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CN111077139A - A reaction chamber for chemiluminescence - Google Patents

A reaction chamber for chemiluminescence Download PDF

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Publication number
CN111077139A
CN111077139A CN201911325633.9A CN201911325633A CN111077139A CN 111077139 A CN111077139 A CN 111077139A CN 201911325633 A CN201911325633 A CN 201911325633A CN 111077139 A CN111077139 A CN 111077139A
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China
Prior art keywords
inlet
guide pipe
reaction chamber
flow guide
outlet
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CN201911325633.9A
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Chinese (zh)
Inventor
黄伟
盛伟明
杨鹏
陈小平
刘中化
王天阳
许进
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Focused Photonics Hangzhou Inc
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Focused Photonics Hangzhou Inc
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Priority to CN201911325633.9A priority Critical patent/CN111077139A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/76Chemiluminescence; Bioluminescence
    • G01N21/766Chemiluminescence; Bioluminescence of gases

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  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
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  • General Health & Medical Sciences (AREA)
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  • Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)

Abstract

本发明公开了一种用于化学发光法的反应室,包括滤光片、密封罩、集成模块、第一导流管和第二导流管,所述密封罩的上端固定有所述滤光片,下端连接有所述集成模块,所述集成模块包括加热模块、第一入口和第二入口,所述第一导流管的一端与所述第一入口相连,另一端设在所述密封罩内,所述第二导流管设置在所述第一导流管内部,所述第二导流管的一端与第二入口相连,另一端设在密封罩内。本发明的优点是:保证了标气与样气的混合均匀性,提高样气的反应程度,同时反应区域近距离的设计与高反罩的共同作用有效提高了反应信号强度,将化学反应室应用于化学发光法臭氧分析仪,其检出限可以达到0.4ppb及以下。

Figure 201911325633

The invention discloses a reaction chamber for chemiluminescence, comprising a filter, a sealing cover, an integrated module, a first guiding tube and a second guiding tube, wherein the filter is fixed on the upper end of the sealing cover The lower end is connected with the integrated module, the integrated module includes a heating module, a first inlet and a second inlet, one end of the first guide pipe is connected with the first inlet, and the other end is arranged in the seal In the cover, the second guide pipe is arranged inside the first guide pipe, one end of the second guide pipe is connected with the second inlet, and the other end is arranged in the sealing cover. The advantages of the invention are as follows: the mixing uniformity of the standard gas and the sample gas is ensured, and the reaction degree of the sample gas is improved; at the same time, the close design of the reaction area and the joint action of the high reflection cover effectively improve the strength of the reaction signal, and the chemical reaction chamber Applied to chemiluminescence ozone analyzer, its detection limit can reach 0.4ppb and below.

