CN109716118A - Acetylene gas analytical equipment and analysis method for buried cable - Google Patents
Acetylene gas analytical equipment and analysis method for buried cable Download PDFInfo
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- CN109716118A CN109716118A CN201680089457.1A CN201680089457A CN109716118A CN 109716118 A CN109716118 A CN 109716118A CN 201680089457 A CN201680089457 A CN 201680089457A CN 109716118 A CN109716118 A CN 109716118A
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- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 title claims abstract description 135
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 title claims abstract description 135
- 238000004458 analytical method Methods 0.000 title claims abstract description 27
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 claims abstract description 76
- 238000006703 hydration reaction Methods 0.000 claims abstract description 75
- 239000003054 catalyst Substances 0.000 claims abstract description 47
- 230000036571 hydration Effects 0.000 claims abstract description 45
- 238000001514 detection method Methods 0.000 claims abstract description 40
- 238000004868 gas analysis Methods 0.000 claims abstract description 19
- 150000001412 amines Chemical class 0.000 claims description 30
- 238000005259 measurement Methods 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 18
- -1 silane compound Chemical class 0.000 claims description 18
- 229910000077 silane Inorganic materials 0.000 claims description 16
- 239000002159 nanocrystal Substances 0.000 claims description 12
- 239000012528 membrane Substances 0.000 claims description 9
- 238000004445 quantitative analysis Methods 0.000 claims description 9
- 125000003277 amino group Chemical group 0.000 claims description 7
- 125000000879 imine group Chemical group 0.000 claims description 7
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 claims description 6
- 238000010276 construction Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 4
- 150000001345 alkine derivatives Chemical class 0.000 claims description 3
- 230000000149 penetrating effect Effects 0.000 claims description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 239000013078 crystal Substances 0.000 claims 1
- 238000002444 silanisation Methods 0.000 claims 1
- 238000003745 diagnosis Methods 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 125
- 239000000243 solution Substances 0.000 description 24
- 238000004817 gas chromatography Methods 0.000 description 6
- 150000002466 imines Chemical class 0.000 description 6
- 230000035945 sensitivity Effects 0.000 description 5
- IFRZFIUBFCZXKK-UHFFFAOYSA-N 3-triethoxysilylpropan-1-amine;n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CCO[Si](OCC)(OCC)CCCN.CO[Si](OC)(OC)CCCNCCN IFRZFIUBFCZXKK-UHFFFAOYSA-N 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 4
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000004587 chromatography analysis Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000002441 reversible effect Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- LPLLVINFLBSFRP-UHFFFAOYSA-N 2-methylamino-1-phenylpropan-1-one Chemical compound CNC(C)C(=O)C1=CC=CC=C1 LPLLVINFLBSFRP-UHFFFAOYSA-N 0.000 description 1
- 240000003023 Cosmos bipinnatus Species 0.000 description 1
- 235000005956 Cosmos caudatus Nutrition 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000001960 triggered effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/129—Diode type sensors, e.g. gas sensitive Schottky diodes
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0004—Gaseous mixtures, e.g. polluted air
- G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
- G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
- G01N33/0036—General constructional details of gas analysers, e.g. portable test equipment concerning the detector specially adapted to detect a particular component
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- General Physics & Mathematics (AREA)
- Pathology (AREA)
- Immunology (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Combustion & Propulsion (AREA)
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Abstract
The application provides a kind of acetylene gas analytical equipment and analysis method for buried cable.Equipment utilization gas to be analyzed contacts with acetylene hydration catalyst, and generated acetaldehyde analyzes the acetylene content in the gas.Therefore, it can be detected the only acetylene gas of a small amount of about 10mL by the application, detection lower bound is about 0.01ppm, can be used for Precise Diagnosis, and can carry, therefore can directly carry out acetylene gas analysis at the scene.
Description
Technical field
This application involves a kind of acetylene gas analytical equipment and analysis methods, are used for underground more specifically to one kind
The acetylene gas analytical equipment and analysis method of cable.
Background technique
Buried cable is a kind of facility by electric wire embedment underground, and composed structure is complicated, can replace it is overhead communicate and
Power transmission line promotes urban, is continuously increased in demand.In addition, in order to reduce the possibility complained in construction,
When developing NPD projects garden, public domain internal frame good buried cable facility of the meeting in advance inside garden.
