Rapid qualitative device and method for flame retardant components

Abstract

The invention belongs to the technical field of flame retardant detection, and particularly discloses a device and a method for quickly determining the nature of flame retardant components, which are used for quickly determining the nature of the flame retardant components. The device comprises a combustion chamber, a sample introduction device, an ignition device and a spectrum acquisition device, wherein the spectrum acquisition device consists of an optical fiber, an optical fiber spectrometer and a computer control and data processing system. The sampling device and the ignition device are arranged in the combustion chamber, the top wall of the combustion chamber is connected with the ignition device, the ignition device is wirelessly connected with the computer control and data processing system, and the bottom wall of the combustion chamber is connected with the sampling device. The front side wall of the combustion chamber is provided with a window for flame light to penetrate through, the end of the optical fiber right faces the center position of the window, the side wall of the combustion chamber below the window is provided with a plurality of ventilation holes, and the top wall of the combustion chamber is provided with an exhaust port which is detachably connected with a tail gas treatment device. The method is rapid and effective, and is suitable for screening and testing of materials containing 0.5% or above of halogen or phosphorus flame retardants.

Description

Technical Field

[0001] The present invention belongs to the technical field of flame retardant detection, and particularly relates to a device and method for rapid qualitative analysis of flame retardant components. Background Art

[0002] A flame retardant is a functional additive used to reduce the risk of combustion and explosion of materials, and is widely used in various fields of production and life such as building materials, textiles, electronic devices, printed circuit boards, etc. There are various types of flame retardants, including halogen-based, phosphorus-based, nitrogen-based, carbon-based, silicon-based, metal hydroxides, and composite flame retardants, etc. Among them, halogen-based and phosphorus-based flame retardants are widely used in various industrial fields due to their high flame retardancy efficiency.

[0003] Halogen-based flame retardants are mainly compounds and their derivatives containing bromine and chlorine elements, and rely on the release of strongly electronegative hydrogen halides (HX) and halogen free radicals (X·) to capture the free radicals (·OH) released by the combustion of the matrix material in the gas phase, thereby interrupting or slowing down the chemical combustion reaction. However, halogen-based flame retardants will release toxic carcinogenic substances such as dioxins and corrosive hydrogen halide gases during the combustion process, and halogen-based flame retardants themselves, as a kind of persistent organic pollutant, cause serious harm to human and environmental health. Phosphorus-based flame retardants such as organophosphates decompose PO· free radicals, etc., which can quench H· and ·OH free radicals, thereby interrupting the combustion chain reaction and achieving the flame retardant effect, but phosphorus-containing substances are prone to cause eutrophication of water resources and also pose a potential threat to the safety of the ecological environment.

[0004] Therefore, in recent years, more and more attention has been paid to the risks existing in the application process of halogen-based and phosphorus-based flame retardants at home and abroad. Relevant regulations have been introduced to manage and restrict their use, and new green flame retardants have been gradually developed and applied to some products with higher environmental protection requirements, replacing halogen-based and phosphorus-based flame retardants. However, due to the relatively high price of green flame retardants compared with the former two, there are some manufacturers in the market who pass off inferior goods as superior ones, claiming that the products use green flame retardants, but in fact they are still halogen-based and phosphorus-based.

[0005] Currently, the methods for detecting halogen-based and phosphorus-based flame retardants are mainly used to measure trace pollution in water bodies or soils, and a method combining extraction and concentration with mass spectrometry detection is adopted, rarely involving the direct qualitative analysis of the types of flame retardants in products. The most commonly used methods for extraction and concentration are liquid-liquid extraction (LLE), solid-phase extraction (SPE), Soxhlet extraction, etc. The main disadvantage of LLE is that it is time-consuming and consumes a large amount of organic solvents; SPE requires less solvent, but the cost is high; Soxhlet extraction not only requires heating but also takes a long time. The instrument detection methods are mainly liquid chromatography-mass spectrometry (LC-MS) and gas chromatography-mass spectrometry (GC-MS), which perform qualitative and quantitative analysis simultaneously, and the detection limit can be as low as 10 -6. The GC-MS method is not only based on the retention time of the components to be tested in the sample on the spectrum, but more importantly, based on the characteristic ion fragments of the target object during this retention time. The mass spectrometer accurately determines the target object according to its molecular weight and molecular structure, thus overcoming the disadvantage of misjudging the impurity peak as the target object due to the overlap of the retention time of the impurity peak that has not been purified with the target object. Therefore, GC-MS technology has great advantages in trace component analysis. In addition, highly polar, thermally unstable, high molecular weight and low volatility flame retardants can also be detected by LC-MS.

[0006] Although the above method can accurately quantify the content of flame retardants, it is very expensive, the detection steps are cumbersome, the sample processing process is complicated and time-consuming, the Soxhlet extraction process alone takes 8 to 16 hours, and the requirements and dependence on instruments and equipment are relatively high. In the industrial field, it is necessary to quickly batch test the type and content of flame retardants in materials. In law enforcement inspections, it is also necessary to promptly discover the behavior of using banned and restricted flame retardants as green flame retardants in the market to improve product quality. Therefore, it is urgent to develop a fast and effective flame retardant rapid screening technology to simplify acceptance work.

[0007] The present invention proposes a method and device for rapid qualitative detection of flame retardant components based on flame spectrum feature recognition, which will effectively solve the above problems. The optical fiber spectrometer is used to identify the spectral characteristics of spontaneous chemiluminescence of the material combustion flame, and the information of the intermediate products of the material combustion is obtained by comparing the spectrum library. By identifying whether HX or PO· free radicals are released during the combustion process, it is quickly determined whether there are halogen or phosphorus flame retardants in the material and roughly quantified by the characteristic peak radiation intensity, providing effective measures for law enforcement inspections to quickly identify the authenticity of green flame retardants in products, and at the same time, it provides a fast screening foundation for the subsequent selection of the optimal quantitative detection method for halogen or phosphorus flame retardants. Summary of the invention

[0008] One object of the present invention is to provide a rapid qualitative analysis device for flame retardant components, which effectively solves the problem that the existing flame retardant detection method has cumbersome steps and a complicated and time-consuming sample processing process, and is not suitable for rapid qualitative analysis of flame retardant components.

[0009] In order to solve the above technical problems, the technical solution adopted by the present invention is:

[0010] A rapid qualitative device for flame retardant components comprises a combustion chamber, a sampling device, an ignition device and a spectrum collection device, wherein the spectrum collection device is composed of an optical fiber, an optical fiber spectrometer and a computer control and data processing system.

[0011] The sample injection device and the ignition device are both arranged inside the combustion chamber, the top wall of the combustion chamber is connected to the ignition device, the ignition device is wirelessly connected to the computer control and data processing system, and the bottom wall of the combustion chamber is connected to the sample injection device.