Figure 201911325633

Description

Reaction chamber for chemiluminescence method
Technical Field
The invention relates to the technical field of environmental monitoring, in particular to a reaction chamber for a chemiluminescence method of an ozone analyzer.
Background
The chemiluminescence method technology is a main technology of a nitrogen oxide analyzer in the field of automatic monitoring of environmental atmospheric quality, and has the advantages of good selectivity, high measurement precision and the like. The measurement principle is as follows: introducing NO and O into the reaction chamber3Gas, NO and O3Reacting to form excited NO2Molecule, and NO2Molecules not stably present, which rapidly decay to ground state NO2And emits fluorescence with a spectral range of 600-3000 nm and a central wavelength of 1200 nm. When O is present3In the case of excess, the NO can be considered to be fully reacted approximately, and the measured fluorescence signal is approximately equal to the concentration of NO, so that the nitrogen oxides in the environment can be accurately measured.
In view of the technical characteristics of the chemiluminescence method, the chemiluminescence method has good application in ozone analysis, and compared with the conventional ultraviolet photometry, the chemiluminescence method for measuring ozone can effectively avoid interference substances such as SO2 and the like, and the measurement precision is higher. Ozone measurements by chemiluminescence represent the American API T265. Different from a nitrogen oxide analyzer, the chemiluminescence ozone analyzer has higher requirements on a reaction cavity, and the chemiluminescence ozone analysis adopts NO excess to ensure O3Then O is further carried out3Measuring concentration, in order to ensure the use period of NO, the NO flow is usually relatively small and is usually 3-10 sccm, and the O of nitrogen oxide3Conventional method is 50-100 sccm, solid and chemical luminescence O3The analyzer provides higher requirements for the gas mixing uniformity and temperature and humidity control of the reaction cavity.
The reaction chamber of the existing chemiluminescence method ozone analyzer has certain defects on the accuracy and stability of the measurement result.
Disclosure of Invention
The invention aims to provide a reaction chamber of a chemiluminescence method ozone analyzer with better accuracy and stability of measurement results, so as to realize accurate measurement.
In order to solve the technical problems, the invention is realized by the following technical scheme: a reaction chamber for chemiluminescence method, including light filter, sealed cowling, collection moulding piece, first honeycomb duct and second honeycomb duct, the upper end of sealed cowling is fixed with the light filter, the lower extreme is connected with collection moulding piece, collection moulding piece includes heating module, first entry and second entry, the one end of first honeycomb duct with first entry links to each other, and the other end is established in the sealed cowling, the second honeycomb duct sets up inside the first honeycomb duct, the one end and the second entry of second honeycomb duct link to each other, and the other end is established in the sealed cowling.
Preferably, the end of the first flow guide pipe in the sealing cover is a first outlet, the first outlet is a closed port, the end of the second flow guide pipe in the sealing cover is a second outlet, the second outlet is an open port, and a third inlet for connecting the first flow guide pipe is formed in the side wall of the second flow guide pipe.
Preferably, the third inlet is perpendicular to the second draft tube.
Preferably, the time for the gas in the second guide pipe to reach the second outlet is greater than or equal to the time for the gas in the first guide pipe to reach the pipe wall opposite to the third inlet.
Preferably, the distance from the third inlet to the second outlet is:
Figure BDA0002328315640000021
wherein x1: the distance from the third inlet to the second outlet; d: a first draft tube diameter; d: the diameter of the second draft tube; q1: the flow rate of the first flow guide pipe; q2: and the flow rate of the second flow guide pipe.
Preferably, the heating module comprises a heating rod and a temperature sensor, and the heating module adopts multipoint heating and multipoint temperature detection.
Preferably, the sealing cover is a corrosion-resistant material with high reflective properties.
Compared with the prior art, the invention has the advantages that: the chemical reaction chamber is applied to a chemiluminescence method ozone analyzer, and the detection limit can reach 0.4ppb or below.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a cross-sectional view taken along line B-B of FIG. 1;
FIG. 3 is a cross-sectional view taken along A-A of FIG. 1;
FIG. 4 is an enlarged partial view of a third inlet, a first outlet and a second outlet of the present invention;
fig. 5 is a schematic view of the gas flow at the third inlet, the first outlet and the second outlet of the present invention.
The device comprises a filter 1, a sealing ring 2, a sealing cover 3, an integrated module 4, a second flow guide pipe 5, a first flow guide pipe 6, a heating rod 7, a temperature sensor 8, a second inlet 9, a first inlet 10 and a third inlet 11.
Detailed Description
Embodiments of the invention are further described below with reference to the accompanying drawings:
