Pulse type flame photometric detection device and method

By adopting a pulsed flame photometric detection device in the FPD detector, using the design of interlaced ignition chamber and combustion chamber, the problems of high noise and poor sensitivity in the existing FPD detector are solved, and higher sensitivity and selectivity are achieved.

CN119534429AActive Publication Date: 2025-02-28CHENGDU KAISHENGJIE TECH CO LTD

Patent Information

Application Number
CN202411511197.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-10-28
Publication Date
2025-02-28
Estimated Expiration
2044-10-28

AI Technical Summary

Technical Problem

Continuous flame combustion is used in existing FPD detectors, resulting in high background noise, poor sensitivity and low selectivity.

Method used

The pulse flame photometric detection device is adopted to achieve the effect of the pulse flame by staggering the ignition chamber and the combustion chamber. The ignition chamber is ignited and is prolonged to the combustion chamber, producing flames and emitting characteristic photons, collecting and filtering noise photons through mirrors and light-transmitting components, improving the sensitivity and selectivity of the detector.

Benefits of technology

Effectively reduce noise photons, improve the sensitivity and selectivity of the detector, and enhance the ability to analyze the characteristics of the substance to be tested.

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Abstract

The invention belongs to the technical field of flame detection, and particularly discloses a pulse type flame photometric detection device and method.The pulse type flame photometric detection device comprises a detector body, a combustion chamber, an ignition chamber, a combustion chamber air inlet pipe, an ignition chamber air inlet pipe, a light transmission assembly and a signal processing assembly, and an igniter is installed on the ignition chamber; a circulation cavity is formed in the detector, the combustion chamber is installed in the circulation cavity, the ignition chamber is located above the combustion chamber, and the ignition chamber is communicated with the combustion chamber; the ignition chamber air inlet pipe is communicated with the ignition chamber, the combustion chamber air inlet pipe is communicated with the combustion chamber, and the combustion chamber is further communicated with a sample inlet pipe for introducing a measured substance; one end of the light transmission assembly is located in the circulation cavity and located on one side of the combustion chamber, a reflecting mirror is arranged on the right opposite face of the light transmission assembly, the reflecting mirror and the light transmission assembly are located on the two sides of the combustion chamber, the reflecting mirror is installed on the detector body, and the signal processing assembly is used for collecting and receiving photons transmitted in the light transmission assembly. Noise photons can be reduced, and sensitivity can be improved.
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Description

Technical Field

[0001] The present invention relates to the technical field of flame detection, and in particular to a pulsed flame photometric detection device and method. Background Art

[0002] Gas chromatography is used to detect specific elements (and their compounds) contained in samples. It belongs to qualitative analysis and is generally used in combination with various detectors. In the prior art, FPD detectors, namely flame photometric detectors, are often used for detection. FPD detectors are highly selective and sensitive detectors for phosphorus-containing and sulfur-containing compounds. When the detected object is burned in a hydrogen-rich flame, phosphorus-containing organic compounds mainly emit characteristic light with a wavelength of 526nm in the form of HPO fragments, while sulfur-containing compounds emit characteristic light with a wavelength of S 2 The molecules emit characteristic light with a wavelength of 394nm. The emitted characteristic light passes through the light-passing component and then enters the photomultiplier tube. The photomultiplier tube then converts the optical signal into an electrical signal, which is amplified and recorded by micro-current for easy analysis and research.

[0003] The FPD detector in the prior art adopts continuous flame combustion, which easily generates background noise, resulting in the collection of some unnecessary interfering photons in the characteristic light entering the photomultiplier tube; and the FPD detector in the prior art has poor sensitivity and low selectivity. Summary of the invention

[0004] The invention provides a pulse flame photometric detection device and method, aiming at reducing noise photons and improving sensitivity.

[0005] The present invention is implemented by the following technical scheme: a pulse flame photometric detection device, comprising a detector body, a combustion chamber, an ignition chamber, a combustion chamber air intake pipe, an ignition chamber air intake pipe, a light-transmitting component and a signal processing component, wherein an igniter is installed on the ignition chamber;

[0006] A flow cavity is provided in the detector, the combustion chamber is installed in the flow cavity, the ignition chamber is located above the combustion chamber, and the ignition chamber and the combustion chamber are communicated with each other;

[0007] The ignition chamber air inlet pipe is connected to the ignition chamber, the combustion chamber air inlet pipe is connected to the combustion chamber, and the combustion chamber is also connected to a sample injection tube for introducing the substance to be tested;

[0008] One end of the light-passing component is located in the flow cavity and on one side of the combustion chamber. A reflector is provided directly opposite the light-passing component. The reflector and the light-passing component are located on both sides of the combustion chamber, and the reflector is installed on the detector body. The signal processing component is used to collect and receive photons transmitted in the light-passing component.