Be continuously increased recently as the demand to underground cable installation, for can find and prevent in advance equipment fault,
The exploitation demand of convenient detection technique is also growing day by day.
The traditional Examined effect of one of them acquires in underground cable box according to method defined in ASTM D3612
Gas, and in the lab according to gas-chromatography (GC) analyze.Make with the aforedescribed process, collected gas is separated and surveyed
Amount, then judge whether insulating oil is abnormal, and insulating paper is by gas concentrations such as measured hydrogen, carbon dioxide, methane, acetylene
No overheat, the unit exceptions such as arc discharge and dielectric strength deterioration.However, using gas-chromatography (GC) in the lab
The method for carrying out gas analysis, it is necessary to first acquire the gas in terminal box as sample, be then sent through laboratory.Therefore it carries
Process may will affect the precision of result, and carry out with high costs, the Zhi Nengyou spent needed for the equipment of gas chromatographic analysis
Expert carries out the shortcomings that analysis is also this method.
In addition, there are also use flame ion detector (FID:Flame Ionization in acetylene gas analysis
Detector) this analysis method.If but only contain micro acetylene in sample gas, it is not only difficult to measure, and sample needs
It send from scene to laboratory, during carrying, there may be variations for the composition of gas, may make the precision drop of analysis
It is low.
Therefore, it is the precision for improving fault detection, needs a kind of directly collecting sample, and the side analyzed at the scene
Method.Importantly, need portable detection device when testing staff detects gas anomaly, testing staff's energy is allowed
It is detected at the scene of being directly brought into.
Presently commercially available acetylene detection device can be basically divided into two kinds, first is that carrying out via aerial gas is spread
The diffusion type detection device of detection, second is that forcing sucking gas to be detected via side Pu or air ejector (air aspirator)
Suction-type detection device.For diffusion type detector, be detected by spreading aerial gas, therefore to point
The concentration of gassing body must be very high, for example, concentration must at least reach 10,000ppm or higher, so not being suitable for diagnosing
The exception of electric power facility.For suction-type detector, although sensitivity is better than diffusion type detector, it can detecte out several ppm
To the concentration of 1,000ppm, if but detect required sample size up to several L or more, it has to last for that detector is allowed to suck sample, because
If the only a small amount of gas of this junction box, can not be analyzed.
Therefore, at present for only with a small amount of gas sample can complete acetylene gas detection, and can reduce detection lower bound,
Increase detection precision, and buried cable acetylene gas analytical equipment easy to carry, and can directly being analyzed at the scene
Demand increasing.
Summary of the invention
The project that must be solved
The purpose of the application be to invent it is a kind of with micro sample just can be carried out acetylene gas analysis, reduce detection it is low
Limit improves detection precision, and easy to carry, can directly execute the buried cable acetylene gas point of gas analysis at the scene
Desorption device and its analysis method.
Solve the mode of project
One embodiment of the application is the acetylene gas analytical equipment for buried cable.There is reaction zone inside equipment,
Acetylene hydration catalyst solution is stored, makes gas to be analyzed by acetylene hydration catalyst, can be by the acetylene hydration in gas
Acetaldehyde；There is measurement zone, be connected to reaction zone, when acetaldehyde is introduced measurement zone, measurement zone inner wall has surface to be coated with amine-containing gas silicon
The ZnO nano crystal of hydride compounds can be reacted with acetaldehyde generation, so that conductivity is generated variation, and in measurement conductivity herein
Variable quantity；In addition, there is quantitative analysis area, the resulting conductivity variable quantity of analysis detection is calculated contained in gas to be analyzed
Acetylene content, and show result.
Another embodiment in the application is the method analyzed for the acetylene gas of buried cable, is made first to be analyzed
Gas is reacted with acetylene hydration catalyst, acetaldehyde caused by reacting is recycled, to calculate the acetylene in gas to be analyzed
Content.
Invention effect
Even the application provides the trace sample of 10mL, acetylene gas detection can also be carried out, detection lower bound is
0.1ppm can be used for accurate diagnosis, and easy to carry, can directly execute gas analysis at the scene, detect equipment event in advance
Hinder the acetylene gas analytical equipment and analysis method of situation.
Detailed description of the invention
Fig. 1 is the structure of acetylene gas detection device in the application.