[0012] A window for transmitting flame light is provided on the front side wall of the combustion chamber. The end of the optical fiber is directly opposite to the center position of the window. A plurality of ventilation holes are provided on the side wall of the combustion chamber below the window. An exhaust port is provided on the top wall of the combustion chamber, and the exhaust port is detachably connected to an exhaust gas treatment device.

[0013] Further, the sample introduction device includes a lifting plate and a sample tank, and the sample tank is connected to the lifting plate through a connecting rod.

[0014] Further, the ignition device includes a clamping type heating element igniter, a movable arm and a fixed arm. The top end of the fixed arm is connected to the top wall of the combustion chamber, the bottom end of the fixed arm is pivotally connected to the top end of the movable arm, and the bottom end of the movable arm is connected to the clamping type heating element igniter.

[0015] Further, a collimating lens is provided at the end of the optical fiber.

[0016] Further, the plurality of ventilation holes are uniformly arranged in a circle around the combustion chamber.

[0017] Further, the window is made of quartz glass.

[0018] Further, the window is provided at the center position of the front side wall of the combustion chamber.

[0019] Further, the movable range of the movable arm is to rotate 180° around the fixed arm on a vertical plane.

[0020] Further, the spectral acquisition device is provided in front of the front side of the combustion chamber.

[0021] Further, a flame spectrum underlying database, a characteristic peak position database and a spectrogram comparison and recognition algorithm are stored in the computer control and data processing system.

[0022] Another object of the present invention is to provide a method for quickly qualitatively determining the components of a flame retardant, which effectively solves the problems that the steps of the existing flame retardant detection method are cumbersome and the sample processing process is complex and time-consuming, and it is not suitable for quickly qualitatively determining the components of a flame retardant.

[0023] To solve the above technical problems, the technical solution adopted by the present invention is:

[0024] A method for quickly qualitatively determining the components of a flame retardant, which is applied to the device for quickly qualitatively determining the components of a flame retardant described in the above embodiment, includes the following steps:

[0025] S1. Raise the sample cell to the upper part of the combustion chamber by adjusting the lifting plate. Take out the sample cell from the combustion chamber through the exhaust port, then add the liquid or solid sample to be measured into the sample cell. Subsequently, place the sample cell back into the combustion chamber and lower the lifting plate until the sample cell is at the lower edge of the window.

[0026] S2. Connect the tail gas treatment device to the exhaust port.

[0027] S3. Start the test. Adjust the ignition device above the sample cell and heat to ignite the sample to be measured through the computer control and data processing system. After ignition, stop heating and adjust the ignition device away from the sample cell. At the same time, the fiber optic spectrometer starts to continuously collect data until the flame spectrum of the sample in a stable combustion state is collected. During this period, adjust the height of the sample cell through the lifting plate to reach a position convenient for collecting the flame spectrum.

[0028] S4. Compare and identify whether there are characteristic peaks of HX or PO· free radicals in the collected combustion flame spectrum of the measured sample through the computer control and data processing system. If there is a characteristic peak of HX in the combustion flame spectrum of the measured sample, then HX is released during the combustion process of the measured sample, thereby determining that there is a halogen-based flame retardant in the measured sample; if there is a characteristic peak of PO· free radicals in the combustion flame spectrum of the measured sample, then PO· free radicals are released during the combustion process of the measured sample, thereby determining that there is a phosphorus-based flame retardant in the measured sample.

[0029] Further, the ignition device includes a clamping type heating element igniter, a movable arm, and a fixed arm. The top end of the fixed arm is connected to the top wall of the combustion chamber. The bottom end of the fixed arm is pivotally connected to the top end of the movable arm. The bottom end of the movable arm is connected to the clamping type heating element igniter.

[0030] Further, in step S3, before starting the test, the movable arm and the fixed arm overlap. After starting the test, adjust the movable arm to rotate clockwise through the computer control and data processing system, thereby driving the clamping type heating element igniter above the sample cell and heating to ignite the sample to be measured. After ignition, stop heating and adjust the movable arm to rotate counterclockwise until it overlaps with the fixed arm.

[0031] The beneficial technical effects of the present invention are:

[0032] (1) The present invention uses a fiber optic spectrometer to identify the spectral characteristics of the spontaneous chemiluminescence of the material combustion flame, compares the spectral library to obtain the information of the intermediate products of the material combustion, quickly determines whether there is a halogen-based or phosphorus-based flame retardant in the material by identifying whether HX or PO· free radicals are released during the combustion process, and makes a rough quantification through the radiation intensity of the characteristic peaks, effectively solving the problems that the steps of the existing flame retardant detection methods are cumbersome and the sample treatment process is complex and time-consuming, and it is not suitable for the rapid qualitative analysis of the flame retardant components.

[0033] (2) The present invention provides an effective measure for quickly identifying the authenticity of green flame retardants in products during law enforcement inspections, and at the same time lays a quick screening foundation for subsequent selection of the optimal quantitative detection methods for halogen-based or phosphorus-based flame retardants.

[0034] (3) The present invention is fast, effective, has wide sample applicability, and strong versatility, and is suitable for screening tests of materials containing more than 0.5% halogen-based or phosphorus-based flame retardants. BRIEF DESCRIPTION OF THE DRAWINGS

[0035] In order to clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for use in the embodiments will be briefly introduced below. Obviously, the drawings in the following description are those of some embodiments of the present invention. For those of ordinary skill in the art, other drawings can also be obtained based on these drawings without creative efforts.

[0036] Figure 1 It is a schematic structural diagram of the rapid qualitative device for the components of the flame retardant of the present invention;

[0037] Figure 2 It is the combustion flame spectrogram of Example 1, Example 2 and Example 3 of the present invention.

[0038] Figure 1 In the figure: 1. Combustion chamber;

[0039] 2. Ventilation opening;

[0040] 3. Lifting plate;

[0041] 4. Sample tank;

[0042] 5. Heating element igniter;

[0043] 6. Movable arm;

[0044] 7. Exhaust port;

[0045] 8. Tail gas treatment device;

[0046] 9. Collimating lens;

[0047] 10. Optical fiber;

[0048] 11. Optical fiber spectrometer;

[0049] 12. Computer control and data processing system;

[0050] 13. Window;

[0051] 14. Fixed arm. SPECIFIC EMBODIMENTS

[0052] Embodiment 1:

[0053] A rapid qualitative device for flame retardant components, such as Figure 1 As shown, it includes a combustion chamber 1, a sample injection device, an ignition device and a spectrum collection device, and the spectrum collection device is composed of an optical fiber 10, an optical fiber spectrometer 11 and a computer control and data processing system 12.