[0009] The present invention provides a pulsed flame photometric detection device, which can generate a flame in the combustion chamber by igniting the ignition chamber and then extending the flame into the combustion chamber, thereby emitting photons that propagate through the light-transmitting component and are then collected and received by the signal processing component, thereby facilitating the analysis of the characteristics of the substance being tested.

[0010] In this scheme, when the gas in the combustion chamber and the ignition chamber is used up, the flame goes out, thus achieving the effect of a pulsed flame. This makes it easy to discharge noise photons according to the different wavelengths and emission times of different photons, and obtain the required characteristic photons, thereby improving the sensitivity and selectivity of the detector.

[0011] The reflector in this solution can reflect photons, and can collect and reflect as many photons of various types on the side of the combustion chamber as possible to the light-passing component, so that the photons propagate along the light-passing component, reducing the loss of photons.

[0012] Furthermore, an air bleed channel is provided in the detector body, and the air bleed channel is located between the combustion chamber and the ignition chamber. Interconnected air holes are provided between the top wall of the flow cavity and the air bleed channel, and the ignition chamber air inlet pipe is connected to the flow cavity.

[0013] The air inlet passage can serve as an intermediate bridge connecting the combustion chamber and the ignition chamber, and can guide the gas filled into the flow cavity to the ignition chamber through the air inlet passage and the air hole.

[0014] Furthermore, the bottom of the circulation cavity is connected to an air inlet nozzle, the top of the air inlet nozzle is connected to a lower support block, the top of the circulation cavity is connected to an upper support block, the bottom of the upper support block and the top of the lower support block are both provided with mutually facing slots, the two ends of the combustion chamber are respectively stuck in the slots of the upper support block and the lower support block, and one end of the sample injection tube passes through the air inlet nozzle and the lower support block in sequence to communicate with the combustion chamber;

[0015] A center hole is provided in the center of the upper support block, and the center hole is communicated with the air inlet channel and the combustion chamber. An annular groove is provided at the top of the upper support block, and a plurality of air holes are provided at the bottom of the annular groove along its circumference, and the air holes are communicated with the flow cavity and the air inlet channel.

[0016] In this solution, the air inlet nozzle is connected to the bottom of the circulation chamber, which can not only seal the circulation chamber, but also facilitate the installation of the lower support block. In this solution, the two ends of the combustion chamber are respectively clamped in the grooves of the upper support block and the lower support block, thereby realizing the installation and fixation of the combustion chamber. This assembly method is simple.

[0017] In addition, in the present scheme, the center hole on the upper support block and the air duct provided on the detector body can connect the combustion chamber and the ignition chamber, so as to facilitate ignition of the gas in the combustion chamber to generate a flame. At the same time, the annular groove provided on the upper support block and the setting of multiple air holes can guide the gas entering the combustion chamber into the ignition chamber, so as to facilitate ignition. Compared with the method of directly providing multiple air holes on the upper support block, in the present scheme, an annular groove is provided on the upper support block, and the top of the air hole is located in the annular groove. In such a setting, when the flame generated in the ignition chamber extends downward, the flame can be extinguished when it contacts the annular groove, avoiding burning downward through the air hole. In this way, it can be ensured that the ignition chamber will only ignite the mixed gas in the gas chamber through the center hole of the upper support block.

[0018] Furthermore, the combustion chamber and the ignition chamber are arranged alternately, and the air induction channel is perpendicular to the ignition chamber and the combustion chamber and is interconnected.

[0019] In this scheme, the combustion chamber and the ignition chamber are staggered so that the gases filled into the ignition chamber and the combustion chamber do not interfere with each other. If the two are arranged vertically opposite each other, it is easy to make the design of the gas path leading to the ignition chamber and the combustion chamber more complicated. In this scheme, the two can be connected only through the air duct, which is convenient for ignition.

[0020] Furthermore, the volume of the combustion chamber is 35-39 μl.

[0021] The combustion chamber of this solution has a small volume and low gas consumption, and the small volume of the combustion chamber can increase the equivalent concentration of the measured substance.

[0022] Further, the signal processing component includes a multiplier tube sleeve and a photomultiplier tube, and the photomultiplier tube is located in the multiplier tube sleeve;

[0023] The light-transmitting component includes a support tube and a light guide rod. The light guide rod is located inside the support tube. Both ends of the support tube are open ends. The two ends of the support tube are respectively connected to the multiplier tube sleeve and the detector body. A filter is installed in the multiplier tube sleeve and between the photomultiplier tube and the light guide rod.