Fig. 2 is the rough schematic of conventional gas phase chromatography eudiometry.
Fig. 3 is the general introduction of acetylene gas analysis method used in this application.
Specific embodiment
One embodiment in the application is the acetylene gas analytical equipment for buried cable.There is reaction inside equipment
Acetylene hydration catalyst solution is stored in area, makes gas to be analyzed by acetylene hydration catalyst, can be by the acetylene hydration in gas
For acetaldehyde；There is measurement zone, be connected to reaction zone, when acetaldehyde is introduced measurement zone, measurement zone inner wall has surface to be coated with amine-containing gas
The ZnO nano crystal of silane compound can react with acetaldehyde generation, generate conductivity and change, and in measure conductivity herein
Variable quantity；In addition, there is quantitative analysis area, the resulting conductivity variable quantity of analysis detection is calculated contained in gas to be analyzed
Acetylene content, and show result.
By the analysis method in the application, even the trace sample of about 10mL, acetylene gas detection, inspection also can be carried out
Survey lower bound is 0.1ppm, can be used for accurate diagnosis, and easy to carry, can directly carry out gas analysis at the scene, is detected in advance
Out the case where equipment fault.
Fig. 1 is the structure of acetylene gas detection device in the application.Hereinafter, the second that will be illustrated in embodiment with Fig. 1
Alkynes gas analysis arrangement.
Acetylene gas analytical equipment in the application includes hydration reaction area (100), conductivity measurement area (200) and quantifies
(300) three blocks of analysis area.
Acetylene hydration catalyst (101) are stored in hydration reaction area (100), and it is anti-by hydration to be analysed to gas (G)
When answering the acetylene hydration catalyst in area, the acetylene in gas (G) to be analyzed can generate acetaldehyde via hydration reaction.
Specifically, the container of storage acetylene hydration catalyst solution (101) is double-walled knot in hydration reaction area (100)
Therefore structure keeps the temperature the excellent effect of acetylene hydration catalyst solution, and the acetylene that can be promoted in gas to be analyzed (G) is converted to
The efficiency of acetaldehyde.
Hydration reaction area (100) is not particularly limited in volume, can be between 50mL to 100mL.When within this range,
Equipment can be made easily portable.In addition, storage acetylene hydration catalyst solution is beneficial to promotion from the point of view of by the internal solution stored
The durability of equipment and safety.
Specifically, acetylene hydration catalyst solution (101) includes [Ru of concentration 0.5mM-2.0mMⅢ(EDTA-H)Cl]
2H2O catalyst, concentration can be 0.5mM, 0.6mM, 0.7mM, 0.8mM, 0.9mM, 1.0mM, 1.1mM, 1.2mM, 1.3mM,
1.4mM, 1.5mM, 1.6mM, 1.7mM, 1.8mM, 1.9mM or 2.0mM.In these cases, the acetylene in gas (G) to be analyzed
The efficiency for being converted to acetaldehyde is excellent, can be reduced detection lower bound, and reduces minimum gas flow (G) to be analyzed required when detection.
In embodiment, acetylene hydration catalyst [RuⅢ(EDTA-H)Cl]2H2O solution makes wait divide to the second in gas (G)
Alkynes is converted to the reaction equation of acetaldehyde (hydration reaction) as described in chemical formula 1.
[chemical formula 1]
Be equipped in reaction zone (100) can allow acetylene hydration catalyst solution (101) be maintained at about 70 DEG C to 90 DEG C plus
Hot device (103), within the said temperature range, the efficiency that the acetylene in gas (G) to be analyzed is converted to acetaldehyde are excellent, can be promoted
The sensitivity of analytical equipment, and reduce detection lower bound.
The temperature of acetylene hydration catalyst solution (101) about between 75 DEG C to 85 DEG C, may be adjusted to 75 ± 0.1 DEG C,
76±0.1℃、77±0.1℃、78±0.1℃、79±0.1℃、80±0.1℃、81±0.1℃、82±0.1℃、83±0.1
DEG C, 84 ± 0.1 DEG C or 85 ± 0.1 DEG C.When in above-mentioned temperature range, acetylene in gas to be analyzed (G) can be lifted up and turned
It is changed to the efficiency of acetaldehyde.
