CN115112787A - Polycyclic aromatic hydrocarbon detection method - Google Patents
Polycyclic aromatic hydrocarbon detection method Download PDFInfo
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- CN115112787A CN115112787A CN202210606738.7A CN202210606738A CN115112787A CN 115112787 A CN115112787 A CN 115112787A CN 202210606738 A CN202210606738 A CN 202210606738A CN 115112787 A CN115112787 A CN 115112787A
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- 239000002904 solvent Substances 0.000 claims abstract description 5
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/08—Preparation using an enricher
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
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Abstract
The invention relates to the technical field of chemical analysis, in particular to a polycyclic aromatic hydrocarbon detection method, which mainly solves the problem of low accuracy of detection of polycyclic aromatic hydrocarbon content in smoke after burning of aromatic hydrocarbon in the prior art, and comprises the following steps: removing the core of the incense, crushing the incense by a crusher, and pressing the incense into a strip sample in a die; putting the sample in a closed space for ignition, and collecting smoke volatilized from the air through a smoke collector; adding the roasted anhydrous sodium sulfate and the copper powder, mixing uniformly, adding a mixed solution of n-hexane and acetone, and continuously extracting with 125mL of dichloromethane for 36 hours; performing rotary evaporation and concentration to 5 mL; purifying with alumina and silica gel chromatography column, concentrating the eluate, replacing solvent, transferring into 2mL sampling bottle, and blowing to 0.2mL with nitrogen; and (3) detecting the product in the step 5 by using a gas chromatography-mass spectrometer.
Description
Technical Field
The invention relates to the technical field of chemical analysis, in particular to a polycyclic aromatic hydrocarbon detection method.
Background
Polycyclic Aromatic Hydrocarbons (PAHs) are volatile Hydrocarbons produced when organic substances such as coal, petroleum, wood, tobacco, organic high molecular compounds and the like are incompletely combusted, and are important environmental and food pollutants. More than 200 PAHs have been discovered so far, and many of the PAHs have strong carcinogenicity, teratogenicity and mutagenicity and have immunotoxicity; when a person inhales and is exposed to smoke containing high-concentration PAHs for a long time, the incidence of lung cancer, gastric cancer, skin cancer, bladder cancer, scrotal cancer and the like is increased greatly, and meanwhile, lymphatic tissues are atrophied, and the immunity of the organism is reduced. It is inferred that approximately 75-90% of human cancers are caused by the ingestion of PAHs, a significant proportion of which are caused by inhalation through the respiratory tract. The PAHs are difficult to discover the carcinogenicity of the human body, and the average incubation period of the PAHs is as long as 21 years. The U.S. environmental agency EPA 610 has explicitly listed a list of 16 polycyclic aromatic hydrocarbons.
In addition, there are reports in the literature that incense releases various air pollutants such as particulate matter, formaldehyde, benzene series, Polycyclic Aromatic Hydrocarbons (PAHs), and the like. The existing incense standards mainly comprise GB 26386-2011 general technical conditions for safety of incense products and GB/T26393-2011 testing methods for harmful substances of incense products, but both of the two standards do not relate to the detection requirement of the content of polycyclic aromatic hydrocarbon in smoke after the incense is burnt.