[0024] The signal processing component in this scheme collects photons through a photomultiplier tube and converts them into electrical signals; the light guide rod in the light transmission component in this scheme enables photons to propagate along the light guide rod, and after filtering out noise photons through a filter, they are received by the photomultiplier tube and converted into electrical signals for easy analysis and processing.

[0025] A pulse flame photometry detection method uses a pulse flame photometry detection device as described above, and fills the ignition chamber and the combustion chamber with a mixture of hydrogen and air through the ignition chamber intake pipe and the combustion chamber intake pipe respectively, and at the same time fills the combustion chamber with a substance to be tested through a sampling tube; when the mixed gas reaches the ignition chamber, the igniter starts to ignite, thereby causing combustion in the ignition chamber to generate a flame, and the flame burning in the ignition chamber extends downward to the combustion chamber until the flame is extinguished when it extends to the bottom of the combustion chamber, and from the process of extending the burning process to the end, photons are excited in the combustion chamber, and the photons are reflected by a reflector to the light-transmitting component for transmission, and are collected and received by a signal processing component.

[0026] Furthermore, the noise photons are excluded by setting the time when the signal processing component receives different photons, and the reception of the required characteristic photons is delayed.

[0027] Furthermore, gating electronics are used to exclude noise photons outside the gate window of the photomultiplier tube.

[0028] Furthermore, the ignition chamber air intake pipe fills the ignition chamber with a hydrogen-containing air mixture, and the combustion chamber air intake pipe fills the combustion chamber with a hydrogen-rich air mixture.

[0029] Compared with the prior art, the present invention has the following advantages and beneficial effects:

[0030] The present invention discloses a pulse flame photometry detection device and method, which fills hydrogen-rich mixed air into a combustion chamber through an air inlet pipe of the combustion chamber, fills a substance to be tested into the combustion chamber through an injection tube, fills a hydrogen-containing air mixture into an ignition chamber through an air inlet pipe of the ignition chamber, and ignites an igniter so that the flame in the ignition chamber ignites the mixed gas of the substance to be tested and the hydrogen-rich mixed air in the combustion chamber, thereby generating a flame in the combustion chamber; when in use, the ignition chamber and the combustion chamber can be filled with equal proportions of gas through a proportional design, so that the gases in the ignition chamber and the combustion chamber are burned out at the same time, the flames are extinguished at the same time, and then the gas is filled in again to burn again, thereby achieving the effect of flame pulse combustion.

[0031] The substance under test is ignited by a hydrogen-rich flame in the combustion chamber and produces chemiluminescence (the wavelength of chemiluminescence produced by different substances is different). The characteristic photons produced by the combustion of the substance under test are transmitted through the light-transmitting component and are collected by the signal processing component and converted into electrical signals for easy analysis.

[0032] Since various substances (CH*, C2*, OH*, S2*, P2*, etc.) in the pulsed flame have specific chemiluminescence spectra and specific chemiluminescence delay characteristics. The pulsed flame in this solution can make the light-transmitting component selectively filter according to the different emission times of different photons when transmitting characteristic photons. For example, some photons that do not need to be collected have an earlier emission time and a very short emission time, while the photon substances we need to analyze, such as S2* and P2*, have a later emission time and a longer emission time. Therefore, when the photon substances we need are emitted, the emission of the unnecessary photon substances is completed, so that the unnecessary photon substances emitted first can be filtered to reduce noise. Therefore, the pulsed flame photometric detection device using this solution can easily separate the luminescence of the required substances from the luminescence of the unnecessary substances in terms of time, thereby enhancing its selectivity.

[0033] The difference in emission lifetime of specific substances in this scheme is combined with the dynamics of the propagating flame, allowing the use of time and wavelength information to improve the selectivity of the PFPD detector (i.e., a pulsed flame photometric detection device in the present invention), reduce the observed noise, and improve the sensitivity. The propagating flame uses a lower combustible gas flow rate, which increases the relative analyte concentration. In actual use, gated electronics can also be used to suppress noise outside the specified gate window to further improve the detection rate of the pulsed flame photometric detection device. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] The drawings described herein are used to provide a further understanding of the embodiments of the present invention, constitute a part of this application, and do not constitute a limitation of the embodiments of the present invention. In the drawings: Figure 1 It is a structural schematic diagram of an embodiment of a pulsed flame photometry detection method of the present invention; Figure 2 for Figure 1 A partial enlarged view of the middle A; Figure 3 Time-resolved spectroscopy for pulsed flame emission.

