CN111983115A - Method for detecting VOCs in air - Google Patents
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- CN111983115A CN111983115A CN202010860923.XA CN202010860923A CN111983115A CN 111983115 A CN111983115 A CN 111983115A CN 202010860923 A CN202010860923 A CN 202010860923A CN 111983115 A CN111983115 A CN 111983115A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention belongs to the technical field of volatile organic compound detection, and discloses a method for detecting VOCs in air, which comprises the steps of determining the position of a sampling point, collecting an air sample, and collecting VOCs by using a pump to make the air sample pass through an adsorbent; enriching the collected VOCs by an in-air VOCs adsorption treatment device; analyzing the components and the concentration of the VOCs in the air by adopting a GC-FID/MS coupling technology on the enriched VOCs sample; analyzing the formaldehyde content in the indoor air by an acetylacetone spectrophotometry; preparing a standard sample solution of various volatile compounds, drawing a standard curve, and analyzing the sample enriched with the VOCs to obtain a corresponding detection result. The detection method disclosed by the invention has the advantages of higher accuracy, good repeatability, lower detection limit, no need of processing the sample, low requirement on the collected air sample, simplicity, avoidance of repeated sampling, simplification of detection steps and high sensitivity.
Description
Technical Field
The invention belongs to the technical field of volatile organic compound detection, and particularly relates to a method for detecting VOCs in air.
Background
At present, Volatile Organic Compounds (VOCs) are precursors for forming photochemical smog, ozone and secondary organic aerosol and bring serious influence on human health and natural ecological environment.
Through the above analysis, the problems and defects of the prior art are as follows: the existing detection method has high requirements on samples, the samples need to be preprocessed, the detection process is complicated, the hysteresis quality is achieved, and meanwhile, the detection result is influenced by other factors and is inaccurate in detection.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method for detecting VOCs in air.
The invention is realized in this way, a method for detecting VOCs in air, which comprises the following steps:
determining the position of a sampling point, collecting an air sample by a TH-3000BIV ambient air sampler by using an instantaneous sampling method, closing a valve after the pressure in the ambient air sampler is consistent with the atmospheric pressure of the sampling point, sealing by using a sealing cap, and recording the ambient temperature and the atmospheric pressure of the sampling point; meanwhile, a pump is used for collecting VOCs from an air sample through the adsorbent.
And step two, setting numerical values of an organic waste gas concentration sensor and an air quantity sensor of the VOCs adsorption treatment device in the air through an external controller, and starting an air inlet fan to suck the air to be enriched into the device after a heating net is preheated for 20-25 min by electrifying.
And step three, enabling the collected VOCs to pass through a high-voltage electric field of 12000-20000V of the VOCs adsorption treatment device, simultaneously utilizing an ultraviolet lamp of an ultraviolet generating device to emit ultraviolet light, and irradiating the ultraviolet light emitted by the ultraviolet lamp on a photocatalyst on the surface of the activated carbon adsorption layer in a gathering mode at a specific distance by means of a light gathering device to perform catalytic ionization of gas molecules.
Fourthly, ions generated by catalytic ionization are attached to aerosol particles and are descended to a collector under the action of an electric field; and finally, washing down the sediment on the surface of the collector to obtain the enriched VOCs sample.
And fifthly, analyzing the components and the concentration of the VOCs in the air by adopting a GC-FID/MS combined technology on the enriched VOCs sample.
Taking a 25mL pipette, measuring 25mL ultrapure water, adding the ultrapure water into an absorption tube, and placing the ultrapure water into an insulation box; 5mL of sample to be tested is taken to analyze the content of formaldehyde in the indoor air by an acetylacetone spectrophotometry method.
Step seven, preparing standard sample solutions of various volatile compounds: at the room temperature of 20-25 ℃, 1 1.5mL agilent sample introduction bottle is taken, and a pipette is used for adding 1.0mLCS2Covering and sealing; a standard application solution was prepared by injecting 10.0. mu.L of 0.770g/mL methylcyclohexane, 0.902g/mL ethyl acetate, 0.805g/mL butanone, 0.878g/mL benzene, 0.940g/mL ethyl acrylate, 0.799g/mL methyl isobutyl ketone, 0.867g/mL toluene, 0.867g/mL ethylbenzene, 0.861g/mL p-xylene, 0.880g/mL o-xylene, 0.906g/mL styrene, and 0.947g/mL cyclohexanone in this order into a pure material of all VOCs present in the air using a micro-syringe.