Adjustable gas (G) injection acetylene hydration catalyst solution (101) to be analyzed is equipped in hydration reaction area (100)
The mass flow controller (104) of speed, the adjustable gas (G) to be analyzed of the mass flow controller (104) is with bubble shape
Formula injects the speed of acetylene hydration catalyst solution (101), and flow velocity may be about 20mL/s, 21mL/ in 20mL/s to 30mL/s
s,22mL/s,23mL/s,24mL/s,25mL/s,26mL/s,27mL/s,28mL/s,29mL/s,30mL/s.Within this range,
The efficiency that acetylene in gas (G) to be analyzed is converted to acetaldehyde is excellent, can reduce detection lower bound, and reduces needed for detection most
The amount of low gas to be analyzed (G).
Hydration reaction area (100) is internal to be divided into two spaces up and down again, equipped with the permoselective membrane for only allowing gas to pass through
(105).The permoselective membrane (105) only has gas that can pass through, and acetylene hydration catalyst solution (101) can not pass through.?
Under above situation, gas to be analyzed passes through the acetaldehyde that acetylene hydration catalyst solution (101) generate afterwards, can pass through selectively penetrating
Film (105) is collected.
It is additionally provided with the piston (106) connecting with permoselective membrane (105) in hydration reaction area (100), with control selections
Property permeable membrane (105) axial movement, in these cases, it is easier to adjust the gas to be analyzed (G) containing acetaldehyde pass through selection
Property permeable membrane (105) pressure for being generated when volume changes afterwards, be also easier to the gas flow that control flows into conductivity measurement area.
There are one that can be discharged acetylene hydration catalyst solution (101) in hydration reaction area (100), container inner pressure is adjusted
Outlet (107).Such design can be more easily adjusted interior when being analysed to gas (G) injection hydration reaction area (100)
Pressure caused by portion.
Pressure in hydration reaction area (100) should in about 0.5atm to 1.5atm, such as 0.5atm, 0.6atm, 0.7atm,
0.8atm, 0.9atm, 1.0atm, 1.1atm, 1.2atm, 1.3atm, 1.4atm or 1.5atm.Within the above range, to be analyzed
The efficiency that acetylene in gas (G) is converted to acetaldehyde is excellent, and the speed of gas to be analyzed (G) inflow can be more easily adjusted, and
The portability of lifting means.
In summary content is equipped with the container of storage acetylene hydration catalyst solution, container inside hydration reaction area (100)
The interior heater (103) for being equipped with adjustable acetylene hydration catalyst solution temperature, is adjusted injection acetylene hydration catalyst solution
In gas flow to be analyzed mass flow controller (104), the permoselective membrane for only allowing gas to pass through (105), and discharge
Acetylene hydration catalyst solution adjusts the outlet (106) of internal pressure.Therefore, it is equipped with the acetylene gas of hydration reaction area (100)
The efficiency that the acetylene that body analytical equipment is analysed in gas (G) is converted to acetaldehyde is excellent, adjustable gas (G) stream to be analyzed
The speed entered can reduce detection lower bound, and reduce the required minimum gas flow (G) to be analyzed of detection.
Conductivity measurement area (200) is connected with hydration reaction area (100), is the container reacted.Gas (G) to be analyzed
Acetaldehyde is being generated afterwards by hydration reaction area (100), can then flowed into wherein.
There is surface to be coated with the ZnO nano crystal of amine-containing gas silane compound on the inner wall in conductivity measurement area (200)
(202), the surface of ZnO nano crystal reacts with the acetaldehyde for flowing into conductivity measurement area (200), and conductivity is made to generate change
Change.
In conductivity measurement area (200), can measure surface be coated with the ZnO nano crystal of amine-containing gas silane compound with
The conductivity variation generated when acetaldehyde reacts.
The conductivity variable quantity in conductivity measurement area (200) is from amine gas (amine) and imines (imine) because acetaldehyde is sent out
Raw reversible reaction.
The silane compound of above-mentioned amine-containing gas is N- (2- amine ethyl) aminopropyl triethoxysilane (N- (2-
aminoethyl)aminopropyltrimethoxylsilane).In these cases, ZnO nano crystal and amine-containing gas silane
The binding force of compound and conductivity reception and registration degree are excellent, can promote the accuracy of sensitivity and the detection of analytical equipment.