[0037] Marks and corresponding parts names in the attached drawings:

[0038] Detector body 100, combustion chamber 1, flow cavity 2, ignition chamber 3, igniter 4, reflector 7, light guide rod 8, support tube 80, filter 10, photomultiplier tube 11, injection tube 14, combustion chamber air inlet pipe 15, ignition chamber air inlet pipe 16, multiplier tube sleeve 18, connecting sleeve 19, back-tightening nut 20, air inlet channel 21, connecting port 22, air inlet nozzle 23, upper support block 24, annular groove 241, air hole 242, center hole 243, lower support block 25. DETAILED DESCRIPTION

[0039] In order to make the objectives, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with embodiments and drawings. The exemplary embodiments of the present invention and their description are only used to explain the present invention and are not intended to limit the present invention.

[0040] Example 1

[0041] like Figure 1 As shown, this embodiment 1 provides a pulsed flame photometric detection device, including a detector body 100, a combustion chamber 1, an ignition chamber 3, a combustion chamber air intake pipe 15, an ignition chamber air intake pipe 16, a light transmission component and a signal processing component.

[0042] In this embodiment, a flow chamber 2 and an air inlet passage 21 are provided in the detector body 100 . The flow chamber 2 is provided at the lower part of the detector body 100 , and the air inlet passage 21 is provided at the middle part of the detector body 100 .

[0043] The combustion chamber 1 is installed in the circulation cavity 2, and the ignition chamber 3 is installed on the detector body 100 and is located above the combustion chamber 1, that is, the ignition chamber 3 is installed on the upper body, and the air inlet channel 21 is located between the combustion chamber 1 and the ignition chamber 3 and communicates with the combustion chamber 1 and the ignition chamber 3. In this embodiment, the combustion chamber 1 and the ignition chamber 3 are staggered, that is, the combustion chamber 1 and the ignition chamber 3 are not located on the same straight line, and the air inlet channel 21 is perpendicular to the ignition chamber 3 and the combustion chamber 1 and is interconnected. In this embodiment, the ignition chamber 3 is a pipeline structure, and the bottom end of the ignition chamber 3 is connected with a connecting port 22, and the connecting port 22 is perpendicular to and communicates with the air inlet channel 21, so that the ignition chamber 3 and the combustion chamber 1 are connected through the connecting port 22 and the air inlet channel 21. An igniter 4 is installed on the ignition chamber 3, and the igniter 4 is used to ignite into the ignition chamber 3 and ignite the mixed gas in the ignition chamber 3.

[0044] There are mutually connected air holes 242 between the top wall of the circulation chamber 2 and the air inlet channel 21, the ignition chamber air inlet pipe 16 is connected to the circulation chamber 2, the combustion chamber air inlet pipe 15 is connected to the combustion chamber 1, and the combustion chamber 1 is also connected to the sampling tube 14 for introducing the measured substance. Specifically:

[0045] An air inlet nozzle 23 is connected to the bottom of the circulation chamber 2. In this embodiment, the upper part of the air inlet nozzle 23 extends into the circulation chamber 2 and is threadedly connected to the inner wall of the circulation chamber 2. A sealing ring is installed between the air inlet nozzle 23 and the bottom end of the circulation chamber 2 to ensure the sealing of the circulation chamber 2. An air inlet channel connected to the gas chamber is opened inside the air inlet nozzle 23.

[0046] The top of the air inlet nozzle 23 is connected to a lower support block 25, and the top of the circulation chamber 2 is connected to an upper support block 24. In this embodiment, the lower support block 25 is threadedly connected to the upper part of the air inlet nozzle 23. A groove is provided at the top of the lower body of the detector body 100, and the groove and the circulation chamber 2 form a stepped hole shape. The upper support block 24 is installed in the groove and is located at the top of the circulation chamber 2.

[0047] The bottom of the upper support block 24 and the top of the lower support block 25 are both provided with mutually opposite grooves, and the two ends of the combustion chamber 1 are tightly clamped in the grooves of the upper support block 24 and the lower support block 25, respectively. In this way, the combustion chamber 1 is fixed in the flow cavity 2 under the restricting action of the upper support block 24 and the lower support block 25.