[0054] The sample injection device and the ignition device are both arranged inside the combustion chamber 1, the top wall of the combustion chamber 1 is connected to the ignition device, the ignition device is wirelessly connected to the computer control and data processing system 12, and the bottom wall of the combustion chamber 1 is connected to the sample injection device.

[0055] A window 13 for passing flame light is provided on the front side wall of the combustion chamber 1, the end of the optical fiber 10 is directly opposite to the center of the window 13, a plurality of ventilation holes 2 are provided on the side wall of the combustion chamber 1 below the window 13, an exhaust port 7 is provided on the top wall of the combustion chamber 1, and the exhaust port 7 is detachably connected to the exhaust gas treatment device 8. In this embodiment, the plurality of ventilation holes 2 are evenly arranged around the combustion chamber 1.

[0056] The sample injection device includes a lifting plate 3 and a sample slot 4, and the sample slot 4 is connected to the lifting plate 3 by a connecting rod, so that the height of the sample slot 4 in the combustion chamber 1 can be flexibly adjusted, which is convenient for taking the sample slot 4 out of the combustion chamber 1 through the exhaust port 7 for sample addition and adjusting the position of the sample combustion flame during the experiment.

[0057] The ignition device includes a clamping heating element ignition device 5, a movable arm 6 and a fixed arm 14, the top end of the fixed arm 14 is connected to the top wall of the combustion chamber 1, the bottom end of the fixed arm 14 is pivotally connected to the top end of the movable arm 6, and the bottom end of the movable arm 6 is connected to the clamping heating element ignition device 5.

[0058] In this embodiment, the movable arm 6 has a range of motion of 180° in a vertical plane around the fixed arm 14. Automatic intermittent ignition is achieved outside the combustion chamber 1 through a computer control and data processing system 12. After ignition is completed, the movable arm 6 rotates counterclockwise to lift the clamping heating element igniter 5.

[0059] In this embodiment, the size of the combustion chamber 1 is 200 mm×200 mm×400 mm, which can play a windproof role, so that the combustion flame can be kept as stable as possible and free from interference from chaotic airflow.

[0060] In this embodiment, the ventilation hole 2 is opened at a distance of 100 mm from the bottom surface of the combustion chamber 1 and the diameter of the ventilation hole 2 is 4 mm.

[0061] In this embodiment, the sample slot 4 is a disc with a diameter of 50 mm and a depth of 10 mm, which is suitable for testing solid and liquid samples.

[0062] In this embodiment, the diameter of the exhaust port 7 is 100 mm, and the gas generated by the combustion reaction can be discharged through the tail gas treatment device 8 placed above the combustion chamber 1.

[0063] The rapid qualitative method for flame retardant components is applied to the rapid qualitative device for flame retardant components in this embodiment, and includes the following steps:

[0064] S1. Adjust the lifting plate 3 to raise the sample cell 4 to the upper part of the combustion chamber 1, take out the sample cell 4 from the combustion chamber 1 through the exhaust port 7, then add a liquid or solid sample to be measured into the sample cell 4, and the addition amount is handled according to the specific experimental situation. Subsequently, put the sample cell 4 back into the combustion chamber 1, and lower the lifting plate 3 until the sample cell 4 is at the lower edge of the window 13.

[0065] S2. After sample injection is completed, connect the tail gas treatment device 8 to the exhaust port 7.

[0066] S3. Before starting the test, the movable arm 6 overlaps with the fixed arm 14. After starting the test, the computer-controlled and data processing system 12 is used to adjust the movable arm 6 to rotate clockwise, thereby driving the clamping type heating element igniter 5 above the sample cell 4 and heating to ignite the sample to be measured. After ignition, stop heating and adjust the movable arm 6 to rotate counterclockwise until it overlaps with the fixed arm 14. At the same time, the fiber optic spectrometer 11 starts to continuously collect data until the flame spectrum of the sample in a stable combustion state is collected. During this period, the height of the sample cell 4 is adjusted through the lifting plate 3 to reach a position convenient for collecting the flame spectrum.

[0067] S4. The computer-controlled and data processing system 12 is used to compare and identify whether there are characteristic peaks of HX or PO· free radicals in the collected combustion flame spectrum of the sample to be measured.

[0068] If there is a characteristic peak of HX in the combustion flame spectrum of the sample to be measured, then HX is released during the combustion process of the sample to be measured, thereby determining that there is a halogen-based flame retardant in the sample to be measured.

[0069] If there is a characteristic peak of PO· free radicals in the combustion flame spectrum of the sample to be measured, then PO· free radicals are released during the combustion process of the sample to be measured, thereby determining that there is a phosphorus-based flame retardant in the sample to be measured.

[0070] This embodiment provides an effective measure for law enforcement inspections to quickly identify the authenticity of green flame retardants in products, and at the same time lays a quick screening foundation for subsequent selection of the optimal quantitative detection methods for halogen-based or phosphorus-based flame retardants.

[0071] This embodiment is fast, effective, has wide sample applicability and strong versatility, and is suitable for screening tests of materials containing more than 0.5% halogen-based or phosphorus-based flame retardants.

[0072] Embodiment 2:

[0073] A rapid qualitative device for flame retardant components, as Figure 1 shown, comprising a combustion chamber 1, a sampling device, an ignition device and a spectral acquisition device. The spectral acquisition device consists of an optical fiber 10, an optical fiber spectrometer 11 and a computer control and data processing system 12. The detection spectral range of the optical fiber spectrometer 11 is 200 - 1100 nm.

[0074] Since during the detection process, all optical signals around the flame will enter the optical fiber spectrometer 11, thus affecting the accuracy of the flame spectral signal. Therefore, in this embodiment, a collimating lens 9 is provided at the end of the optical fiber 10 to ensure that the optical fiber spectrometer 11 only obtains the flame spectral data in the forward parallel direction.

[0075] The computer control and data processing system 12 stores a flame spectral bottom layer database, a characteristic peak position database and a spectral pattern comparison and recognition algorithm. The flame spectral database stores the combustion flame spectra of various typical halogen - based or phosphorus - based flame retardant materials with different contents, and establishes an equivalent quantitative standard according to the characteristic peak intensity. For example, the characteristic spectral line of the PO· free radical is located at 327 nm. The spectral pattern comparison and recognition algorithm can compare the combustion flame spectral curve collected by the spectral acquisition device with the peak position and peak intensity in the spectral library and perform equivalent conversion, so as to achieve rapid qualitative and rough quantitative analysis.

[0076] The spectral acquisition device is arranged in front of the front side wall of the combustion chamber 1, facing the center of the quartz glass window 13, and collects the flame spectral signals when the sample reaches the stable combustion stage.

