig. 7:Theory structure scheme six
Fig. 8:Theory structure scheme seven
Fig. 9:Theory structure scheme eight
The design of this detector uses this detector canonical reference completely:《Chemical industry on-line gas chromatography》HG/T4095-2009、 GB 3836.1-2000/GB 3836.1-2010 explosion gas environment electrical installation Part I:General Requirement, GB 3836.5-2004 explosion gas environment electrical installation Part V:Ex "p" enclosure " P ", GB 9669.1-1998 industry Product description general provisions.The analytical instrument test methods of GB/T 11606 are standard.
The organization plan of detector be by:1 purge gass entrance, 2 check-valves, 3 end caps, 4 polymer insulation packing materials, 5 Intensify high insulated cable, 6 electric discharge high voltage insulation cables, 7 high voltage insulating columns, 8 gas outlets, 9 spark arresters, 10, flow sensor, 11 Intensify cartridge, 12 housings, 13 spouts, 14 jet pipe collectors, 15 collection insulated columns, 16, collect signal wire, 17 analysis gases enter Mouth, 18 quartz observing windows, 19, quartz wall, 20 ionized regions, 21 felt pads, 22 high pressure pole pipes, 23 ground wires, 24 high pressure cartridges, 25 Intensify pole pipe, 26 high voltage power supplies, 27 intensify power supply, 28 recorders, 29 operational amplifiers, 30 region of discharges, 31 collecting regions etc..
Explosion-proof helium discharge detector as shown in FIG., the material that can be used in ionized region cavity:Quartz ampoule, alundum tube, The material of tubular zirconium-oxide, earthenware or ceramic coated, zirconium oxide, silica, high temperature resistant, high pressure, high insulation etc. is tightly bonded in The superficial layer of ionized region, the tube wall of formation or skin depth >=0.01 millimeter, ionized region cavity length is at >=0.1 millimeter.
Cartridge in explosion-proof helium discharge detector, pole pipe are using platinum gold, silver, titanium, nickel, zinc, alloy, tungsten, kovar alloy, stainless A variety of good conductivities such as steel, resistant to elevated temperatures intermetallic composite coating form.What is be processed into intensifies cartridge, high pressure cartridge into column, is processed into Intensify pole pipe, high pressure pole pipe and jet pipe collector and be more than 0.1 millimeter into tubulose, their diameter, the diameter of bore of tubulose is more than 0.05 millimeter;Intensify cartridge with high pressure cartridge and the arcing distance for intensifying pole pipe and high-voltage tube more than 0.01 millimeter, intensify cartridge With high pressure cartridge and intensify the discharge end of pole pipe and high-voltage tube and the jet opening distance of spout collector more than 0.01 millimeter.
Explosion-proof helium discharge detector cartridge, the supply voltage of pole pipe swash between minus 10000 to 10000 volt dc source Change pipe, intensify the supply voltage of pole between minus 2000 to 10000 volt direct current.
The key point of invention
1st, have it is simple in construction, stable performance, sensitivity is suitable, and the range of linearity is wide, the analysis of detection limit as little as (ppb levels);
2nd, the resistance to hyperbaric pressures of this detector, the normal work under 1.5Mpa air pressure;
3rd, this detector keeps normal work under 400 DEG C of conditions environmentals;
4th, as low as 10 microlitres of the ionized region cavity volume of this detector;
5th, detector cavity can use py types malleation to purge;
6th, the explosion-proof casing of detector is designed using two class T1 explosion-proof criterias;This detector gas consumption is small, detector of the invention According to national explosion-proof criteria or the design of international explosion-proof criteria, processing, production, use.Detector has back-fire relief, check-valves, quartz The integrated functions such as insulating barrier, flow sensor, explosion-proof, flame proof, malleation purging;
7th, the air intake of detector, analysis gas access use check-valves, and outlet prevents detector circulation chamber using spark arrester Flame extension lights the explosion precaution of the fuel gas in downstream and upstream or the external world;
8th, the check-valves of the air intake in detector employ unique design, special piston seal material, special piston plus Work technique, cavity volume are small, dead angle is small, have accomplished only to enter the characteristics of not flowing back;
9th, detector can ensure detector normal work without temperature element, heater heating;
10th, detector ionized region, insulated column are process using high insulating materials such as ceramic, quartzy tube walls.

Claims (4)

1. the operation principle of explosion-proof helium discharge detector is in detector quartz chamber body or high temperature resistant, height using inert gas helium In pressure, the high ionized region to insulate, constant discharge is rapidly entered after energization, produces pulse direct current electric discharge, ion gun is formed and produces The physical process of curtage signal, it is claimed as follows:
Explosion-proof helium discharge detector is claimed as shown in FIG.:By structural principle scheme one to the design of scheme eight, component, The occupation mode method formed is shown in logical order and all figures.
2. explosion-proof helium discharge detector is claimed as illustrated in the drawing in ionized region cavity using material, volume, length etc., Such as:Quartz ampoule, alundum tube, tubular zirconium-oxide, earthenware or ceramic coated, zirconium oxide, silica, high temperature resistant, high pressure, height insulate Material is tightly bonded in the top layer of ionized region, and the tube wall or skin depth of formation are between 0.01 to 5 millimeters, ionized region cavity length Degree is between 0.1 millimeter to 50 millimeters.
3. explosion-proof helium discharge detector ionized region cavity size, electric discharge cartridge, the fortune of collector as illustrated in the drawing is claimed With, methods, the scope using material, size and spacing of discharging, such as:Ionized region cavity diameter 0.1 to 20 millimeters it Between, between 0.1 to 100 millimeters of length;Electric discharge cartridge and collector using platinum gold, silver, titanium, nickel, zinc, alloy, tungsten, conjunction can be cut down A variety of good conductivities such as gold, stainless steel, resistant to elevated temperatures intermetallic composite coating form;What can be processed into intensifies cartridge, high pressure cartridge Cheng Zhu Shape, intensify pole pipe, high pressure pole pipe and jet pipe collector into tubulose with being processed into, they between 0.1 to 17 millimeters of diameter, pipe The endoporus of shape is between 0.05 to 16 millimeters;Intensify cartridge and high pressure cartridge and intensify pole pipe and the arcing distance of high-voltage tube exists Between 0.01 to 19 millimeters;Intensify the spray of cartridge and high pressure cartridge and the discharge end and spout collector that intensify pole pipe and high-voltage tube Mouth distance is between 0.01 to 5 millimeters.
4. be claimed explosion-proof helium discharge detector cartridge, pole pipe supply voltage scope, such as:Intensify cartridge and high-pressure stage DC voltage is between minus 10000 to 10000 volt.
CN201710765245.7A 2017-08-30 2017-08-30 Explosion-proof helium chromatography with discharge ionization detector Pending CN107356663A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710765245.7A CN107356663A (en) 2017-08-30 2017-08-30 Explosion-proof helium chromatography with discharge ionization detector

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710765245.7A CN107356663A (en) 2017-08-30 2017-08-30 Explosion-proof helium chromatography with discharge ionization detector

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CN107356663A true CN107356663A (en) 2017-11-17

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113376242A (en) * 2021-06-10 2021-09-10 王斌 Hydrocarbon ion detector

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113376242A (en) * 2021-06-10 2021-09-10 王斌 Hydrocarbon ion detector
CN113376242B (en) * 2021-06-10 2023-06-20 王斌 Hydrocarbon ion detector

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Application publication date: 20171117