[0048] One end of the injection tube 14 passes through the air inlet passage of the air inlet nozzle 23 and the lower support block 25 in sequence and communicates with the combustion chamber 1. In this embodiment, a plug hole is provided at the bottom of the slot of the lower support block 25, and the inner diameter of the plug hole is larger than the outer diameter of the injection tube 14, so that after the injection tube 14 passes through the plug hole on the lower support block 25, there is a gap between the plug hole, so that the air inlet passage of the air inlet nozzle 23 can be connected with the combustion chamber through the plug hole. In this embodiment, a sealing ring is provided between the combustion chamber 1 and the slot of the lower support block 25 for sealing to prevent the gas entering from the air inlet nozzle 23 from leaking out of the combustion chamber 1.

[0049] In this embodiment, the injection tube 14 is a quartz capillary tube with a small inner diameter for introducing the substance to be measured. Thus, the injection nozzle portion of the combustion chamber 1 is directly inserted by the quartz capillary tube instead of the nozzle.

[0050] One end of the combustion chamber intake pipe 15 in the present embodiment penetrates into one side of the intake nozzle 23 and communicates with the intake passage of the intake nozzle 23, thereby communicating with the combustion chamber 1 through the intake nozzle 23, so as to facilitate the filling of gas into the combustion chamber 1. In the present embodiment, the gas filled from the combustion chamber intake pipe 15 is a hydrogen-rich air mixture, and the gas filled from the ignition chamber intake pipe 16 is a hydrogen-containing air mixture.

[0051] In this embodiment, the upper support block 24 and the lower support block 25 are both made of PEEK material. PEEK material (polyetheretherketone) has the characteristic of high temperature resistance. The combustion chamber 1 is made of quartz material. In this embodiment, the combustion chamber 1 is specifically a high-transparent quartz tube. The volume of the combustion chamber 1 is 35-39 microliters. The small volume of the combustion chamber 1 can increase the equivalent concentration of the substance being measured, thereby improving the sensitivity of the detector.

[0052] The overall structure formed by the combustion chamber 1, the upper support block 24 and the lower support block 25 are all inert material components, which can reduce the adsorption of various adsorptive gases such as sulfides and phosphides as much as possible, thereby ensuring the accuracy of detection.

[0053] Combination Figure 2As shown, a center hole 243 is provided in the center of the upper support block 24, and the center hole 243 is communicated with the air bleed channel 21 and the combustion chamber. An annular groove 241 is provided at the top of the upper support block 24, and a plurality of air holes 242 are provided at the bottom of the annular groove 241 along its circumference. The plurality of air holes 242 are evenly distributed along the circumference of the annular groove 241, and the air holes 242 are communicated with the flow cavity 2 and the air bleed channel 21.

[0054] Combination Figure 1 As shown, one end of the light-passing component is located in the flow cavity 2 and on one side of the combustion chamber 1. The signal processing component is used to collect characteristic photons transmitted in the light-passing component. A reflector 7 is provided opposite the light-passing component. The reflector 7 and the light-passing component are located on both sides of the combustion chamber 1, and the reflector 7 is installed on the detector body 100. Specifically:

[0055] like Figure 1 As shown, the signal processing component in this embodiment includes a multiplier tube sleeve 18 and a photomultiplier tube 11. The photomultiplier tube 11 is located in the multiplier tube sleeve 18. In this embodiment, one end of the multiplier tube sleeve 18 is detachably connected to a connecting sleeve 19. In this embodiment, the connecting sleeve 19 is threadedly connected to the multiplier tube sleeve 18 for easy disassembly and installation. A through hole is opened at the end of the connecting sleeve 19.

[0056] In the present embodiment, installation channels connected to the flow cavity 2 are provided on both sides facing each other at the lower part of the detector body 100. The installation channels are arranged opposite to the through hole at the end of the connecting sleeve 19. One end of the light-transmitting component is connected to one of the installation channels, and the reflector 7 is installed and connected to the other installation channel. The reflector 7 is arranged opposite to the light-transmitting component. A group of mirror reflectors 7 is added opposite to the light-transmitting component, which can collect as many photons of various types on the side of the combustion chamber 1 as possible and reflect them into the passing component.

[0057] In this embodiment, the light-transmitting component includes a support tube 80 and a light guide rod 8. The light guide rod 8 is located on the inner side of the support tube 80. Both ends of the support tube 80 are open ends, which facilitates the light guide rod 8 to smoothly transmit characteristic photons in the direction of the photomultiplier tube. The two ends of the support tube 80 are respectively connected to the multiplier tube sleeve 18 and the detector body 100. Specifically, in this embodiment, the two ends of the support tube 80 are respectively extended into the through hole of the connecting sleeve 19 and the installation channel on the lower body side of the detector body 100, and are threadedly connected to the through hole of the connecting sleeve 19 and the installation channel of the detector body 100. A sealing ring is provided between the support tube 80 and the through hole and the installation channel of the connecting sleeve 19 to ensure the airtightness of the light-transmitting component.