Step eight, drawing a standard curve: taking 5 1.5mL sampling bottles, accurately adding 1.0mL CS respectively by a pipette2Immediately sealing and pressing by a silicon rubber spacer and sealing by a cover; injecting 5.0, 10.0, 15.0, 20.0 and 25.0 microliter of standard application liquid into a microinjector to prepare a standard series, and placing the standard series into a thermal desorption instrument to measure the volatile organic compounds in the air.
Step nine, drawing a standard curve based on the retention time and concentration series of the compound obtained by the determination in the step eight; and analyzing the sample enriched with the VOCs by adopting a thermal desorption-gas mass combination method based on the drawn standard curve to obtain a corresponding detection result.
Further, in the first step, the conditions for collecting the air sample by adopting the TH-3000BIV ambient air sampler are as follows: the sampling flow is set to be 30-45 ml/min, and the sampling time is set to be 10-20 min.
Further, in the first step, the adsorbent is Tenax or activated carbon.
Further, in the second step, the organic waste gas concentration sensor and the air volume sensor are both electrically connected with an external controller, the model of the organic waste gas concentration sensor is PID-A1, and the model of the air volume sensor is KGF 2.
Further, in the third step, the surface of the activated carbon adsorption layer is coated with a photocatalyst, and the photocatalyst is nano titanium dioxide.
Further, in the third step, before the enrichment of the sample of the VOCs, a water removal operation is also included; the method for removing water comprises the following steps:
and a plurality of stages of cold traps connected in series are used, and the temperature of the first cold trap is slowly increased when the target compound is transferred from the previous cold trap to the next extremely cold trap so as to prevent the transfer of water vapor.
Further, in step eight, the thermal desorption conditions are as follows: the temperature of the transmission line is 100 ℃, and the temperature of the valve is 260 ℃; carrying out dry blowing on the sampling tube for 4-8 min, and carrying out desorption at 290 ℃, wherein the desorption time is 4-6 min, and the desorption flow is 30 mL/min; and (3) raising the temperature of the cold trap from room temperature to 260 ℃ at the maximum temperature rise rate, and then keeping the temperature for 3-5 min, wherein the resolving flow of the cold trap is 18 mL/min.
Further, in the ninth step, the conditions of the gas chromatograph-mass spectrometer are as follows: the sample introduction temperature is set to be 180 ℃, the transmission lead is set to be 100 ℃, the ion source is set to be 280 ℃, and the mass ratio of the sample introduction temperature to the transmission lead is set to be 20: 1, and setting the delay time of the solvent retarder to be 60-80 s.
Further, setting the initial column temperature to be 25 ℃ and maintaining for 4-8 min; then increasing the column temperature to 320 ℃ at the speed of 8 ℃/min and then maintaining for 4-8 min; helium was passed at a rate of 1mL/min as a carrier gas.
Further, in the ninth step, the method for detecting the sample enriched with the VOCs by using the thermal desorption-gas mass spectrometry method further includes:
and matching the detected result with data in a database after thermal desorption-gas chromatography-mass spectrometry detection, wherein the substances with the similarity of more than 70 percent are effective substances.
By combining all the technical schemes, the invention has the advantages and positive effects that: the detection method disclosed by the invention has the advantages of higher accuracy, good repeatability, lower detection limit, no need of processing the sample, no high requirement on the collected air sample, simplicity, comprehensive and accurate detection of the components and the concentration of the detected VOCs, and improvement on the accuracy of an evaluation conclusion. The invention avoids repeated sampling for many times, simplifies the detection steps and has high sensitivity. The invention is matched with a TH-3000BIV ambient air sampler for sampling, and an acetylacetone spectrophotometry is used for analyzing the formaldehyde content in the indoor air, so that compared with the prior art, the data integrity of the invention is better, and more detailed scientific basis is provided for comprehensively reflecting the pollution characteristics of VOCs in the indoor air.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings needed to be used in the embodiments of the present application will be briefly described below, and it is obvious that the drawings described below are only some embodiments of the present application, and it is obvious for those skilled in the art that other drawings can be obtained from the drawings without creative efforts.