The detection of polycyclic aromatic hydrocarbon in incense by the existing incense manufacturers is mostly adopted, such as Chinese patent application numbers: 201610551686.2 discloses a polycyclic aromatic hydrocarbon detection method, which comprises the following steps: 1) extracting and taking a solid sample to be crushed or a crushed solid sample, adding a weak polar solvent with the mass volume of 5-10 times of that of the sample for extraction, adding the weak polar solvent with the mass volume of 5 times of that of the sample for dissolving or taking a liquid oily sample after concentrating an extracting solution to be dry, and directly adding the weak polar solvent with the mass volume of 5-10 times of that of the sample for extraction; 2) acidifying and removing impurities, adding a sulfuric acid solution with the concentration of 50% -80% which is 0.5-1 time of the volume of the solution obtained in the step 1 into the solution prepared in the step 1, fully shaking, and standing to stratify; after passing through a microporous filter membrane, carrying out mass spectrum detection on the upper organic phase; 3) weighing a reference substance with a known concentration in the acidification treatment, dissolving the reference substance by using an organic solvent, adding a sulfuric acid solution with the concentration of 50% -80% and the volume of 0.1-0.2 time that of the reference substance, fully shaking, standing for layering, and allowing an upper organic phase to pass through a microporous filter membrane for mass spectrum detection; 4) and (3) gas chromatography mass spectrometry detection, namely simultaneously detecting the substances obtained in the step (2) and the step (3) by using the gas chromatography mass spectrometry, and carrying out quantitative analysis by using an external standard method to obtain a detection result. The method adopts 5-10 times of organic phase solvent (normal hexane, cyclohexane or petroleum ether) with similar polarity to polycyclic aromatic hydrocarbon for extraction, and reduces the interference of polar components in the sample on detection. The sample is acidized by sulfuric acid with certain concentration (50-80%) and a certain amount (0.5-1.0 mL), so that the sample is simple in pretreatment, easy to operate, low in cost and obvious in impurity removal effect, and meanwhile, the ionization efficiency of the polycyclic aromatic hydrocarbon during mass spectrometry is improved by acidizing, and the sensitivity of the mass spectrometry on the detection of 4 polycyclic aromatic hydrocarbons is effectively improved. The standard substance is also acidified by using a certain concentration and a certain amount of sulfuric acid, so that the standard substance and the sample have the same ionization efficiency during mass spectrometry, and the consistency of the influence of the sample acidification impurity removal process on 4 kinds of polycyclic aromatic hydrocarbon during mass spectrometry is ensured.
However, the method has low accuracy in detecting the content of the polycyclic aromatic hydrocarbon in smoke after burning of the fuel, is only used as a reference, and cannot be popularized and used.
Disclosure of Invention
Therefore, aiming at the problems, the invention provides a method for detecting polycyclic aromatic hydrocarbon, which mainly solves the problem that the accuracy of detecting the content of the polycyclic aromatic hydrocarbon in smoke after burning the aromatic hydrocarbon is low in the prior art.
In order to realize the purpose, the invention adopts the following technical scheme:
a detection method of polycyclic aromatic hydrocarbon comprises the following steps:
1) removing the core of the incense, crushing the incense by using a crusher, filtering and screening particles with uniform diameters, fully shaking the particles uniformly, measuring 0.78-0.82 g of the particles, and pressing the particles in a mold to prepare a strip-shaped sample;
2) putting a sample in a closed space for ignition, enabling gas in the closed space to circularly flow through a smoke collector, collecting smoke volatilized in the air through the smoke collector, sealing a glass test tube by using 15L of smoke with the flow of 0.6L/min through the smoke collector, and storing in a refrigerator at the temperature of-13 ℃;
3) adding roasted anhydrous sodium sulfate and copper powder, mixing, adding 200mL of mixed solution of n-hexane and acetone at a ratio of 1:1, wrapping with extracted filter paper, and continuously extracting with 125mL of dichloromethane for 36 h;
4) concentrating to 5mL by rotary evaporation;
5) purifying with alumina and silica gel chromatography column, concentrating the eluate, replacing solvent, transferring into 2mL sampling bottle, and blowing to 0.2mL with nitrogen;
6) and (4) placing the product in the step (5) in a gas chromatography-mass spectrometer for detection, wherein a chromatographic column of the gas chromatography-mass spectrometer adopts a capillary column HP-5MS, an ion source is an EI source, and the temperature is 300 ℃.