[0058] In this embodiment, the light guide rod 8 is a high-transmittance quartz light guide rod. Both ends of the light guide rod 8 are polished to form a mirror surface by a mirror polishing process. Various characteristic photons generated by the combustion of the measured substance in the combustion chamber 1 are propagated from the light guide rod 8 through the side wall of the guide rod to the surroundings. In this embodiment, a silver mirror coating 9 is plated on the outer circumference of the light guide rod 8 and the mirror surface at both ends, that is, the silver plating process is used on the outer circumference of the guide rod and the mirror surface at both ends to ensure that various photons of different angles are refracted and propagated in the quartz rod as much as possible, reduce the loss of photons during propagation, and enhance the collection of weak light signals of the excitation light, thereby improving the weak light detection capability. Compared with the traditional structure, the light-transmitting component designed by this embodiment can greatly improve the light collection efficiency of the photomultiplier tube 11, increase the sensitivity of the detector and the minimum detection limit.

[0059] In this embodiment, the support tube 80 is made of bakelite, and the thermal conductivity is between 0.15-19. The detector body 100 is made of 316 stainless steel. The temperature of the detector body 100 can reach up to 300°C. The light-transmitting component between the detector and the photomultiplier tube 11 adopts this structural design. Various photons are transmitted through the highly transparent quartz light guide rod 8. The thermal conductivity of the light guide rod 8 is only between 1.3-1.65 when it is ≤300°C. The distance between the detector body 100 and the photomultiplier tube 11 is 30 mm. After the high temperature of the detector body 100 is blocked by the highly transparent quartz light guide rod and the support tube 80 made of bakelite, the temperature on the photomultiplier tube 11 can be basically consistent with the ambient temperature, avoiding affecting the accuracy and performance of the photomultiplier tube 11.

[0060] like Figure 2 As shown, a filter 10 is installed inside the multiplier tube sleeve 18 and between the photomultiplier tube 11 and the light guide rod 8. Specifically: in this embodiment, the filter 10 is located on the inner side of a connecting sleeve 19 connected to the multiplier tube sleeve 18, and the characteristic photons passing through the light-transmitting component will be filtered by the filter 10.

[0061] In this embodiment, the connection sleeve 19 is internally threaded with a back-tightening nut 20, and a through hole is coaxially provided in the center of the back-tightening nut 20, so that characteristic photons can pass through and be received by the photomultiplier tube 11. By tightening the back-tightening nut 20, the filter 10 is pressed, and the filter 10 is limited so that the filter 10 is firmly fixed in the connection sleeve 19. In this embodiment, sealing rings are provided between the filter 10 and the connection sleeve 19 and the back-tightening nut 20, that is, sealing rings are provided on both sides of the filter, so that when the back-tightening nut 20 is tightened, the surface of the filter 10 will not be damaged, and the airtight seal can be ensured at the same time.

[0062] Example 2

[0063] The difference between this embodiment and embodiment 1 is that: this embodiment discloses a pulse flame photometry detection method, using a pulse flame photometry detection device as in embodiment 1, respectively filling the ignition chamber and the combustion chamber with a mixture of hydrogen and air through the ignition chamber intake pipe and the combustion chamber intake pipe, and at the same time filling the combustion chamber with the substance to be tested through the sampling pipe. In this embodiment, the ignition chamber intake pipe fills the ignition chamber with a hydrogen-containing air mixture, and the combustion chamber intake pipe fills the combustion chamber with a hydrogen-rich air mixture, and the hydrogen-containing air mixture first enters the flow cavity, and then moves upward and enters the ignition chamber 3 through the air hole 242 on the upper support block 24;

[0064] When the mixed gas reaches the ignition chamber, the igniter starts to ignite, causing the ignition chamber to burn and generate a flame. The flame in the ignition chamber extends downward to the combustion chamber until it reaches the bottom of the combustion chamber and then goes out. When in use, the ignition chamber 3 and the fuel gas chamber can be filled with equal proportions of gas through a proportional design, so that the gases in the ignition chamber 3 and the fuel gas chamber are burned out at the same time, and the flames are extinguished at the same time, and then the mixed gas is filled in and burned again, thereby achieving the effect of flame pulse combustion.

[0065] From the start of the burning process to the end, photons are excited and generated in the combustion chamber. The photons are reflected by the reflector to the light-transmitting component for transmission and are collected and received by the signal processing component.