In embodiment, amine-containing gas silane compound is N- (2- amine ethyl) aminopropyl triethoxysilane (N- (2-
aminoethyl)aminopropyltrimethoxylsilane).The amine gas (amine) and imines generated after being reacted with acetaldehyde
(imine) reversible reaction efficiency is excellent, can increase the variation of conductivity.The reaction occurred in these cases, such as chemistry
Shown in formula 2.
[chemical formula 2]
It is equipped in conductivity measurement area (200) and can trigger the light source (203) that amine gas is reacted with acetaldehyde, amine gas and second is adjusted
The reaction initial time and reaction speed of aldehyde.
There are also conductivity test instrument (204) in conductivity measurement area (200), can be amine-containing in gas to be analyzed and surface cladding
After the ZnO nano crystal contact of gas silane compound, the variable quantity of conductivity is measured.
In conductivity measurement area (200), quantitative analysis can be shown in by changing calculated acetylene content via conductivity
Area (300).Therefore, display device (301) are equipped in quantitative analysis area (300), can show result value, and display device
(301) type is not particularly limited.
In quantitative analysis area (300), via following formula 1, the acetylene content in gas to be analyzed (G) can be calculated.
[formula 1]
Ac (ppm)={ Ec2/ (Mw2/F) }-{ Ec1/ (Mw1/F) }
In formula 1, Ac is the acetylene gas scale of construction (unit: ppm) for including in gas to be analyzed, and Ec1 is starts to analyze preceding institute
The conductivity (unit: mho) measured, Mw1 are the molecular weight (unit: g/mol) of imine group (imine group), and Ec2 is to open
Begin conductivity (unit: mho) measured after analyzing, and Mw2 is the molecular weight (unit: g/ of amine groups (amine group)
Mol), F is then Faraday constant (Faraday constant) (unit: C/mol).
In formula 1, " before starting analysis " refers to the state that gas to be analyzed (G) is flowed into before hydration reaction area (100),
" after starting analysis " refers to the state that gas to be analyzed (G) is flowed into after hydration reaction area (100), or can refer to survey in conductivity
Amine gas is with acetaldehyde because light source generates the state after reacting in amount area (200).
In embodiment, the silane compound of amine-containing gas is N- (2- amine ethyl) aminopropyl triethoxysilane (N- (2-
Aminoethyl) aminopropyltrimethoxylsilane), Faraday constant F is 96485 (C/mol), Mw1 imido grpup
The molecular weight of group (imine group) is 265.29 (g/mol), and the molecular weight of Mw2 amine groups is 237.29 (g/mol).Via
Following formula 1A can calculate the inner acetylene content of gas to be analyzed (G) in quantitative analysis area (300).
[formula 1A]
Ac (ppm)=(Ec2/0.002459)-(Ec1/0.002750)
In formula 1A, Ac is the acetylene gas scale of construction (unit: ppm) for including in gas to be analyzed, and Ec1 is starts to analyze preceding institute
The conductivity (unit: mho) measured, Ec2 are conductivity (unit: mho) measured after starting analysis.In addition, in formula 1A,
The value of 0.002459 (mg/mC) be by 237.29/96485=0.002459 calculate gained, the value of 0.002750 (mg/mC) be by
265.29/96485=0.002750 calculates gained.
It is used for the acetylene analytical equipment of buried cable in the application, can detect that the acetylene content in gas to be analyzed (G),
Lower bound is detected in 10ppm or less, it may be possible to 10ppm, 5ppm, 1ppm or 0.1ppm, therefore can be directly by equipment belt to scene, i.e.,
Make only minimum gas, can also be detected.
The acetylene analytical equipment of buried cable in the application, analyzable minimum gas flow about in 5mL or more, such as
5mL, 10mL, 15mL, 20mL, 25mL, 30mL, 35mL, 40mL, 45mL, 50mL or more.It therefore can be directly by equipment belt to now
, even if being only collected into micro gas, it also can detect that exception.
Another embodiment in the application, be make gas to be analyzed contacted with acetylene hydration catalyst generate acetaldehyde, and
Calculate the analysis method of acetylene content in the gas.And this method must be held by acetylene gas analytical equipment above-mentioned
Row.