Further, in the step 5, after the aluminum oxide and the silica gel are extracted by dichloromethane for 72 hours, the aluminum oxide and the silica gel are respectively activated at 130 ℃ and 450 ℃ for 24 hours, and then the aluminum oxide and the silica gel are cooled to normal temperature, and then ultrapure water with the mass percent of 3% of the aluminum oxide and the silica gel is added for deactivation, and then n-hexane is added and stored in a dryer for standby.
Further, the analysis program of the gas chromatography-mass spectrometer in the step 6 is that the flow rate of carrier He is 1mL/min, the sample injection amount is 1 muL, the temperature of a sample injection port is 280 ℃, and split-flow sample injection is not carried out; the temperature programming is to start at 50 deg.C, keep for 1min, raise 20 deg.C/min to 200 deg.C, then raise 10 deg.C/min to 290 deg.C, keep for 15 min.
Furthermore, the closed space is provided with an inlet positioned on the left side and an outlet positioned on the lower end, and an air deflector is arranged in the closed space and on the right side.
Furthermore, the air deflector is of an arc-shaped structure, and the concave surface of the air deflector faces the left side.
Furthermore, the smoke collector comprises a shell, the shell is provided with an air inlet, an air outlet and an inner cavity connected with the air inlet and the air outlet, the air inlet and the air outlet are respectively detachably connected with an air inlet pipe and an air outlet pipe, the air inlet pipe is communicated with the outlet, the air outlet pipe is communicated with the inlet, the inner cavity comprises a gas collecting cavity and a balance cavity, a connector is arranged at the balance cavity, the connecting port is detachably connected with a connecting pipe, the other end of the connecting pipe is connected with an air inlet pipe through a tee joint, a pressure regulating valve is arranged on the connecting pipe, a quartz fiber filter membrane is arranged between the gas collection cavity and the balance cavity, the air inlet pipe is provided with a pumping device, the pumping flow rate of the pumping device is 0.6L/min, the air inlet is provided with a switch valve, the air outlet is provided with a flow speed regulating valve, and the flow speed of the flow speed regulating valve is 0.35L/min.
Further, the flow rate regulating valve comprises a first valve body, a first flow channel located in the first valve body, a first valve seat, a first valve rod and a plug, the first valve body comprises a first portion and a second portion, the first portion and the second portion are connected with a rotating portion in a clamping mode to achieve relative rotation, a threaded sleeve is embedded in the first portion and connected with the rotating portion in a threaded mode, the first valve rod is fixedly arranged on the threaded sleeve, the plug is arranged on the first valve rod, and the rotating portion is rotated to drive the threaded sleeve to move along the axial direction of the first portion, so that the first valve rod drives the plug to be matched with the valve seat to adjust the flow area of the first flow channel.
Furthermore, the pressure regulating valve comprises a second valve body, a second flow passage located in the second valve body, a second valve seat arranged on the second flow passage, a second valve rod and balls, a through hole communicated with the second flow passage is formed in the second valve seat, the balls are abutted against the through hole, an adjusting rod is arranged on the second valve body, a worm is arranged on the adjusting rod, a worm wheel meshed with the worm is arranged at the upper end of the second valve rod, the second valve rod is in threaded connection with the second valve seat, a top plate is arranged at the lower end of the second valve rod, a spring is arranged between the top plate and the balls, the top plate is driven to move through the second valve rod by rotating the adjusting rod, the distance between the top plate and the balls is adjusted, and the compression stroke of the spring is changed.
By adopting the technical scheme, the invention has the beneficial effects that: this polycyclic aromatic hydrocarbon's detection method, reduce the unnecessary impurity in the burning incense combustion process, improve burning incense's combustion efficiency and burning quality, volatile smog is abundant in the assurance burning, and through the better smog of collecting burning incense burning of smoke collector, through filtering the composition that diffuses in smog and the air, rethread cold is preserved and is realized the composition in the air and subsides, improve the efficiency of collecting the product thing after burning incense burning, through the volatile dual collection mode of filtration and air, the problem that it is difficult to comparatively comprehensive collection to diffuse smog in the air has been solved, and through foretell preparation step, the interference of false positive is difficult to appear, improve the accuracy of testing result, the sensitivity of detection is high.