[0066] In this embodiment, the substance to be measured is ignited by a hydrogen-rich flame in the combustion chamber 1 and produces chemiluminescence (the wavelength of chemiluminescence produced by different substances is different). The photons generated by the combustion of the substance to be measured are reflected by the reflector 7 to the light guide rod 8 in the light-passing component for propagation, and after being filtered out by the filter 10 for unnecessary photons (i.e., noise photons), they are received by the photomultiplier tube 11 and converted into electrical signals for easy analysis.

[0067] In this embodiment, the signal processing component is set to receive different photons at different times to exclude noise photons, and the required characteristic photons are received at a delayed rate. Specifically, in this embodiment, the noise photons are excluded outside the gate window of the photomultiplier tube by using a gate-controlled electronic device. The gate-controlled electronic device excludes a large amount of flame background noise by adjusting the gate width and delaying the gate integration method, thereby improving the sensitivity of the detector.

[0068] Since various substances (CH*, C2*, OH*, S2*, P2*, etc.) in the pulsed combustion flame have specific chemiluminescence spectra and specific chemiluminescence delays, when measuring the three compounds containing sulfur, phosphorus, and carbon, the emission time of the excited state molecular fragments generated by the detected object in the flame is usually relatively long, while the emission time of other substances, such as hydrocarbon molecular fragments, is relatively short. Therefore, the difference in emission time and emission wavelength of different photons can be used to first integrate the noise photons with very short emission time, such as Figure 3As shown, the leftmost peak of each spectral line is a noise photon, which has a very short emission time (0-5ms). Therefore, when collecting characteristic photons, a gating electronic device is used to exclude this part of the noise photons first, and then the characteristic photons are received by the photomultiplier tube about 5ms after emission. By combining the difference in emission lifetime of specific substances with the dynamics of propagating flames, the time and wavelength information can be used to improve the selectivity of the PFPD, reduce the observed noise, and improve the sensitivity.

[0069] It should be noted that the above description of the disclosed embodiments enables professionals and technicians in the field to implement or use the present application. Various modifications to these embodiments will be apparent to professionals and technicians in the field, and the general principles defined herein can be implemented in other embodiments without departing from the scope of the present application. Therefore, the present application will not be limited to the embodiments shown herein, but should conform to the widest scope consistent with the principles and novel features disclosed herein.

[0070] In the description of the present invention, it should be noted that the terms "first", "second", "third", etc. are only used to distinguish the description and cannot be understood as indicating or implying relative importance.

[0071] In the description of this document, terms such as "up", "down", "left", "right", "front", "back", "top", "bottom", "inside", "outside", "middle", "vertical", "horizontal", "lateral", and "longitudinal" indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only used to illustrate the relative positional relationships between the various components or components, and do not particularly limit the specific installation orientations of the various components or components.

[0072] In the description of this document, some terms may be used to express other meanings in addition to indicating orientation or positional relationship. For example, the term "on" may also be used to express a certain dependency or connection relationship in some cases. For those of ordinary skill in the art, the specific meanings of these terms in this application can be understood according to the specific circumstances.

[0073] In the description of this document, the terms "installed", "set", "provided with", "connected", and "connected" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral structure; it can be a mechanical connection, or an electrical connection; it can be a direct connection, or an indirect connection through an intermediate medium, or it can be an internal connection between two devices, elements, or components. For those of ordinary skill in the art, the specific meanings of the above terms in this application can be understood according to specific circumstances.

[0074] The structures, proportions, sizes, etc. drawn in the drawings in this application are only used to match the contents disclosed in this technical briefing book for technical personnel in this field to understand and read, and are not used to limit the restrictive conditions for the implementation of this application. Therefore, they have no substantive technical significance. Any structural modification, change in proportional relationship or adjustment of size should still fall within the scope of the technical content disclosed in this application without affecting the effects and purposes that can be achieved by this application.

[0075] The terms used in this document are those common terms currently widely used in the art in consideration of the functions of the present disclosure, but these terms may vary according to the intention of a person of ordinary skill in the art, precedents, or new technologies in the art. In addition, specific terms may be selected by the applicant, and in this case, their detailed meanings will be described in the detailed description of the present disclosure. Therefore, the terms used in the document should not be understood as simple names, but rather as an overall description based on the meaning of the terms and the present disclosure.

[0076] Flowcharts or text are used in this document to illustrate the operating steps performed according to the embodiments of the present application. It should be understood that the operating steps in the embodiments of the present application are not necessarily accurately performed in the order of recording. On the contrary, various steps can be processed in reverse order or simultaneously as needed. At the same time, other operations can also be added to these processes, or a certain step or several steps can be removed from these processes.