[0077] The sampling device and the ignition device are both arranged inside the combustion chamber 1. The top wall of the combustion chamber 1 is connected to the ignition device, the ignition device is wirelessly connected to the computer control and data processing system 12, and the bottom wall of the combustion chamber 1 is connected to the sampling device.

[0078] A window 13 for transmitting the flame light is provided on the front side wall of the combustion chamber 1. The end of the optical fiber 10 faces the center position of the window 13. A plurality of ventilation holes 2 are provided on the side wall of the combustion chamber 1 below the window 13. An exhaust port 7 is provided on the top wall of the combustion chamber 1, and the exhaust port 7 is detachably connected to a tail gas treatment device 8.

[0079] In this embodiment, the plurality of ventilation holes 2 are uniformly arranged around the combustion chamber in a circle.

[0080] The sample injection device includes a lifting plate 3 and a sample slot 4, and the sample slot 4 is connected to the lifting plate 3 by a connecting rod, so that the height of the sample slot 4 in the combustion chamber 1 can be flexibly adjusted, which is convenient for taking the sample slot 4 out of the combustion chamber 1 through the exhaust port 7 for sample addition and adjusting the position of the sample combustion flame during the experiment.

[0081] The ignition device comprises a clamping heating element ignition tool 5, a movable arm 6 and a fixed arm 7, wherein the top end of the fixed arm 7 is connected to the top wall of the combustion chamber 1, the bottom end of the fixed arm 7 is pivotally connected to the top end of the movable arm 6, and the bottom end of the movable arm 6 is connected to the clamping heating element ignition tool 5. In this embodiment, the movable arm 6 has a range of motion of 180° rotation around the fixed arm on a vertical plane. Automatic intermittent ignition is achieved outside the combustion chamber 1 through a computer control and data processing system 12, and after ignition is completed, the movable arm 6 rotates counterclockwise to lift the clamping heating element ignition tool 5.

[0082] In this embodiment, the size of the combustion chamber 1 is 200 mm×200 mm×400 mm, which can play a windproof role, so that the combustion flame can be kept as stable as possible and free from interference from chaotic airflow.

[0083] In this embodiment, the ventilation hole 2 is opened at a distance of 100 mm from the bottom surface of the combustion chamber 1 and the diameter of the ventilation hole 2 is 4 mm.

[0084] In this embodiment, the sample slot 4 is a disc with a diameter of 50 mm and a depth of 10 mm, which is suitable for testing solid and liquid samples.

[0085] In this embodiment, the diameter of the exhaust port 7 is 100 mm, and the gas generated by the combustion reaction can be discharged through the exhaust gas treatment device 8 placed above the combustion chamber 1.

[0086] The flame retardant component rapid qualitative method is applied to the flame retardant component rapid qualitative device described in this embodiment, comprising the following steps:

[0087] S1. The sample trough 4 is raised to the upper part of the combustion chamber 1 by adjusting the lifting plate 3, and the sample trough 4 is taken out from the combustion chamber 1 through the exhaust port 7. Then, a liquid or solid sample to be tested is added to the sample trough 4, and the added amount is adjusted according to the specific experimental situation. Subsequently, the sample trough 4 is put back into the combustion chamber 1, and the lifting plate 3 is lowered until the sample trough 4 is at the lower edge of the window 13.

[0088] S2. After the sample injection is completed, the tail gas treatment device 8 is connected to the exhaust port 7.

[0089] S3. Before the test starts, the movable arm 7 overlaps with the fixed arm 14. After the test starts, the computer control and data processing 12 system adjusts the movable arm 7 to rotate clockwise, thereby driving the clamping type heating element igniter 5 above the sample cell 4 and heating to ignite the sample to be tested. After ignition, heating is stopped and the movable arm 7 is adjusted to rotate counterclockwise until it overlaps with the fixed arm 14. At the same time, the fiber optic spectrometer 11 starts to continuously collect data until the flame spectrum of the sample in a stable combustion state is collected. During this period, the height of the sample cell 4 is adjusted by the lifting plate 3 to reach a position convenient for collecting the flame spectrum.

[0090] S4. The computer control and data processing system 12 is used to compare and identify whether there are characteristic peaks of HX or PO· free radicals in the collected combustion flame spectrum of the sample to be tested.

[0091] If there is a characteristic peak of HX in the combustion flame spectrum of the sample to be tested, then HX is released during the combustion process of the sample to be tested, thereby determining that there is a halogen-based flame retardant in the sample to be tested.

[0092] If there is a characteristic peak of PO· free radicals in the combustion flame spectrum of the sample to be tested, then PO· free radicals are released during the combustion process of the sample to be tested, thereby determining that there is a phosphorus-based flame retardant in the sample to be tested.

[0093] This embodiment provides an effective measure for law enforcement inspections to quickly identify the authenticity of green flame retardants in products, and at the same time lays a quick screening foundation for subsequent selection of the optimal quantitative detection methods for halogen-based or phosphorus-based flame retardants.

[0094] This embodiment is fast, effective, has wide sample applicability and strong generality, and is suitable for screening tests of materials containing more than 0.5% halogen-based or phosphorus-based flame retardants.

[0095] Embodiment 3:

[0096] A device for rapid qualitative determination of flame retardant components, as Figure 1 shown, includes a combustion chamber 1, a sample injection device, an ignition device, and a spectrum collection device. The spectrum collection device is composed of an optical fiber 10, a fiber optic spectrometer 11, and a computer control and data processing system 12. The detection spectral range of the fiber optic spectrometer 11 is 200 - 1100 nm.

[0097] Since during the detection process, all optical signals around the flame will enter the fiber optic spectrometer 11, thus affecting the accuracy of the flame spectrum signal. Therefore, in this embodiment, a collimating lens 9 is provided at the end of the optical fiber 10 to ensure that the fiber optic spectrometer 11 only obtains the flame spectrum data in the forward parallel direction.

[0098] The computer control and data processing system 12 stores a flame spectrum underlying database, a characteristic peak position database, and a spectrum comparison and recognition algorithm. The flame spectrum database stores the combustion flame spectra of various typical halogen-based or phosphorus-based flame retardant materials with different contents, and establishes an equivalent quantitative standard based on the characteristic peak intensity. For example, the characteristic spectral line of the PO· free radical is located at 327 nm. The spectrum comparison and recognition algorithm can compare the combustion flame spectrum curve collected by the spectrum collection device with the peak position and peak intensity of the spectrum library, and perform equivalent conversion, so as to achieve rapid qualitative and rough quantitative analysis.