as shown in fig. 1 to 4, a reaction chamber for a chemiluminescence method comprises an optical filter 1, a sealing cover 3, an integrated module 4, a first flow guide pipe 6 and a second flow guide pipe 5, wherein the optical filter is fixed at the upper end of the sealing cover, the integrated module is connected at the lower end of the sealing cover, the integrated module comprises a heating module, a first inlet 10 and a second inlet 9, one end of the first flow guide pipe is connected with the first inlet, the other end of the first flow guide pipe is arranged in the sealing cover, the second flow guide pipe is arranged in the first flow guide pipe, one end of the second flow guide pipe is connected with the second inlet, and the other end of the second flow guide pipe is arranged in the sealing cover. The one end that first honeycomb duct is in the sealed cowling is first export, first export is for closing the mouth, the one end that the second honeycomb duct is in the sealed cowling is the second export, the second export is the opening, it has third entry 11 to be used for connecting first honeycomb duct to open on the lateral wall of second honeycomb duct. The third inlet is perpendicular to the second draft tube. The heating module comprises a heating rod 7 and a temperature sensor 8, multipoint heating and multipoint temperature measurement are adopted, and PID control can be carried out. The sealing cover is made of stainless steel and is polished, and the roughness of the inner wall surface is not more than 0.2 microns. The integrated module, the sealing cover and the optical filter are sealed by a sealing ring 3 such as a fluororubber ring.
The second entry is used for communicateing the appearance gas, and first entry is used for communicateing the mark gas, the time more than or equal to that the appearance gas in the second nozzle reaches the second export the time that the mark gas in the first nozzle arrived the opposite pipe wall of third entry: ,
namely, it is
Figure BDA0002328315640000041
Wherein x1Is the distance from the third inlet to the second outlet, D is the diameter of the second flow-guiding pipe, u1Is the speed of the marker gas in the Z-axis direction in the second guide pipe u2The velocity of the sample gas in the x-axis direction in the second guide pipe.
It is known that
Figure BDA0002328315640000042
Wherein S1Is the cross-sectional area of the first flow-guiding pipe, S2Is the cross-sectional area, Q, of the second flow-guide tube1Is the flow rate of the first flow guide pipe, Q2The flow rate of the second flow guide pipe.
Converted to
Figure BDA0002328315640000043
D is the diameter of the first draft tube.
As shown in FIG. 5, the lower edge 11 of the standard gas and the upper edge 12 of the standard gas are obtained through a large number of experiments, D is greater than or equal to 0.25mm and less than or equal to 1.5mm, D is greater than or equal to 5mm and less than or equal to 15mm, x1 is greater than or equal to 20mm and x2 is greater than or equal to 1mm and less than or equal to 10mm, and in one embodiment, the reaction chamber has a better effect when D is 0.5mm, D is 10mm, x1 is 5mm and x2 is 5 mm.
When the device is used, the flow of a sample to be measured is 500sccm, the sample enters the second flow guide pipe from the second inlet, the flow of a reaction standard gas is 8sccm, the sample enters the first flow guide pipe from the first inlet and then enters the second flow guide pipe from the third inlet, the sample gas and the standard gas are negative pressure when the end part of the second flow guide pipe is mixed and enters the reaction cavity of the reaction cavity, and the pressure is about 2 psi. Calculated from the Reynolds coefficient Re ═ ρ μ d/u, ρ is the density of the gas, μ is the viscosity coefficient of the gas, u is the incident velocity of the gas, and d is the incident aperture diameter of the gas
Obtaining Reynolds coefficient Rep of the sample gas 0.1488 0.106 0.01/1.72e-5 9.17;
the reynolds coefficient of the standard gas is 0.1437 0.68 0.0005/1.72e-5 2.84;
the Reynolds coefficient of the two is less than 2000, so the gas mixture belongs to laminar diffusion, and the jet curve of the graph of FIG. 5 can be obtained:
when the time for the sample gas in the second guide pipe to reach the second outlet is shorter than the time for the standard gas in the first guide pipe to reach the pipe wall opposite to the third inlet, the upper edge 13 of the incident standard gas cannot be crossed with the upper pipe wall of the second guide pipe, namely, the sample gas and the standard gas enter the reaction cavity layer by layer under the condition that the sample gas and the standard gas are not completely mixed.
When the time that the sample gas in the second guide pipe reaches the pipe orifice is more than or equal to the time that the standard gas in the first guide pipe reaches the pipe wall opposite to the third inlet, the upper edge 13 of the incident standard gas can be crossed with the upper pipe wall of the second guide pipe, so that the sample gas and the standard gas are fully mixed and then enter the reaction cavity.
Meanwhile, considering the timeliness of the chemical reaction luminescence of NO/O3 and the quenching phenomenon of light in the reaction cavity, in order to increase the number of detected photons as much as possible and improve the signal intensity of the detector, the shorter the distance between the reaction starting point of the sample gas and the standard gas and the detector is, the better, and a large number of experiments show that the signal intensity detected by the detector can meet the requirements of instruments under the condition that X1+ X2 is not more than 30 mm.
The roughness of the inner wall of the high-reflection sealing cover is 0.2 micron, two-point heating and two-point temperature measurement are adopted, the temperature is controlled at 48 ℃ through PID control, and the heating temperature fluctuation is less than 0.5 ℃. Ozone analysis using chemiluminescence method, the detection limit was less than 0.4 ppb.
The above description is only an embodiment of the present invention, but the technical features of the present invention are not limited thereto, and any changes or modifications within the technical field of the present invention by those skilled in the art are covered by the claims of the present invention.