Fig. 1 is a flowchart of a method for detecting VOCs in air according to an embodiment of the present invention.
Fig. 2 is a flowchart of a method for determining a sampling point position and collecting an air sample according to an embodiment of the present invention.
Fig. 3 is a flowchart of a method for enriching collected VOCs by an adsorption processing device for VOCs in air according to an embodiment of the present invention.
Fig. 4 is a flowchart of a method for drawing a standard curve according to an embodiment of the present invention.
FIG. 5 is a flow chart of a method for preparing a standard application solution according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In view of the problems in the prior art, the present invention provides a method for detecting VOCs in air, which is described in detail below with reference to the accompanying drawings.
As shown in fig. 1, a method for detecting VOCs in air according to an embodiment of the present invention includes:
and S101, determining the position of a sampling point, collecting an air sample, and collecting VOCs (volatile organic compounds) of the air sample through an adsorbent by using a pump.
And S102, enriching the collected VOCs by the VOCs adsorption treatment device in the air.
And S103, analyzing the components and the concentration of the VOCs in the air by adopting a GC-FID/MS combined technology on the enriched VOCs sample.
S104, taking a 25mL pipette, measuring 25mL ultrapure water, adding the ultrapure water into an absorption tube, and placing the ultrapure water into an insulation box; 5mL of sample to be tested is taken to analyze the content of formaldehyde in the indoor air by an acetylacetone spectrophotometry method.
And S105, preparing standard sample solutions of various volatile compounds and drawing a standard curve.
And S106, based on the drawn standard curve, determining the volatile organic compounds in the VOCs sample by adopting a thermal desorption-gas mass spectrometry method, and obtaining a corresponding detection result.
As shown in fig. 2, in step S101, the method for determining a sampling point position and collecting an air sample includes:
s201, determining the position of a sampling point, and collecting an air sample by a TH-3000BIV ambient air sampler by using an instantaneous sampling method.
S202, after the pressure in the ambient air sampler is consistent with the atmospheric pressure of the sampling point, closing the valve, sealing the valve by using a sealing cap, and recording the ambient temperature and the atmospheric pressure of the sampling point.
And S203, simultaneously, carrying out VOCs collection on the air sample through the adsorbent by using a pump.
In step S201 provided in the embodiment of the present invention, the conditions for collecting the air sample by using the TH-3000BIV ambient air sampler are as follows: the sampling flow is set to be 30-45 ml/min, and the sampling time is set to be 10-20 min.
In step S201 provided in the embodiment of the present invention, the adsorbent is Tenax or activated carbon.
As shown in fig. 3, in step S102, the method for performing enrichment processing on collected VOCs by using an adsorption processing apparatus for VOCs in air according to an embodiment of the present invention includes:
s301, setting numerical values of an organic waste gas concentration sensor and an air quantity sensor of the VOCs adsorption treatment device in the air through an external controller, preheating a heating net for 20-25 min after electrifying, and starting an air inlet fan to suck air to be enriched into the device.
S302, enabling the collected VOCs to pass through a high-voltage electric field of a VOCs adsorption treatment device 12000-20000V, emitting ultraviolet light by an ultraviolet lamp of an ultraviolet generating device, and irradiating the ultraviolet light emitted by the ultraviolet lamp on a photocatalyst on the surface of an activated carbon adsorption layer in a gathering mode at a specific distance by means of a light gathering device to perform catalytic ionization of gas molecules.
S303, ions generated by catalytic ionization are attached to aerosol particles and are descended to a collector under the action of an electric field; and finally, washing down the sediment on the surface of the collector to obtain the enriched VOCs sample.
As shown in fig. 4, in step S105 provided in the embodiment of the present invention, the method for drawing the standard curve includes:
s401, taking 5 1.5mL sampling bottles, accurately adding 1.0mLCS by a pipette respectively2Immediately, the sealing and pressing of the silicon rubber spacer and the sealing of the cover are carried out.
S402, injecting 5.0, 10.0, 15.0, 20.0 and 25.0 mu L of standard application liquid into the micro-injector in sequence to prepare a standard series, and placing the standard series into a thermal desorption instrument to measure the volatile organic compounds in the air.
And S403, drawing a standard curve based on the retention time and concentration series of the measured compounds.