[0099] The spectrum collection device is arranged in front of the front side of the combustion chamber 1, facing the center of the quartz glass window 13, and collects the flame spectrum signal of the sample when it reaches the stable combustion stage.

[0100] The sample injection device and the ignition device are both arranged inside the combustion chamber 1. The top wall of the combustion chamber 1 is connected to the ignition device, the ignition device is wirelessly connected to the computer control and data processing system 12, and the bottom wall of the combustion chamber 1 is connected to the sample injection device.

[0101] A window 13 for transmitting flame light is provided on the front side wall of the combustion chamber 1. In this embodiment, the window 13 is made of quartz glass. The window 13 is arranged at the center position of the front side wall of the combustion chamber 1.

[0102] The end of the optical fiber 10 faces the center position of the window 13. A plurality of ventilation holes 2 are provided on the side wall of the combustion chamber 1 below the window 13. An exhaust port 7 is provided on the top wall of the combustion chamber 1, and the exhaust port 7 is detachably connected to the tail gas treatment device 8.

[0103] In this embodiment, the plurality of ventilation holes 2 are uniformly arranged around the combustion chamber 1 in a circle.

[0104] The sample injection device includes a lifting plate 3 and a sample tank 4. The sample tank 4 is connected to the lifting plate 3 through a connecting rod, so that the height of the sample tank 4 in the combustion chamber 1 can be flexibly adjusted, which is convenient for taking out the sample tank 4 from the combustion chamber 1 through the exhaust port 7 for sample addition and adjusting the position of the sample combustion flame during the experiment.

[0105] The ignition device includes a clamping type heating element igniter 5, a movable arm 6 and a fixed arm 14. The top end of the fixed arm 14 is connected to the top wall of the combustion chamber 1, the bottom end of the fixed arm 14 is pivotally connected to the top end of the movable arm 6, and the bottom end of the movable arm 6 is connected to the clamping type heating element igniter 5.

[0106] In this embodiment, the movable range of the movable arm 6 is to rotate 180° around the fixed arm on the vertical plane. Automatic intermittent ignition is realized through the computer control and data processing system 12 outside the combustion chamber. After ignition is completed, the movable arm 6 rotates counterclockwise to lift the clamping type heating element igniter 5.

[0107] In this embodiment, the size of the combustion chamber 1 is 200mm×200mm×400mm, which can play a role in wind prevention, keep the combustion flame as stable as possible, and avoid being interfered by the disordered air flow.

[0108] In this embodiment, the ventilation hole 2 is opened at a position 100mm away from the bottom surface of the combustion chamber 1 and the diameter of the ventilation hole 2 is 4mm.

[0109] In this embodiment, the sample cell 4 is a disc with a diameter of 50mm and a depth of 10mm, which is suitable for testing solid and liquid samples.

[0110] In this embodiment, the diameter of the exhaust port 7 is 100mm, and the gas generated by the combustion reaction can be discharged through the tail gas treatment device 8 placed above the combustion chamber 1.

[0111] In this embodiment, the size of the quartz glass window 13 is 100mm×100mm, which ensures that the spectral acquisition device can collect spectral signals with sufficient intensity.

[0112] The rapid qualitative method for flame retardant components is applied to the rapid qualitative device for flame retardant components described in this embodiment, and includes the following steps:

[0113] S1. Adjust the lifting plate 3 to raise the sample cell 4 to the upper part of the combustion chamber 1, take out the sample cell 4 from the combustion chamber 1 through the exhaust port 7, then add the liquid or solid sample to be tested into the sample cell 4, and the addition amount is handled according to the specific experimental situation. Subsequently, put the sample cell 4 back into the combustion chamber 1, and lower the lifting plate 3 until the sample cell 4 is at the lower edge of the window 13.

[0114] S2. After sample injection is completed, connect the tail gas treatment device 8 to the exhaust port 7.

[0115] S3. Before starting the test, the movable arm 6 overlaps with the fixed arm 14. After starting the test, adjust the movable arm 6 to rotate clockwise through the computer control and data processing system 12, so as to drive the clamping type heating element igniter 5 above the sample cell 4 and heat to ignite the sample to be tested. After ignition, stop heating and adjust the movable arm 6 to rotate counterclockwise until it overlaps with the fixed arm 14. At the same time, the fiber optic spectrometer 11 starts to continuously collect data until the flame spectrum of the sample in a stable combustion state is collected. During this period, adjust the height of the sample cell 4 through the lifting plate 3 to reach a position convenient for collecting the flame spectrum.

[0116] S4. Compare and identify, through a computer control and data processing system 12, whether there are characteristic peaks of HX or PO· free radicals in the combustion flame spectrum of the measured sample collected.

[0117] If there is a characteristic peak of HX in the combustion flame spectrum of the measured sample, then HX is released during the combustion process of the measured sample, thereby determining that there is a halogen-based flame retardant in the measured sample.

[0118] If there is a characteristic peak of PO· free radicals in the combustion flame spectrum of the measured sample, then PO· free radicals are released during the combustion process of the measured sample, thereby determining that there is a phosphorus-based flame retardant in the measured sample.

[0119] This embodiment provides an effective measure for law enforcement inspections to quickly identify the authenticity of green flame retardants in products, and at the same time lays a quick screening foundation for subsequent selection of the optimal quantitative detection methods for halogen-based or phosphorus-based flame retardants.

[0120] This embodiment is fast, effective, has wide sample applicability and strong generality, and is suitable for screening tests of materials containing more than 0.5% halogen-based or phosphorus-based flame retardants.

[0121] It should be noted that in the description of the present invention, unless otherwise specified, the meaning of "a plurality" is two or more.

[0122] In the description of the present invention, unless otherwise clearly defined and limited, terms such as "set", "connected", etc. should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or integrated; it can be directly connected, or indirectly connected through an intermediate medium; if the connection method is not specifically described, conventional means mature in the prior art are adopted. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood according to specific situations.

[0123] In the description of this specification, the description referring to the term "some specific embodiments" means that the specific features, structures, materials, or characteristics described in connection with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic description of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials, or characteristics described can be combined in a suitable manner in any one or more embodiments or examples.

[0124] Next, the embodiments of the present invention will be further described in detail with reference to the drawings and examples.

[0125] Example 1:

[0126] Use the flame spectrum acquisition device for rapid qualitative analysis of the flame retardant components described in Embodiment 3 of the present invention to collect the combustion flame spectra of various typical halogen-based or phosphorus-based flame retardant materials with different contents, such as organophosphates, polybrominated biphenyls, etc., establish a basic database of flame spectra of halogen-based and phosphorus-based flame retardant materials, and establish an equivalent quantitative standard based on the characteristic peak intensities. The operation steps are as follows.