Drawings
FIG. 1 is a schematic structural diagram of an embodiment of the present invention;
FIG. 2 is a schematic view, partly in section, of a smoke collector in an embodiment of the invention;
FIG. 3 is a schematic sectional view of a flow rate regulating valve according to an embodiment of the present invention;
fig. 4 is a schematic sectional structure view of the pressure regulating valve in the embodiment of the invention.
Detailed Description
The invention will now be further described with reference to the accompanying drawings and detailed description.
The embodiment of the invention is as follows:
a detection method of polycyclic aromatic hydrocarbon comprises the following steps:
1) removing the core of the incense, crushing the incense by using a crusher, filtering and screening particles with uniform diameters, fully shaking the particles uniformly, measuring 0.78-0.82 g of the particles, and pressing the particles in a mold to prepare a strip-shaped sample;
2) putting a sample in a closed space 1 for ignition, enabling gas in the closed space to circularly flow through a smoke collector 3, collecting smoke volatilized in the air through the smoke collector 3, sealing a glass test tube by using 15L of smoke with the flow of 0.6L/min through the smoke collector 3, and storing in a refrigerator at-13 ℃;
3) placing the roasted anhydrous sodium sulfate and the copper powder, mixing uniformly, adding 200mL of mixed solution of n-hexane and acetone in a ratio of 1:1, wrapping the sample with extracted filter paper, and continuously extracting with 125mL of dichloromethane for 36 hours;
4) concentrating to 5mL by rotary evaporation;
5) purifying by using alumina and silica gel chromatographic column chromatography, transferring a leacheate into a 2mL sample injection bottle after concentrating and replacing a solvent, blowing 0.2mL with nitrogen, extracting the alumina and the silica gel by using dichloromethane for 72h, respectively activating at 130 ℃ and 450 ℃ for 24h, cooling to normal temperature, adding ultrapure water with the mass of 3% of that of the alumina and the silica gel for deactivation, adding n-hexane, and storing in a dryer for later use;
6) placing the product in the step 5 in a gas chromatography-mass spectrometer for detection, wherein a capillary column HP-5MS is adopted as a chromatographic column of the gas chromatography-mass spectrometer, an ion source is an EI source, the temperature is 300 ℃, and the analysis program of the gas chromatography-mass spectrometer is that the flow rate of carrier He is 1mL/min, the sample injection amount is 1 mu L, the sample injection port temperature is 280 ℃, and no-flow sampling is carried out; the temperature programming is to start at 50 deg.C, keep for 1min, raise to 200 deg.C at 20 deg.C/min, then raise to 290 deg.C at 10 deg.C/min, keep for 15 min.
This polycyclic aromatic hydrocarbon's detection method, reduce the unnecessary impurity in the burning process of burning incense, improve the combustion efficiency and the burning quality of burning incense, it is abundant to guarantee the smog that volatilizees in the burning, and through the smog collector better smog of collecting burning incense burning, through filtering the composition that diffuses in smog and the air, the composition in the rethread cold storage realization air subsides, realize burning incense abundant collection of back smog, through the filtration and the volatile dual mode of collecting of air, the problem that the smog is difficult to comparatively comprehensive collection in the air has been solved, and through foretell preparation step, the interference of false positive is difficult to appear, improve the accuracy of testing result, the sensitivity of detection is high.