As shown in fig. 5, in step S105 provided in the embodiment of the present invention, the preparation method of the standard application solution includes:
s501, taking 1 1.5mL Agilent sample introduction bottle at room temperature of 20-25 ℃, and adding 1.0mL CS by using a pipette2And (5) covering and sealing.
S502, 10.0 μ L of 0.770g/mL methylcyclohexane, 0.902g/mL ethyl acetate, 0.805g/mL butanone, 0.878g/mL benzene, 0.940g/mL ethyl acrylate, 0.799g/mL methyl isobutyl ketone, 0.867g/mL toluene, 0.867g/mL ethylbenzene, 0.861g/mL p-xylene, 0.880g/mL o-xylene, 0.906g/mL styrene, and 0.947g/mL cyclohexanone are injected into pure substances of all VOCs existing in the air by a micro-syringe in sequence to prepare a standard application liquid.
The thermal desorption conditions provided by the embodiment of the invention are as follows: the temperature of the transmission line is 100 ℃, and the temperature of the valve is 260 ℃; carrying out dry blowing on the sampling tube for 4-8 min, and carrying out desorption at 290 ℃, wherein the desorption time is 4-6 min, and the desorption flow is 30 mL/min; and (3) raising the temperature of the cold trap from room temperature to 260 ℃ at the maximum temperature rise rate, and then keeping the temperature for 3-5 min, wherein the resolving flow of the cold trap is 18 mL/min.
The gas chromatography-mass spectrometer provided by the embodiment of the invention has the following conditions: the sample introduction temperature is set to be 180 ℃, the transmission lead is set to be 100 ℃, the ion source is set to be 280 ℃, and the mass ratio of the sample introduction temperature to the transmission lead is set to be 20: 1, injecting sample at a split ratio, and setting the delay time of the solvent retarder to be 60-80 s; setting the initial column temperature to be 25 ℃ and maintaining for 4-8 min; then increasing the column temperature to 320 ℃ at the speed of 8 ℃/min and then maintaining for 4-8 min; helium was passed at a rate of 1mL/min as a carrier gas.
The method for detecting the sample enriched with the VOCs by adopting the thermal desorption-gas chromatography-mass spectrometry provided by the embodiment of the invention further comprises the following steps: and matching the detected result with data in a database after thermal desorption-gas chromatography-mass spectrometry detection, wherein the substances with the similarity of more than 70 percent are effective substances.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention, and the scope of the present invention is not limited thereto, and any modification, equivalent replacement, and improvement made by those skilled in the art within the technical scope of the present invention disclosed herein, which is within the spirit and principle of the present invention, should be covered by the present invention.
Claims (10)
1. A method for detecting VOCs in air is characterized by comprising the following steps:
determining the position of a sampling point, collecting an air sample by a TH-3000BIV ambient air sampler by using an instantaneous sampling method, closing a valve after the pressure in the ambient air sampler is consistent with the atmospheric pressure of the sampling point, sealing by using a sealing cap, and recording the ambient temperature and the atmospheric pressure of the sampling point; meanwhile, a pump is used for collecting VOCs from an air sample through an adsorbent;
setting numerical values of an organic waste gas concentration sensor and an air quantity sensor of the VOCs adsorption treatment device in the air through an external controller, and starting an air inlet fan to suck air to be enriched into the device after a heating net is preheated for 20-25 min by electrifying;
thirdly, enabling the collected VOCs to pass through a high-voltage electric field of 12000-20000V of the VOCs adsorption treatment device, simultaneously utilizing an ultraviolet lamp of an ultraviolet generating device to emit ultraviolet light, and gathering and irradiating the ultraviolet light emitted by the ultraviolet lamp on a photocatalyst on the surface of the activated carbon adsorption layer at a specific distance by means of a light gathering device to perform catalytic ionization of gas molecules;
fourthly, ions generated by catalytic ionization are attached to aerosol particles and are descended to a collector under the action of an electric field; finally, washing down the sediment on the surface of the collector to obtain an enriched VOCs sample;
analyzing the components and the concentration of the VOCs in the air by adopting a GC-FID/MS coupling technology on the enriched VOCs sample;