[0127] S1. Adjust the lifting plate to raise the sample cell to the upper part of the combustion chamber, take out the sample cell from the combustion chamber through the exhaust port, then add the liquid or solid sample to be measured into the sample cell. The addition amount is handled according to the specific experimental situation. Subsequently, put the sample cell back into the combustion chamber and lower the lifting plate until the sample cell is at the lower edge of the window.

[0128] S2. After the sample injection is completed, connect the tail gas treatment device to the exhaust port.

[0129] S3. Before starting the test, the movable arm overlaps with the fixed arm. After starting the test, adjust the movable arm to rotate clockwise through the computer control and data processing system, so as to drive the clamping type heating element igniter above the sample cell and heat to ignite the sample to be measured. After ignition, stop heating and adjust the movable arm to rotate counterclockwise until it overlaps with the fixed arm. At the same time, the fiber optic spectrometer starts to continuously collect data until the flame spectrum of the sample in a stable combustion state is collected. During this period, adjust the height of the sample cell through the lifting plate to reach a position convenient for collecting the flame spectrum.

[0130] S4. Identify the characteristic peak positions of the intermediate products HCl, HBr, and PO· free radicals through the computer control and data processing system.

[0131] Then, use the flame spectrum acquisition device for rapid qualitative analysis of the flame retardant components described in Embodiment 3 of the present invention to rapidly qualitatively analyze the flame retardant components in the electrolyte of 1# commercial lithium-ion battery. The specific operation steps are as follows.

[0132] First, adjust the lifting plate to raise the sample cell to the upper part of the combustion chamber, take out the sample cell from the combustion chamber through the exhaust port, then add 3 mL of the electrolyte to be measured into the sample cell. Subsequently, put the sample cell back into the combustion chamber and lower the lifting plate until the sample cell is at the lower edge of the window.

[0133] Then, after the sample injection is completed, connect the tail gas treatment device to the exhaust port.

[0134] Before starting the test, the movable arm overlaps with the fixed arm. After starting the test, the movable arm is adjusted to rotate clockwise through the computer control and data processing system, thereby driving the clamping type heating element igniter above the sample tank and heating to ignite the sample to be tested. After ignition, the heating is stopped and the movable arm is adjusted to rotate counterclockwise until it overlaps with the fixed arm. At the same time, the fiber optic spectrometer starts to continuously collect data until the flame spectrum of the sample in a stable combustion state is collected. During this period, the height of the sample tank is adjusted by the lifting plate to reach a position convenient for collecting the flame spectrum.

[0135] Finally, the computer control and data processing system is used to identify and compare the collected combustion flame spectra of the samples to be measured.

[0136] The comparison and identification result is Figure 2 For the flame spectrum curve of dimethyl carbonate + trimethyl phosphate (solvent DMC + flame retardant additive TMP) in , there is a characteristic peak of PO· free radical at 327 nm, indicating that PO· free radical is released during the combustion process of the sample to be measured. Thus, it can be quickly judged that the flame retardant component in the sample to be measured is a phosphorus-based flame retardant, providing a direction for the subsequent selection of the quantitative detection method for the flame retardant.

[0137] Example 2:

[0138] Use the flame retardant component rapid qualitative device described in Embodiment 3 of the present invention to collect the combustion flame spectra of various typical halogen-based or phosphorus-based flame retardant materials with different contents, such as organophosphates, polybrominated biphenyls, etc., establish a bottom layer database of the flame spectra of halogen-based and phosphorus-based flame retardant materials, and establish an equivalent quantitative standard according to the characteristic peak intensity. The operation steps are as follows.

[0139] S1. Adjust the lifting plate to raise the sample tank to the upper part of the combustion chamber, take out the sample tank from the combustion chamber through the exhaust port, then add the liquid or solid sample to be measured into the sample tank. The addition amount is handled according to the specific experimental situation. Subsequently, put the sample tank back into the combustion chamber and lower the lifting plate until the sample tank is at the lower edge of the window.

[0140] S2. After the sample injection is completed, connect the tail gas treatment device to the exhaust port.

[0141] S3. Before starting the test, the movable arm overlaps with the fixed arm. After starting the test, the movable arm is adjusted to rotate clockwise through the computer control and data processing system, thereby driving the clamping type heating element igniter above the sample tank and heating to ignite the sample to be tested. After ignition, the heating is stopped and the movable arm is adjusted to rotate counterclockwise until it overlaps with the fixed arm. At the same time, the fiber optic spectrometer starts to continuously collect data until the flame spectrum of the sample in a stable combustion state is collected. During this period, the height of the sample tank is adjusted by the lifting plate to reach a position convenient for collecting the flame spectrum.

[0142] S4. Identify the characteristic peak positions of the intermediate products HCl, HBr, and PO· radicals through the computer control and data processing system.

[0143] Then, use the flame retardant component rapid qualitative device described in Embodiment 3 of the present invention to collect and identify the combustion flame spectra of pure solvent dimethyl carbonate (DMC). The specific operation steps are as follows.

[0144] First, adjust the lifting plate to raise the sample cell to the upper part of the combustion chamber, take out the sample cell from the combustion chamber through the exhaust port, then add 3 mL of DMC liquid sample to the sample cell, and then put the sample cell back into the combustion chamber and lower the lifting plate until the sample cell is at the lower edge of the window.

[0145] Then, after the sample injection is completed, connect the tail gas treatment device to the exhaust port.

[0146] Before starting the test, the movable arm overlaps with the fixed arm. After starting the test, adjust the movable arm to rotate clockwise through the computer control and data processing system, so as to drive the clamping type heating element igniter above the sample cell and heat to ignite the sample to be tested. After ignition, stop heating and adjust the movable arm to rotate counterclockwise until it overlaps with the fixed arm. At the same time, the fiber optic spectrometer starts to continuously collect data until the flame spectrum of the sample in a stable combustion state is collected. During this period, adjust the height of the sample cell through the lifting plate to reach a position convenient for collecting the flame spectrum.

[0147] Finally, identify and compare the collected combustion flame spectra of the tested sample through the computer control and data processing system.

[0148] The comparison and identification result is Figure 2 In the flame spectrum curve of pure DMC, no characteristic peaks of HCl, HBr, or PO· radicals are identified, and the characteristic peak intensity of ·OH required for the combustion chain reaction at 309 nm is significantly higher than that of the DMC + TMP sample, indicating that no HX or PO· radicals are released during the combustion process of the tested sample, and there are no halogen-based or phosphorus-based flame retardants in the tested sample.

