CN113203809A - Pretreatment method for efficiently extracting organic components from atmospheric particulates - Google Patents
Pretreatment method for efficiently extracting organic components from atmospheric particulates Download PDFInfo
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- CN113203809A CN113203809A CN202110472925.6A CN202110472925A CN113203809A CN 113203809 A CN113203809 A CN 113203809A CN 202110472925 A CN202110472925 A CN 202110472925A CN 113203809 A CN113203809 A CN 113203809A
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- 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
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- 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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- 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
- G01N2030/062—Preparation extracting sample from raw material
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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
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- G01N2030/067—Preparation by reaction, e.g. derivatising the sample
Abstract
The invention discloses a pretreatment method for efficiently extracting organic components from atmospheric particulates, which mainly comprises the following steps: (1) collecting PM in sample atmosphere by using sampler2.5(ii) particulate matter; (2) extracting the collected sample by using an ASE350 rapid solvent extractor to obtain an extraction liquid; (3) the extraction liquid is processed to a certain degree, and then the processed extraction liquid is analyzed by GC/MS. The method makes up the defects of the existing technology for extracting the organic components in the atmospheric particulates, in particular the defects of monitoring the organic components in the atmospheric particulates by using a gas chromatography-mass spectrometry; the method improves the extraction efficiency, reduces the using amount of the extraction solvent, shortens the extraction time, and can effectively and quickly extract and analyze the PM in the atmosphere2.5Organic components in the particulate.
Description
Technical Field
The invention belongs to the technical field of pretreatment methods of environmental organic pollutants, and particularly relates to a pretreatment method for efficiently extracting organic components from atmospheric particulates.
Background
Organic components in the atmospheric particulates can provide important geochemical information, and most of the organic components in the atmospheric particulates have certain toxicity to organisms, can cause strong stimulation to the respiratory system of a human body, can also cause the obstruction of the nervous system and the damage of the skin, and even can cause the risk of canceration of the skin; the research on the pollution characteristics of organic components in the particles has double significance in the aspects of resolving atmospheric fine particle sources and protecting human health.
At present, a lot of researches on organic components in the atmospheric particulates have been carried out in the world, and most of pretreatment processes for the organic components in the atmospheric particulates adopt a traditional pretreatment mode. The traditional pretreatment mode has the defects of consuming a large amount of solvent, generating a large amount of waste liquid, narrow application field coverage, long extraction time, low automation degree, low extraction efficiency, large human error, high extraction cost and the like. ASE350 accelerated solvent extractors are devices that rapidly extract organic material from solid and semi-solid samples. Rapid solvent extraction is a process of extracting a solid or semi-solid sample with a solvent at a certain temperature and pressure. The extraction efficiency is improved by using the conventional solvent and increasing the temperature and the pressure, so that the extraction time is greatly shortened, and the using amount of the extraction solvent is obviously reduced. The ASE rapid solvent extraction technology well solves the defects existing in the traditional pretreatment mode, has the advantages of short time, less solvent and high extraction efficiency, greatly improves the working efficiency of extraction due to the obvious characteristics of the ASE, has the advantages and is well applied to a plurality of fields, but has relatively less application in the field of analysis of organic components of atmospheric particulates, and has no well-recognized unified pretreatment experimental conditions at present.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a pretreatment method for efficiently extracting organic components from atmospheric particulates. The method makes up the defects of the existing technology for extracting organic components from atmospheric particulates, improves the extraction efficiency, reduces the usage amount of an extraction solvent, and shortens the extraction time.
In order to realize the purpose, the invention adopts the following technical scheme:
a pretreatment method for efficiently extracting organic components in atmospheric particulates comprises the following steps:
(1) collecting a sample: before collecting a sample, the flow of the sampler needs to be corrected, a filter membrane clamp and an adsorbent sleeve are sequentially installed and connected with the sampler, the sampling flow is adjusted, and the sampling is started;
(2) extracting a sample: taking a certain amount of quartz filter membrane, shearing, placing in an extraction tank with a cellulose membrane at the bottom layer, adding diatomite, mixing with the quartz filter membrane sample, placing in the extraction tank, adding an extraction solvent for extraction, and taking out the extract after extraction is finished;
(3) and (3) analyzing the extract: concentrating the extract liquor in the step (2) to be nearly dry by using a rotary evaporator and a nitrogen blower, performing derivatization reaction by using N, O-bistrimethylsilyl-trifluoroacetamide, and directly analyzing by using GC/MS.