taking a 25mL pipette, measuring 25mL ultrapure water, adding the ultrapure water into an absorption tube, and placing the ultrapure water into an insulation box; 5mL of sample to be detected is taken to analyze the formaldehyde content in the indoor air by an acetylacetone spectrophotometry;
step seven, preparing standard sample solutions of various volatile compounds: at room temperature of 20-25 ℃, 1 1.5mL of Agilent sample introduction bottles are taken, and 1.0mL of CS is added by a pipette2Covering and sealing; a pure substance of all VOCs present in the air was injected into 10.0. mu.L of 0.770g/mL methylcyclohexane, 0.902g/mL ethyl acetate, 0.805g/mL butanone, 0.878g/mL benzene, 0.940g/mL ethyl acrylate, 0.799g/mL methyl isobutyl ketone, 0.867g/mL toluene, 0.867g/mL ethylbenzene, 0.861g/mL p-xylene, 0.880g/mL o-xylene, 0.906g/mL styrene and 0.947g/mL p-xylene in this order by a micro-syringeCyclohexanone, which is prepared into standard application liquid;
step eight, drawing a standard curve: taking 5 1.5mL sampling bottles, accurately adding 1.0mL CS respectively by a pipette2Immediately sealing and pressing by a silicon rubber spacer and sealing by a cover; injecting 5.0, 10.0, 15.0, 20.0 and 25.0 microliter of standard application liquid into a microinjector in sequence to prepare a standard series, and placing the standard series into a thermal desorption instrument to measure volatile organic compounds in the air;
step nine, drawing a standard curve based on the retention time and concentration series of the compound obtained by the determination in the step eight; and analyzing the sample enriched with the VOCs by adopting a thermal desorption-gas mass combination method based on the drawn standard curve to obtain a corresponding detection result.
2. The method according to claim 1, wherein in the first step, the conditions for collecting the air sample by using the TH-3000BIV ambient air sampler are as follows: the sampling flow is set to be 30-45 ml/min, and the sampling time is set to be 10-20 min.
3. The method according to claim 1, wherein in the first step, the adsorbent is Tenax or activated carbon.
4. The method according to claim 1, wherein in the second step, the organic waste gas concentration sensor and the air volume sensor are both electrically connected to an external controller, the type of the organic waste gas concentration sensor is PID-a1, and the type of the air volume sensor is KGF 2.
5. The method according to claim 1, wherein in step three, the surface of the activated carbon adsorption layer is coated with a photocatalyst, and the photocatalyst is nano titanium dioxide.
6. The method according to claim 1, wherein in step three, before the enriching of the samples of VOCs, the method further comprises a water removal operation; the method for removing water comprises the following steps:
and a plurality of stages of cold traps connected in series are used, and the temperature of the first cold trap is slowly increased when the target compound is transferred from the previous cold trap to the next extremely cold trap so as to prevent the transfer of water vapor.
7. The method according to claim 1, wherein in step eight, the thermal desorption conditions are as follows: the temperature of the transmission line is 100 ℃, and the temperature of the valve is 260 ℃; carrying out dry blowing on the sampling tube for 4-8 min, and carrying out desorption at 290 ℃, wherein the desorption time is 4-6 min, and the desorption flow is 30 mL/min; and (3) raising the temperature of the cold trap from room temperature to 260 ℃ at the maximum temperature rise rate, and then keeping the temperature for 3-5 min, wherein the resolving flow of the cold trap is 18 mL/min.
8. The method according to claim 1, wherein in the ninth step, the conditions of the GC-MS are as follows: the sample introduction temperature is set to be 180 ℃, the transmission lead is set to be 100 ℃, the ion source is set to be 280 ℃, and the mass ratio of the sample introduction temperature to the transmission lead is set to be 20: 1, and setting the delay time of the solvent retarder to be 60-80 s.
9. The method according to claim 8, wherein the initial column temperature is set at 25 ℃ and maintained for 4-8 min; then increasing the column temperature to 320 ℃ at the speed of 8 ℃/min and then maintaining for 4-8 min; helium was passed at a rate of 1mL/min as a carrier gas.
10. The method for detecting VOCs in air according to claim 1, wherein in step nine, the method for detecting the sample enriched with VOCs by using the combined thermal desorption-gas mass spectrometry further comprises:
and matching the detected result with data in a database after thermal desorption-gas chromatography-mass spectrometry detection, wherein the substances with the similarity of more than 70 percent are effective substances.
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