[0077] The above are only preferred embodiments of the present application and are not intended to limit the present application. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present application should be included in the protection scope of the present application.

Claims

1. A pulse flame photometry detection device, characterized in that: It includes a detector body, a combustion chamber, an ignition chamber, a combustion chamber air intake pipe, an ignition chamber air intake pipe, a light transmission component and a signal processing component, and an igniter is installed on the ignition chamber; A flow cavity is provided in the detector, the combustion chamber is installed in the flow cavity, the ignition chamber is located above the combustion chamber, and the ignition chamber and the combustion chamber are communicated with each other; The ignition chamber air inlet pipe is connected to the ignition chamber, the combustion chamber air inlet pipe is connected to the combustion chamber, and the combustion chamber is also connected to a sample injection tube for introducing the substance to be tested; One end of the light-passing component is located in the flow cavity and on one side of the combustion chamber. A reflector is provided directly opposite the light-passing component. The reflector and the light-passing component are located on both sides of the combustion chamber, and the reflector is installed on the detector body. The signal processing component is used to collect and receive photons transmitted in the light-passing component.

2. A pulsed flame photometry detection device according to claim 1, characterized in that: An air bleed channel is provided in the detector body, and the air bleed channel is located between the combustion chamber and the ignition chamber. Interconnected air holes are provided between the top wall of the flow cavity and the air bleed channel, and the ignition chamber air inlet pipe is connected to the flow cavity.

3. A pulsed flame photometry detection device according to claim 2, characterized in that: The bottom of the circulation cavity is connected to an air inlet nozzle, the top of the air inlet nozzle is connected to a lower support block, the top of the circulation cavity is connected to an upper support block, the bottom of the upper support block and the top of the lower support block are both provided with mutually facing slots, the two ends of the combustion chamber are respectively stuck in the slots of the upper support block and the lower support block, and one end of the sample injection tube passes through the air inlet nozzle and the lower support block in sequence to communicate with the combustion chamber; A center hole is provided in the center of the upper support block, and the center hole is communicated with the air inlet channel and the combustion chamber. An annular groove is provided at the top of the upper support block, and a plurality of air holes are provided at the bottom of the annular groove along its circumference, and the air holes are communicated with the flow cavity and the air inlet channel.

4. A pulsed flame photometry detection device according to claim 2, characterized in that: The combustion chamber and the ignition chamber are arranged alternately, and the air induction channel is perpendicular to the ignition chamber and the combustion chamber and is communicated with each other.

5. A pulsed flame photometry detection device according to claim 1, characterized in that: The volume of the combustion chamber was 35-39 μl.

6. A pulsed flame photometry detection device according to claim 1, characterized in that: The signal processing component includes a multiplier tube sleeve and a photomultiplier tube, wherein the photomultiplier tube is located in the multiplier tube sleeve; The light-transmitting component includes a support tube and a light guide rod. The light guide rod is located inside the support tube. Both ends of the support tube are open ends. The two ends of the support tube are respectively connected to the multiplier tube sleeve and the detector body. A filter is installed in the multiplier tube sleeve and between the photomultiplier tube and the light guide rod.

7. A pulsed flame photometric detection method, using a pulsed flame photometric detection device as claimed in any one of claims 1 to 6, characterized in that: A mixture of hydrogen and air is filled into the ignition chamber and the combustion chamber through the ignition chamber intake pipe and the combustion chamber intake pipe respectively, and the substance to be tested is filled into the combustion chamber through the sampling tube; when the mixture reaches the ignition chamber, the igniter starts to ignite, thereby causing combustion in the ignition chamber to produce a flame, and the flame burning in the ignition chamber extends downward to the combustion chamber until it is extinguished when it extends to the bottom of the combustion chamber. From the burning process to the end, photons are excited in the combustion chamber, and the photons are reflected by the reflector to the light-transmitting component for transmission, and are collected and received by the signal processing component.

8. A pulsed flame photometry detection method according to claim 7, characterized in that: By setting the time when the signal processing component receives different photons, noise photons are excluded and the required characteristic photons are received with delay.

9. A pulsed flame photometry detection method according to claim 8, characterized in that: Use gating electronics to exclude noise photons outside the gate window of the photomultiplier tube.

10. A pulsed flame photometry detection method according to any one of claims 7 to 9, characterized in that: The ignition chamber air intake pipe fills the ignition chamber with a hydrogen-containing air mixture, and the combustion chamber air intake pipe fills the combustion chamber with a hydrogen-rich air mixture.

Citation Information

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