In this embodiment, referring to fig. 1, the enclosed space 1 has an inlet 11 located on the left side and an outlet 12 located at the lower end, the air deflector 2 is disposed in the enclosed space and located on the right side, the air deflector 2 is in an arc structure, a concave surface of the air deflector 2 faces the left side, specifically, the air deflector 2 includes a first arc portion 21 and a second arc portion 22, an area size of the first arc portion 21 is smaller than an area size of the second arc portion 22, a curvature radius of the first arc portion 21 is smaller than a curvature radius of the second arc portion 22, the first arc portion 21 is located on the left side of the second arc portion 22 and is distributed at intervals, so that a channel 23 is formed between the first arc portion 21 and the second arc portion 22, air holes 24 are disposed on the first arc portion 21, when in use, an air flow enters from the left side to the right side through the inlet 11, and further drives smoke in the air to move, and the smoke is guided into the outlet 12 through the channel 23 on the guide plate 2 and discharged, the opening at the upper part of the guide plate can be guided into the channel 23 in the air flow through the arrangement of the first arc-shaped part 21 and the second arc-shaped part 22, the adsorption effect can be better formed due to the pressure difference caused by the concentrated flow when the burning of the burning incense is shortened, and meanwhile, the smoke diffused in the closed space is better and intensively discharged through the adsorption effect of the air holes 24, so that the collection and detection of the smoke are facilitated.
In addition, referring to fig. 1 and fig. 2, the smoke collector 3 includes a housing 31, the housing 31 has an air inlet 32, an air outlet 33, and an inner cavity connecting the air inlet 32 and the air outlet 33, the air inlet 32 and the air outlet 33 are detachably connected to an air inlet pipe 34 and an air outlet pipe 35, the air inlet pipe 34 is communicated with the outlet 12, the air outlet pipe 35 is communicated with the inlet 11, the inner cavity includes a gas collecting cavity 36 and a balance cavity 37, a connection port 38 is disposed at the position of the balance cavity 36, the connection port 38 is detachably connected to a connection pipe 39, the other end of the connection pipe 39 is connected to the air inlet pipe 34 through a tee joint, a pressure regulating valve 4 is disposed on the connection pipe 39, a quartz fiber filter membrane 5 is disposed between the gas collecting cavity 36 and the balance cavity 37, a pumping device 6 is disposed on the air inlet pipe 34, and the pumping flow rate of the pumping device 6 is 0.6L/min, the air inlet 32 is provided with a switch valve 7, the air outlet 33 is provided with a flow rate adjusting valve 8, the flow rate of the flow rate adjusting valve 8 is 0.35L/min, the smoke in the closed space 1 is driven to flow through the particle collection of the smoke collector 3 and the smoke collection diffused in the air by the pumping action of the pumping device 6, the closed space 1 and the smoke collector 3 form a circulating flow system, the smoke is collected in an gathering manner, the particle collection can be realized while the particles are filtered by the pumping flow rate of the pumping device 6 and the flow rate difference of the flow rate adjusting valve 8, the subsequent detection accuracy is guaranteed, meanwhile, the particles of the quartz fiber filter membrane 5 are blocked during the filtration to cause the pressure difference at two sides of the quartz fiber filter membrane 5, and the air consumed by the burning incense in the combustion process to cause the pressure reduction in the closed space 1, therefore, the filtering effect of the quartz fiber filter membrane 5 is ensured through the pumping flow rate of the pumping device 6 and the flow rate difference of the flow rate regulating valve 8 and the pressure regulating valve 4 arranged on the connecting pipe 39 and the connecting pipe 39, the pressure difference in the gas collection cavity 36, the balance cavity 37 and the closed space 1 is kept, the flow guidance property of smoke and the filtering effect are ensured, and meanwhile, when the air-conditioning device is used, the switch valve 7 is closed and is detached from the air inlet pipe 34 and the air outlet pipe 35, so that the shell 31 forms an air outlet cavity, a transfer storage can be formed well, the use convenience is improved, and the operation difficulty is reduced.