The analysis method (a) of acetylene gas is that gas to be analyzed is allowed to contact with acetylene hydration catalyst solution, collects and generates
Acetaldehyde, the ZnO nano crystal for (b) making acetaldehyde coat amine-containing gas silane compound with surface reacted, institute after measurement reaction
The conductivity variable quantity of generation (c) and via conductivity variable quantity calculates the acetylene content in gas to be analyzed.
Specifically, aforementioned hydration reaction can carry out at about 70 DEG C to 90 DEG C.Within the said temperature range, gas to be analyzed
It is excellent that acetylene in body (G) converts the efficiency to acetaldehyde, and can promote the sensitivity of analytical equipment, reduces the lower bound of detection.
The temperature of hydration reaction is about at 75 DEG C to 85 DEG C, for example, being adjustable to 75 ± 0.1 DEG C, 76 ± 0.1 DEG C, 77 ± 0.1
DEG C, 78 ± 0.1 DEG C, 79 ± 0.1 DEG C, 80 ± 0.1 DEG C, 81 ± 0.1 DEG C, 82 ± 0.1 DEG C, 83 ± 0.1 DEG C, 84 ± 0.1 DEG C or 85
±0.1℃.Within the said temperature range, acetylene in gas to be analyzed (G) can be more promoted to convert to the efficiency of acetaldehyde.
[Ru containing 0.5mM to 2.0mM in acetylene hydration catalyst solutionⅢ(EDTA-H)Cl]2H2O catalyst.?
Under above situation, the efficiency that the acetylene in gas (G) to be analyzed is converted to acetaldehyde is excellent, can reduce detection lower bound, and reduce inspection
Required minimum gas flow (G) to be analyzed when survey.
In addition, above-mentioned acetylene gas analysis method is the ZnO nano crystalline substance for coating amine-containing gas silane compound using surface
Body is reacted with acetaldehyde, and measures the variable quantity of conductivity.
The reaction is the reversible reaction for generating amine gas (amine) and imines (imine) using acetaldehyde, measures conductivity
Variable quantity.
In the above method, the silane compound of amine-containing gas is N- (2- amine ethyl) aminopropyl triethoxysilane (N- (2-
aminoethyl)aminopropyltrimethoxylsilane).In these cases, the silicon of ZnO nano crystal and amine-containing gas
The binding force of hydride compounds and conductivity reception and registration degree are excellent, can promote the sensitivity and detection precision of analytical equipment.
In addition, amine gas with reacting for acetaldehyde is triggered via light source.
The acetylene content in gas to be analyzed can be calculated via following formulas 1.
[formula 1]
Ac (ppm)={ Ec2/ (Mw2/F) }-{ Ec1/ (Mw1/F) }
In formula 1, Ac is the acetylene gas scale of construction (unit: ppm) for including in gas to be analyzed, and Ec1 starts preceding institute for analysis
The conductivity (unit: mho) measured, Mw1 are the molecular weight (unit: g/mol) of imine group (imine group), and Ec2 is point
Analysis starts rear measured conductivity (unit: mho), and Mw2 is the molecular weight (unit: g/ of amine groups (amine group)
Mol), F is then Faraday constant (Faraday constant) (unit: C/mol).
Buried cable acetylene analytical equipment in the application can check the acetylene content in gas to be analyzed (G), detection
Lower bound is 10ppm or hereinafter, may be for 10ppm, 5ppm, 1ppm or 0.1ppm, therefore can directly be carried equipment to scene, i.e.,
Make only micro gas, also can detecte out.
Buried cable acetylene analytical equipment in the application can analyze minimum about 5mL of gas or more, such as 5mL,
10mL, 15mL, 20mL, 25mL, 30mL, 35mL, 40mL, 45mL, 50mL or more.Therefore equipment can be carried to scene, i.e.,
Make only to be collected into micro gas, can also detect exception.
Embodiment
In following examples, the configuration and operating method of the application will be described in detail, however, following the description is
In order to help to understand the application, and scope of the present application is not limited to following embodiment.In addition, the content not described in this specification
Belong to all presumable content of those skilled in the art, and the description is omitted.
Embodiment 1
There is the double-walled container that can store acetylene hydration catalyst solution in the hydration reaction area of equipment, heater will be to
The mass flow controller of the gas injection container of analysis；Collect the permoselective membrane of air；And control acetylene hydration
The discharge rate of catalyst aqueous solution adjusts the outlet of container internal pressure.