Further, in the step (1), a quartz filter membrane is adopted to collect PM of the sample2.5Particulate matter, the flow rate of the collected sample is 1.3m3min-1。
Further, in the step (1), the sample is stored at the temperature of below 4 ℃ in a dark place after the collection is finished.
Further, the sample extracted in the step (2) is extracted by using an ASE350 rapid solvent extractor; the extraction apparatus comprises a solvent bottle, a pump, a gas circuit, a heating furnace chamber, a stainless steel extraction tank and a collection bottle.
Further, the specific operation method of the sample extraction in the step (2) is as follows: manually loading the sample collected in the step (1) into an extraction pool of an ASE350 rapid solvent extraction instrument, placing the extraction pool on a disc type conveying device, conveying the extraction pool into a heating furnace chamber by the disc type conveying device, connecting the extraction pool with a collection bottle with a relative number, conveying the extraction solvent to the extraction pool by a pump, heating and pressurizing the extraction pool in the heating furnace chamber, carrying out static extraction at a set temperature and pressure, adding a small amount of cleaning solvent into the extraction pool for multiple times, automatically introducing the extraction liquid into the collection bottle through a filter membrane, purging the extraction pool and a pipeline by nitrogen, and completely introducing the extraction liquid into the collection bottle to be analyzed.
Further, the extraction parameters of the extraction cell include the following: extracting solvent: mixed solution of dichloromethane and methanol in a volume ratio of 2:1, system pressure: 1500psi, extraction temperature: static extraction time at 100 ℃: 3min, cycle number: 2 times, volume of wash: 50%, purge time: for 60 s.
Further, the GC/MS analysis conditions in the step (3) are as follows: (1) the gas chromatography-mass spectrometer adopts Agilent 7890A, and the tandem mass spectrometer adopts Agilent 5975C; a chromatographic column: HP-5MS capillary column, the specification is: 30 m.times.0.25 mm.times.0.25 μm; temperature of the column oven: maintaining at 50 deg.C for 2 min, heating to 120 deg.C at 15 deg.C per minute, heating to 300 deg.C at 5 deg.C per minute, and maintaining for 16 min; mobile phase type: n-hexane; the flow rate of the mobile phase: 1 mL/min; sample introduction amount of a sample to be analyzed: 2 μ L.
Compared with the prior art, the method has the following advantages: the method makes up the defects of the existing technology for extracting the organic components in the atmospheric particulates, in particular the defects of monitoring the organic components in the atmospheric particulates by using a gas chromatography-mass spectrometry; the method improves the extraction efficiency, reduces the usage amount of the extraction solvent and shortens the extraction time.
Drawings
FIG. 1 is an ASE350 accelerated solvent extractor.
FIG. 2 is a graph of the concentration ratio of the primary and secondary organic tracer to organic carbon OC in spring and summer.
FIG. 3 is a diurnal variation graph of a primary organic aerosol.
FIG. 4 is a diurnal variation graph of a secondary organic aerosol.
Detailed Description
Preferred embodiments of the present invention will be described in detail with reference to the following examples. It is to be understood that the following examples are given for illustrative purposes only and are not intended to limit the scope of the present invention. Various modifications and substitutions may be made by those skilled in the art without departing from the spirit and scope of the invention, and all such modifications and substitutions are intended to be within the scope of the claims.