In order to improve the filter effect of quartz fiber filter membrane, be equipped with filtering support 9 in the casing 31, filtering support 9 filters supporting part 92 and the third of connecting first filtering supporting part 91 and second filtering supporting part 92 and filters supporting part 93 including the first supporting part 91 that filters that is the loop configuration, the second that is circular arc structure, third filtering supporting part 93 is the radius platform structure, quartz fiber filter membrane 5 covers on filtering support 9, has reduced the granule in the smog filtration from this and has blockked up quartz fiber filter membrane 5 and cause filtration efficiency to reduce by a wide margin, and simultaneously, in filtering process, when air impact second filters supporting part 92, plays the water conservancy diversion effect by it, better flow in first filtering supporting part 91 department and third filtering supporting part 93 department, reduce the noise.
Specifically, referring to fig. 3, the flow rate adjusting valve 8 includes a first valve body 81, a first flow channel 82 located in the first valve body 81, a first valve seat 83 disposed on the first flow channel 82, a first valve rod 84, and a plug 85, where the first valve body 81 includes a first portion 811 and a second portion 812, the first portion 811 and the second portion 812 are connected to the rotating portion 86 in a clamped manner to realize relative rotation, a threaded sleeve 87 is embedded in the first portion 811, the threaded sleeve 87 is connected to the rotating portion 86 in a threaded manner, the first valve rod 84 is fixedly disposed on the threaded sleeve 87, the plug 85 is disposed on the first valve rod 84, and the rotating portion 86 is rotated to drive the threaded sleeve 87 to move along the axial direction of the first portion 811, so that the plug 85 is driven by the first valve rod 84 to cooperate with the first valve seat 83 to adjust the flow area of the first flow channel 82.
Referring to fig. 4, the pressure regulating valve 4 includes a second valve body 41, a second flow passage 42 in the second valve body 41, a second valve seat 43 provided on the second flow passage 42, a second stem 44, and a ball 45, a through hole 46 communicated with the second flow passage 42 is arranged on the second valve seat 43, the ball 45 is abutted against the through hole 46, an adjusting rod 47 is arranged on the second valve body 41, a worm 48 is arranged on the adjusting rod 47, the second valve rod 44 is provided at an upper end thereof with a worm wheel 49 engaged with the worm 48, the second valve rod 44 is screw-coupled with the second valve seat 43, a top plate 50 is provided at the lower end of the second valve rod 44, a spring 60 is provided between the top plate 50 and the ball 45, and by rotating the adjusting rod 47, the second valve rod 44 drives the top plate 50 to move, and the distance between the top plate 50 and the ball 45 is adjusted, so that the compression stroke of the spring 60 is changed.
While the invention has been particularly shown and described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (8)
1. A polycyclic aromatic hydrocarbon detection method is characterized in that: the method comprises the following steps:
1) crushing the incense by a crusher after coring, filtering and screening particles with uniform diameters, fully shaking uniformly, measuring 0.78-0.82 g, and pressing in a die to form a strip sample;
2) putting a sample in a closed space for ignition, enabling gas in the closed space to circularly flow through a smoke collector, collecting smoke volatilized in the air through the smoke collector, sealing a glass test tube by 15L of smoke with the flow of 0.6L/min through the smoke collector, and storing in a refrigerator at-13 ℃;
3) adding roasted anhydrous sodium sulfate and copper powder, mixing, adding 200mL of mixed solution of n-hexane and acetone at a ratio of 1:1, wrapping with extracted filter paper, and continuously extracting with 125mL of dichloromethane for 36 h;
4) concentrating to 5mL by rotary evaporation;
5) purifying with alumina and silica gel column chromatography, concentrating the eluate, replacing solvent, transferring into 2mL sampling bottle, and blowing to 0.2mL with nitrogen;
6) and (3) placing the product obtained in the step (5) in a gas chromatography-mass spectrometer for detection, wherein a capillary column HP-5MS is adopted as a chromatographic column of the gas chromatography-mass spectrometer, an EI source is used as an ion source, and the temperature is 300 ℃.