Gas to be analyzed containing acetaldehyde can flow into coupled conductivity measurement area behind hydration reaction area.It is conductive
The inner wall of rate measurement zone is equipped with surface and is coated with the ZnO nano crystal of amine-containing gas silane compound, by light source can trigger its with
The reaction of acetaldehyde.
In addition, quantitative analysis area is connect with conductivity measurement area, calculated in gas to be analyzed via conductivity variable quantity
The result of acetylene content can be shown in herein.
50mL distilled water is filled in hydration reaction area, and excludes inner air using piston, and concentration 0.5mM is then added
[RuⅢ(EDTA-H)Cl]2H2The temperature of catalyst solution is controlled at 80 ± 0.1 DEG C with heater, is made by O catalyst solution
Pressure is 1atm, and the speed that gas to be analyzed flows into is 20mL/ minutes.
Using the acetylene gas analytical equipment of embodiment 1, whether confirmation can detecte in the simulated environment of 1ppm acetylene
To acetylene.
Embodiment 2 to 12
In addition to the concentration of acetylene in simulated environment, the concentration of catalyst aqueous solution, reaction pressure and reaction temperature such as the following table 1
Except be shown with part changes, acetylene detection is carried out using equipment same as Example 1.
After detection, the catalyst aqueous solution in embodiment 2 to 12 is analyzed to confirm hydration rate, as a result as shown in table 2 below.
[table 1]
[table 2]
| Hydration rate (Mhr-1) | |
| Embodiment 2 | 0.78×103 |
| Embodiment 3 | 1.51×103 |
| Embodiment 4 | 2.07×103 |
| Embodiment 5 | 2.42×103 |
| Embodiment 6 | 0.34×103 |
| Embodiment 7 | 0.72×103 |
| Embodiment 8 | 1.22×103 |
| Embodiment 9 | 1.54×103 |
| Embodiment 10 | 0.77×103 |
| Embodiment 11 | 1.23×103 |
| Embodiment 12 | 1.52×103 |
Comparative example 1
The acetylene less than 1ppm is taken to be placed in sampler bag as sample, to promote the gas installed in laboratory in simulated environment
The detection lower bound of phase chromatography (GC) system, adjustment gas flow and quantitative loop (sample loop), installation acquire sample, then will
The sample that acquisition comes injects gas chromatograph.Mass flow controller and o controller are set, to adjust the flow velocity of sample.Sample
This can inject a period of time (about 30 seconds) with regard to being cut off automatically by GC operation sequence, reduce the consumption of sample as far as possible.Matter
Measure the sample that flow regulator can be injected according to preset flow velocity (50cc/min) in sampler bag.
Comparative example 2
Minimum gas flow needed for confirming the detection lower bound and analysis of diffusion type detector (NEW COSMOS, XP-3160),
And confirm the instrument in the simulated environment of the acetylene less than 1ppm a possibility that acetylene detection.
Comparative example 3
Minimum gas needed for confirming the detection lower bound and analysis of suction-type detector (Honeywell, MiniMaxX4)
Amount, and confirm the instrument in the simulated environment of the acetylene less than 1ppm a possibility that acetylene detection.
[table 3]
Appended drawing reference:
100 hydration reaction areas
200 conductivity measurement areas
300 quantitative analysis areas
Claims (18)
1. it is a kind of detect buried cable acetylene gas analytical equipment, characterized by comprising:
It is hydrated into the hydration reaction area of acetaldehyde, catalyst solution containing acetylene hydration passes through gas to be analyzed；
Hydration reaction area is connected, the acetaldehyde flowed into is made and the ZnO nano that inner wall surface coats amine-containing gas silane compound is set
Crystal reaction,
Conductivity measurement area, measurement conductivity variation；And
Quantitative analysis area can calculate gas acetylene content to be analyzed via conductivity variable quantity.
2. acetylene gas analytical equipment according to claim 1, which is characterized in that having in hydration reaction area can be by acetylene
Hydration catalyst solution temperature controls the heater between 70 DEG C to 90 DEG C.
3. acetylene gas analytical equipment according to claim 1, which is characterized in that there is adjustable stream in hydration reaction area
Enter the mass flow controller of the gas flow to be analyzed of acetylene hydration catalyst solution.