Claims (7)

1. The utility model provides a reaction chamber for chemiluminescence method, its characterized in that, includes light filter, sealed cowling, integrated module, first honeycomb duct and second honeycomb duct, the upper end of sealed cowling is fixed with the light filter, the lower extreme is connected with integrated module, integrated module includes heating module, first entry and second entry, the one end of first honeycomb duct with first entry links to each other, and the other end is established in the sealed cowling, the second honeycomb duct sets up inside the first honeycomb duct, the one end and the second entry of second honeycomb duct link to each other, and the other end is established in the sealed cowling.
2. The reaction chamber of claim 1, wherein the first flow guide tube has a first outlet at an end thereof in the sealed housing, the first outlet is closed, the second flow guide tube has a second outlet at an end thereof in the sealed housing, the second outlet is open, and a third inlet is formed at a sidewall of the second flow guide tube for connecting the first flow guide tube.
3. The reaction chamber of claim 2, wherein the third inlet is perpendicular to the second flow conduit.
4. A reaction chamber for use in a chemiluminescent process according to claim 3 wherein the time for the gas in the second flow conduit to reach the second outlet is greater than or equal to the time for the gas in the first flow conduit to reach the wall of the tube opposite the third inlet.
5. A reaction chamber for use in a chemiluminescent process according to claim 3 wherein the distance from the third inlet to the second outlet is:
Figure FDA0002328315630000011
wherein
x1: the distance from the third inlet to the second outlet,
d: the diameter of the first draft tube is smaller than that of the second draft tube,
d: the diameter of the second flow guide pipe is smaller than that of the first flow guide pipe,
Q1: the flow rate of the first flow guide pipe,
Q2: and the flow rate of the second flow guide pipe.
6. The reaction chamber of claim 1, wherein the heating module comprises a heating rod and a temperature sensor, and the heating module uses multi-point heating and multi-point temperature detection.
7. The reaction chamber of claim 1, wherein the sealing cap is a corrosion resistant material with high reflective properties.
CN201911325633.9A 2019-12-20 2019-12-20 A reaction chamber for chemiluminescence Pending CN111077139A (en)

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3710107A (en) * 1971-01-25 1973-01-09 Radiation And Environmental Ma Atmospheric monitor by means of chemiluminescent reaction
JPS6446745A (en) * 1986-12-09 1989-02-21 Canon Kk Recording medium
US5271894A (en) * 1992-02-27 1993-12-21 Shimadzu Corporation Chemiluminescent analyzer
JP2003232724A (en) * 2002-02-07 2003-08-22 Dkk Toa Corp Analysis unit
WO2009035008A1 (en) * 2007-09-13 2009-03-19 Okayama Prefecture Industrial Promotion Foundation Method of measuring chemiluminescence and chemiluminescence measuring apparatus
CN203981592U (en) * 2014-07-04 2014-12-03 中节能六合天融环保科技有限公司 A reaction device for measuring the concentration of nitrogen oxides by chemiluminescence
CN109310979A (en) * 2016-04-07 2019-02-05 全球分析仪系统有限公司 Photolysis converter
CN212207116U (en) * 2019-12-20 2020-12-22 聚光科技(杭州)股份有限公司 Reaction chamber for chemiluminescence method

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3710107A (en) * 1971-01-25 1973-01-09 Radiation And Environmental Ma Atmospheric monitor by means of chemiluminescent reaction
JPS6446745A (en) * 1986-12-09 1989-02-21 Canon Kk Recording medium
US5271894A (en) * 1992-02-27 1993-12-21 Shimadzu Corporation Chemiluminescent analyzer
JP2003232724A (en) * 2002-02-07 2003-08-22 Dkk Toa Corp Analysis unit
WO2009035008A1 (en) * 2007-09-13 2009-03-19 Okayama Prefecture Industrial Promotion Foundation Method of measuring chemiluminescence and chemiluminescence measuring apparatus
CN203981592U (en) * 2014-07-04 2014-12-03 中节能六合天融环保科技有限公司 A reaction device for measuring the concentration of nitrogen oxides by chemiluminescence
CN109310979A (en) * 2016-04-07 2019-02-05 全球分析仪系统有限公司 Photolysis converter
CN212207116U (en) * 2019-12-20 2020-12-22 聚光科技(杭州)股份有限公司 Reaction chamber for chemiluminescence method

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Application publication date: 20200428