[0149] Example 3:

[0150] Use the flame retardant component rapid qualitative device described in Embodiment 3 of the present invention to collect the combustion flame spectra of various typical halogen-based or phosphorus-based flame retardant materials with different contents, such as organophosphates, polybrominated biphenyls, etc., establish a bottom layer database of flame spectra of halogen-based and phosphorus-based flame retardant materials, and establish an equivalent quantitative standard according to the characteristic peak intensity. The operation steps are as follows.

[0151] S1. Raise the sample cell to the upper part of the combustion chamber by adjusting the lifting plate. Take out the sample cell from the combustion chamber through the exhaust port, then add the liquid or solid sample to be measured into the sample cell. The addition amount is determined according to the specific experimental situation. Subsequently, place the sample cell back into the combustion chamber and lower the lifting plate until the sample cell is at the lower edge of the window.

[0152] S2. After sample injection is completed, connect the tail gas treatment device to the exhaust port.

[0153] S3. Before starting the test, the movable arm overlaps with the fixed arm. After starting the test, adjust the movable arm to rotate clockwise through the computer control and data processing system, thereby driving the clamping type heating element igniter above the sample cell and heating to ignite the sample to be measured. After ignition, stop heating and adjust the movable arm to rotate counterclockwise until it overlaps with the fixed arm. At the same time, the fiber optic spectrometer starts to continuously collect data until the flame spectrum of the sample in a stable combustion state is collected. During this period, adjust the height of the sample cell through the lifting plate to reach a position convenient for collecting the flame spectrum.

[0154] S4. Identify the characteristic peak positions of the intermediate products HCl, HBr, and PO· free radicals through the computer control and data processing system.

[0155] Then, quickly qualitatively analyze the flame retardant components in the No. 2 electrolyte solution using the flame retardant component rapid qualitative device described in Embodiment 3 of the present invention. The specific operation steps are as follows.

[0156] First, raise the sample cell to the upper part of the combustion chamber by adjusting the lifting plate. Take out the sample cell from the combustion chamber through the exhaust port, then add 3 mL of the electrolyte solution to be measured into the sample cell. Subsequently, place the sample cell back into the combustion chamber and lower the lifting plate until the sample cell is at the lower edge of the window.

[0157] Then, after sample injection is completed, connect the tail gas treatment device to the exhaust port.

[0158] Before starting the test, the movable arm overlaps with the fixed arm. After starting the test, adjust the movable arm to rotate clockwise through the computer control and data processing system, thereby driving the clamping type heating element igniter above the sample cell and heating to ignite the sample to be measured. After ignition, stop heating and adjust the movable arm to rotate counterclockwise until it overlaps with the fixed arm. At the same time, the fiber optic spectrometer starts to continuously collect data until the flame spectrum of the sample in a stable combustion state is collected. During this period, adjust the height of the sample cell through the lifting plate to reach a position convenient for collecting the flame spectrum.

[0159] Finally, identify and compare the collected combustion flame spectrum of the measured sample through the computer control and data processing system.

[0160] The comparison and identification result is Figure 2The flame spectral curve of dimethyl carbonate + lithium hexafluorophosphate (solvent DMC + lithium salt LiPF6) has a characteristic peak of PO· radical at 327 nm, indicating that PO· radicals are released during the combustion process of the measured sample, thus quickly determining that the flame retardant component in the measured sample is a phosphorus-based flame retardant. In fact, lithium hexafluorophosphate, the lithium salt added to the electrolyte as a lithium ion source, also has potential flame retardant effects and health and environmental hazards.

[0161] Example 4:

[0162] Use the flame retardant component rapid qualitative device described in Embodiment 3 of the present invention to collect the combustion flame spectra of various typical halogen-based or phosphorus-based flame retardant materials with different contents, such as organophosphates, polybrominated biphenyls, etc., establish a bottom database of flame spectra of halogen-based and phosphorus-based flame retardant materials, and establish an equivalent quantitative standard based on the characteristic peak intensity. The operation steps are as follows.

[0163] S1. Adjust the lifting plate to raise the sample tank to the upper part of the combustion chamber, take out the sample tank from the combustion chamber through the exhaust port, then add the liquid or solid sample to be measured into the sample tank, and the addition amount can be handled according to the specific experimental situation. Subsequently, put the sample tank back into the combustion chamber and lower the lifting plate until the sample tank is at the lower edge of the window.

[0164] S2. After sample injection is completed, connect the tail gas treatment device to the exhaust port.

[0165] S3. Before starting the test, the movable arm overlaps with the fixed arm. After starting the test, adjust the movable arm to rotate clockwise through the computer control and data processing system, so as to drive the clamping type heating element igniter above the sample tank and heat to ignite the sample to be measured. After ignition, stop heating and adjust the movable arm to rotate counterclockwise until it overlaps with the fixed arm. At the same time, the fiber optic spectrometer starts to continuously collect data until the flame spectrum of the sample in a stable combustion state is collected. During this period, adjust the height of the sample tank through the lifting plate to reach a position convenient for collecting the flame spectrum.

[0166] S4. Identify the characteristic peak positions of the intermediate products HCl, HBr, and PO· radicals through the computer control and data processing system.

[0167] Then, use the flame retardant component rapid qualitative device described in Embodiment 3 of the present invention to rapidly qualitatively analyze the flame retardant components in textiles. The specific operation steps are as follows.

[0168] First, adjust the lifting plate to raise the sample tank to the upper part of the combustion chamber, take out the sample tank from the combustion chamber through the exhaust port, then add 3 g of the sample to be measured into the sample tank, and then put the sample tank back into the combustion chamber and lower the lifting plate until the sample tank is at the lower edge of the window.

[0169] Then, after the injection is complete, connect the tail gas treatment device to the exhaust port.

[0170] Before the test begins, the movable arm overlaps with the fixed arm. After the test begins, the computer control and data processing system adjusts the movable arm to rotate clockwise, thereby driving the clamping heating element igniter to the top of the sample slot and heating and igniting the sample to be tested. After ignition, the heating is stopped and the movable arm is adjusted to rotate counterclockwise to overlap with the fixed arm. At the same time, the fiber optic spectrometer begins to continuously collect data until the flame spectrum of the sample in a stable combustion state is collected. During this period, the height of the sample slot is adjusted by the lifting plate to reach a position that is convenient for collecting the flame spectrum.

[0171] Finally, the collected combustion flame spectrum of the tested sample is identified and compared through the computer control and data processing system.

[0172] The results of data collection and comparison and identification showed that the combustion flame spectrum of the textile had overlapping peak positions with the flame spectrum curve of the material containing polybrominated biphenyls in the database, and there was a characteristic peak of the intermediate product HBr, indicating that the flame retardant component in the tested sample included brominated flame retardants, which provided direction for the subsequent selection of quantitative detection methods for flame retardants.