4. acetylene gas analytical equipment according to claim 1, which is characterized in that about contain in acetylene hydration catalyst solution
Catalyst [the Ru of concentration 0.5mM to 2.0mMⅢ(EDTA-H)Cl]2H2O。
5. acetylene gas analytical equipment according to claim 1, which is characterized in that second can be stored by being equipped in hydration reaction area
The container of alkynes hydration catalyst solution has the heater of adjustable acetylene hydration catalyst solution temperature in container；It is adjustable
Gas to be analyzed flows into the mass flow controller of acetylene hydration catalyst solution flow；Collect the selectively penetrating of gas
Net；And acetylene hydration catalyst solution can be discharged, to maintain the outlet of container inner pressure.
6. acetylene gas analytical equipment according to claim 5, which is characterized in that permoselective membrane is connected with piston,
With the axial movement of control selections permeable membrane (105).
7. acetylene gas analytical equipment according to claim 1, which is characterized in that the silane compound of amine-containing gas is N-
(2- amine ethyl) aminopropyl triethoxysilane.
8. acetylene gas analytical equipment according to claim 1, which is characterized in that touched using light source in conductivity measurement area
Hair amine gas is reacted with acetaldehyde.
9. acetylene gas analytical equipment according to claim 1, which is characterized in that coat amine-containing gas silanization using surface
The ZnO nano crystal for closing object is reacted with acetaldehyde generation, changes conductivity, and measure.
10. a kind of acetylene gas analysis method, which is characterized in that contact gas to be analyzed with acetylene hydration catalyst, then pass through
The acetaldehyde being generated by it calculates the acetylene content in gas to be analyzed.
11. acetylene gas analysis method according to claim 10, which is characterized in that
(a) it contacts gas to be analyzed with acetylene hydration catalyst solution, then collects the acetaldehyde generated after reaction,
(b) acetaldehyde being collected into is reacted with the ZnO nano crystal that surface coats amine-containing gas silane compound again, measurement is anti-
The conductivity variable quantity that should be generated afterwards, and
(c) acetylene content in gas to be analyzed is calculated via conductivity variable quantity again.
12. acetylene gas analysis method according to claim 11, which is characterized in that hydration reaction temperature is about arrived at 70 DEG C
Between 90 DEG C.
13. acetylene gas analysis method according to claim 11, which is characterized in that urged in acetylene hydration catalyst solution
Agent [RuⅢ(EDTA-H)Cl]2H2The concentration of O is about between 0.5mM to 2.0mM.
14. acetylene gas analysis method according to claim 11, which is characterized in that the silane compound of amine-containing gas is N-
(2- amine ethyl) aminopropyl triethoxysilane.
15. acetylene gas analysis method according to claim 11, which is characterized in that amine gas is reacted with acetaldehyde by light source
To trigger.
16. acetylene gas analysis method according to claim 11, which is characterized in that calculated by conductivity variable quantity
When acetylene content in gas to be analyzed, minimum detection value is 0.1ppm.
17. acetylene gas analysis method according to claim 11, which is characterized in that the minimum gas flow of gas to be analyzed
About 10mL.
18. acetylene gas analysis method according to claim 11, which is characterized in that carry out the acetylene in gas to be analyzed
When content analysis, calculated via following formula 1:
[formula 1]
Ac (ppm)={ Ec2/ (Mw2/F) }-{ Ec1/ (Mw1/F) }
In formula 1, Ac is the acetylene gas scale of construction (unit: ppm) for including in gas to be analyzed, and Ec1 is measured before analysis starts
Conductivity (unit: mho), Mw1 be imine group (imine group) molecular weight (unit: g/mol), Ec2 be analysis open
Measured conductivity (unit: mho) after beginning, Mw2 are the molecular weight (unit: g/mol) of amine groups (amine group), and F is then
For Faraday constant (Faraday constant) (unit: C/mol).
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| KR1020160145232A KR101840191B1 (en) | 2016-11-02 | 2016-11-02 | Device for acetylene gas analysis of underground transmission cables and method for acetylene gas analysis |
| PCT/KR2016/013995 WO2018084362A1 (en) | 2016-11-02 | 2016-11-30 | Underground cable acetylene gas analysis apparatus and acetylene gas analysis method |
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| KR101840191B1 (en) | 2018-03-21 |
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