2. The method for detecting polycyclic aromatic hydrocarbons according to claim 1, wherein: in the step 5, the alumina and the silica gel are extracted by dichloromethane for 72 hours, then are respectively activated at 130 ℃ and 450 ℃ for 24 hours, are cooled to normal temperature, are added with ultrapure water with the mass percent of 3% for deactivation, are added with n-hexane and are stored in a dryer for standby.
3. The method for detecting polycyclic aromatic hydrocarbons according to claim 1, wherein: the analysis program of the gas chromatography-mass spectrometer in the step 6 is that the flow rate of carrier He is 1mL/min, the sample injection amount is 1 mu L, the temperature of a sample injection port is 280 ℃, and split-flow sample injection is not carried out; the temperature programming is to start at 50 deg.C, keep for 1min, raise 20 deg.C/min to 200 deg.C, then raise 10 deg.C/min to 290 deg.C, keep for 15 min.
4. The method for detecting polycyclic aromatic hydrocarbons according to any one of claims 1 to 3, wherein: the closed space is provided with an inlet positioned on the left side and an outlet positioned on the lower end, and an air deflector is arranged in the closed space and on the right side.
5. The method for detecting polycyclic aromatic hydrocarbons according to claim 4, wherein: the air deflector is of an arc-shaped structure, and the concave surface of the air deflector faces the left side.
6. The method for detecting polycyclic aromatic hydrocarbons according to claim 4, wherein: the smoke collector comprises a shell, the shell is provided with an air inlet, an air outlet and an inner cavity for connecting the air inlet and the air outlet, the air inlet and the air outlet are respectively detachably connected with an air inlet pipe and an air outlet pipe, the air inlet pipe is communicated with the outlet, the air outlet pipe is communicated with the inlet, the inner cavity comprises a gas collecting cavity and a balance cavity, a connector is arranged at the balance cavity, the connecting port is detachably connected with a connecting pipe, the other end of the connecting pipe is connected with an air inlet pipe through a tee joint, a pressure regulating valve is arranged on the connecting pipe, a quartz fiber filter membrane is arranged between the gas collection cavity and the balance cavity, the air inlet pipe is provided with a pumping device, the pumping flow rate of the pumping device is 0.6L/min, the air inlet is provided with a switch valve, the air outlet is provided with a flow speed regulating valve, and the flow speed of the flow speed regulating valve is 0.35L/min.
7. The method for detecting polycyclic aromatic hydrocarbons according to claim 6, wherein: the flow rate regulating valve comprises a first valve body, a first flow channel located in the first valve body, a first valve seat, a first valve rod and a plug, wherein the first valve body comprises a first portion and a second portion, the first portion and the second portion are connected with a rotating portion in a clamping mode to achieve relative rotation, a threaded sleeve is embedded in the first portion and is connected with the rotating portion in a threaded mode, the first valve rod is fixedly arranged on the threaded sleeve, the plug is arranged on the first valve rod, the rotating portion rotates to drive the threaded sleeve to move along the axial direction of the first portion, and then the first valve rod drives the plug to be matched with the valve seat to adjust the flow area of the first flow channel.
8. The method for detecting polycyclic aromatic hydrocarbons according to claim 7, wherein: the pressure regulating valve comprises a second valve body, a second flow channel located in the second valve body, a second valve seat arranged on the second flow channel, a second valve rod and balls, wherein a through hole communicated with the second flow channel is formed in the second valve seat, the balls are abutted against the through hole, an adjusting rod is arranged on the second valve body, a worm is arranged on the adjusting rod, a worm wheel meshed with the worm is arranged at the upper end of the second valve rod, the second valve rod is in threaded connection with the second valve seat, a top plate is arranged at the lower end of the second valve rod, a spring is arranged between the top plate and the balls, the top plate is driven to move through the second valve rod by rotating the adjusting rod, the distance between the top plate and the balls is adjusted, and the compression stroke of the spring is changed.
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