[0173] At present, the research on the detection of halogen and phosphorus flame retardants mainly focuses on the investigation of trace pollution in water or soil. The method of combining extraction concentration with mass spectrometry detection is adopted to carry out qualitative and quantitative analysis simultaneously, and the detection limit can be as low as 10 -6 , but the cost is very high, the detection steps are cumbersome, the sample processing process is complicated and time-consuming, the Soxhlet extraction process alone takes 8 to 16 hours, and the requirements and dependence on instruments and equipment are relatively high. In the industrial field, it is necessary to quickly batch test the type and content of flame retardants in materials. In law enforcement inspections, it is also necessary to promptly discover the behavior of using banned flame retardants as green flame retardants in the market to improve product quality. Therefore, it is urgent to develop a fast and effective flame retardant rapid screening technology to simplify acceptance work.

[0174] The flame retardant component rapid qualitative detection method and device based on flame spectrum feature recognition provided by the present invention effectively solve the above problems. The present invention uses a fiber optic spectrometer to identify the spectral characteristics of spontaneous chemiluminescence of the material combustion flame, compares the spectrum library to obtain the information of the intermediate products of the material combustion, and quickly determines whether halogen or phosphorus flame retardants exist in the material by identifying whether HX or PO· free radicals are released during the combustion process and roughly quantifies them by the characteristic peak radiation intensity, providing effective measures for law enforcement inspections to quickly identify the authenticity of green flame retardants in products, and at the same time, providing a fast screening foundation for the subsequent selection of the optimal halogen or phosphorus flame retardant quantitative detection method.

[0175] The invention is quick and effective, has wide sample applicability and strong versatility, and is suitable for screening tests of materials containing more than 0.5% of halogen or phosphorus flame retardants.

[0176] Of course, the above description is not a limitation of the present invention, and the present invention is not limited to the above examples. Changes, modifications, additions or substitutions made by those skilled in the art within the scope of the essence of the present invention should also fall within the protection scope of the present invention.

Claims

1. A rapid qualitative device for flame retardant components, characterized in that, It includes a combustion chamber, a sampling device, an ignition device and a spectral acquisition device. The spectral acquisition device consists of an optical fiber, an optical fiber spectrometer and a computer control and data processing system; Both the sampling device and the ignition device are arranged inside the combustion chamber. The top wall of the combustion chamber is connected to the ignition device. The ignition device is wirelessly connected to the computer control and data processing system. The bottom wall of the combustion chamber is connected to the sampling device; A window for transmitting flame light is provided on the front side wall of the combustion chamber. The end of the optical fiber is directly opposite to the center of the window. A plurality of ventilation holes are provided on the side wall of the combustion chamber below the window. An exhaust port is provided on the top wall of the combustion chamber. The exhaust port is detachably connected to a tail gas treatment device.

2. The rapid qualitative device for flame retardant components according to claim 1, characterized in that, The sampling device includes a lifting plate and a sample tank. The sample tank is connected to the lifting plate through a connecting rod.

3. The rapid qualitative device for the flame retardant composition according to claim 1, characterized in that, The ignition device includes a clamping type heating element igniter, a movable arm and a fixed arm. The top end of the fixed arm is connected to the top wall of the combustion chamber. The bottom end of the fixed arm is pivotally connected to the top end of the movable arm. The bottom end of the movable arm is connected to the clamping type heating element igniter.

4. The rapid qualitative device for flame retardant components according to claim 1, characterized in that, A collimating lens is provided at the end of the optical fiber.

5. The rapid qualitative device for flame retardant components according to any one of claims 1-4, characterized in that, A plurality of the ventilation holes are evenly arranged around the combustion chamber in a circle.

6. The rapid qualitative device for flame retardant components according to claim 5, characterized in that The window is made of quartz glass.

7. The rapid qualitative device for flame retardant components according to claim 6, characterized in that The window is provided at the center of the front side wall of the combustion chamber.

8. The rapid qualitative device for flame retardant components according to claim 7, characterized in that, The movable range of the movable arm is to rotate 180° around the fixed arm on a vertical plane.

9. The rapid qualitative device for the flame retardant composition according to claim 1, characterized in that, The spectral acquisition device is arranged in front of the front side of the combustion chamber.

10. The rapid qualitative device for flame retardant components according to claim 1, wherein, The computer control and data processing system stores a flame spectrum underlying database, a characteristic peak position database and a spectrum comparison and identification algorithm.

11. A rapid qualitative method for flame retardant components, characterized in that Applied to the flame retardant component rapid qualitative device according to any one of claims 2-10, it includes the following steps: S1. Adjust the lifting plate to raise the sample tank to the upper part of the combustion chamber. Take out the sample tank from the combustion chamber through the exhaust port. Then add a liquid or solid sample to be measured into the sample tank. Subsequently, put the sample tank back into the combustion chamber and lower the lifting plate until the sample tank is at the lower edge of the window; S2. Connect the tail gas treatment device to the exhaust port; S3. Start the test. Adjust the ignition device to above the sample tank through the computer control and data processing system and heat to ignite the sample to be measured. After ignition, stop heating and adjust the ignition device away from the sample tank. At the same time, the optical fiber spectrometer starts to continuously collect data until the flame spectrum of the sample in a stable combustion state is collected. During this period, adjust the height of the sample tank through the lifting plate to reach a position convenient for collecting the flame spectrum; S4. Compare and identify through the computer control and data processing system whether there are characteristic peaks of HX or PO· free radicals in the collected combustion flame spectrum of the measured sample. If there is an HX characteristic peak in the combustion flame spectrum of the measured sample, then HX is released during the combustion process of the measured sample, so as to determine that there is a halogen-based flame retardant in the measured sample; if there is a characteristic peak of PO· free radicals in the combustion flame spectrum of the measured sample, then PO· free radicals are released during the combustion process of the measured sample, so as to determine that there is a phosphorus-based flame retardant in the measured sample.

12. The rapid qualitative method for the flame retardant composition according to claim 11, characterized in that, The ignition device includes a clamping type heating element igniter, a movable arm and a fixed arm. The top end of the fixed arm is connected to the top wall of the combustion chamber. The bottom end of the fixed arm is pivotally connected to the top end of the movable arm. The bottom end of the movable arm is connected to the clamping type heating element igniter.

13. The rapid qualitative method for a flame retardant composition according to claim 12, characterized in that, In step S3, before the test starts, the movable arm overlaps with the fixed arm. After the test starts, the movable arm is adjusted to rotate clockwise through the computer control and data processing system, so as to drive the clamping type heating element igniter above the sample tank and heat to ignite the sample to be tested. After ignition, the heating is stopped and the movable arm is adjusted to rotate counterclockwise until it overlaps with the fixed arm.

Images