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified. Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
Examples
A pretreatment method for efficiently extracting organic components in atmospheric particulates comprises the following steps:
(1) collecting a sample: correcting the flow of the sampler before collecting the sample, sequentially installing a filter membrane clamp and an adsorbent sleeve, connecting with the sampler, adjusting the sampling flow, starting sampling, and collecting the PM of the sample by using a quartz filter membrane in the sampling process2.5Particulate matter, the flow rate of the collected sample is 1.3m3min-1The sampling time is determined according to specific conditions, and after the sample is collected, the sample is stored at the dark state below 4 ℃;
(2) extracting a sample: taking a certain amount of quartz filter membrane, cutting into pieces, placing the quartz filter membrane into an extraction tank of an ASE350 rapid solvent extraction instrument of which the bottom layer is padded with a cellulose membrane, adding diatomite, uniformly mixing with a quartz filter membrane sample, then loading the quartz filter membrane sample into the extraction tank, manually loading the sample collected in the step (1) into the extraction tank of the ASE350 rapid solvent extraction instrument, placing the extraction tank on a disc type conveying device, conveying the extraction tank into a heating furnace chamber by the disc type conveying device, connecting the extraction tank with a collection bottle with a relative number, conveying the extraction solvent to the extraction tank by a pump, and setting the parameters of the extraction tank as follows: the extraction solvent is a mixed solution of dichloromethane and methanol with the volume ratio of 2: 1; system pressure: 1500 psi; the extraction temperature is as follows: 100 ℃; static extraction time: 3 min; cycle number: 2 times; flush volume: 50 percent; purging time: 60 s; heating and pressurizing the extraction tank in a heating furnace cavity, performing static extraction at a set temperature and pressure, adding a small amount of cleaning solvent into the extraction tank for multiple times, automatically allowing the extract to enter a collection bottle through a filter membrane, purging the extraction tank and a pipeline with nitrogen, and allowing all the extract to enter the collection bottle to be analyzed;
(3) and (3) analyzing the extract: concentrating the extract liquor in the step (2) to be nearly dry by using a rotary evaporator and a nitrogen blower, performing derivatization reaction by using N, O-bistrimethylsilyl-trifluoroacetamide, and directly performing GC/MS analysis under the following analysis conditions: adopting a gas chromatography-mass spectrometer Agilent 7890A and a tandem mass spectrometer Agilent 5975C; a chromatographic column: HP-5MS capillary column, the specification is: 30 m.times.0.25 mm.times.0.25 μm; temperature of the column oven: maintaining at 50 deg.C for 2 min, heating to 120 deg.C at 15 deg.C per minute, heating to 300 deg.C at 5 deg.C per minute, and maintaining for 16 min; mobile phase type: n-hexane; the flow rate of the mobile phase: 1 mL/min; sample introduction amount of a sample to be analyzed: 2 μ L.
PM collected in Beijing urban area in spring and summer in 2017 is analyzed by using ASE extraction pretreatment method and GC/MS analysis method2.5The concentration levels of the major primary and secondary organic tracers in (fig. 2) and the diurnal variation characteristics (fig. 3 and 4). The primary organic tracer includes Phytane and pristanane (phytone)&Pristine), Polycyclic Aromatic Hydrocarbons (PAHs), Levoglucosan (levoglucan) and Trehalose (Trehalose), four primary sources that may be indicated are motor vehicle exhaust emissions, coal and fossil fuel combustion, biomass combustion and sand dust, respectively. The secondary organic tracers comprise Isoprene oxidation products (Isoprene SOA tracers), Pinene oxidation products (alpha/beta-Pinene SOA tracers), caryophyllenic acid (beta-Caryophyllinic acid) and 2, 3-Dihydroxy-4-pentanoic acid (2,3-Dihydroxy-4-oxopentanoic acid), the former three types are tracers of biological secondary organic aerosol, and the 2, 3-Dihydroxy-4-pentanoic acid is a tracer of artificial source (mainly toluene). Phytane&The ratios of pristane and polycyclic aromatic hydrocarbons to organic carbon OC are higher in summer than in spring (fig. 2a), the ratios of levoglucosan and trehalose to organic carbon OC are higher in spring than in summer (fig. 2b), because fossil fuel combustion, including motor vehicle exhaust emissions, is a local primary emission, and biomass combustion and dust are mainly derived from regional transport, so the two groups of organic tracers exhibit the seasonal variation characteristics described above. The ratio of secondary organic aerosol tracer to organic carbon OC showed higher summer than spring (fig. 2c and 2d), mainly because the photochemical reaction was stronger in summer, more favorable for the generation of secondary organic aerosol. FIGS. 3 and 4 show the diurnal activity of these classes of organic tracersA changing characteristic. Phytanes as man-made primary organic tracers&Pristane, polycyclic aromatic hydrocarbons and levoglucosan, exhibit a low daytime and high night characteristic, probably mainly as a result of nighttime emissions and a low accumulation of boundary layers, whereas secondary organic tracers exhibit a low daytime and low night variation characteristic, mainly because they are produced in large quantities during the day when the photochemical reaction is intense.
Test examples
And comparing the recovery rates of the standard samples under different extraction conditions, selecting the optimal extraction condition parameters, and comparing the optimal extraction condition parameters with the traditional ultrasonic extraction pretreatment method.
The traditional ultrasonic extraction method comprises the following steps: a sample filter membrane with a certain area is placed in a sample bottle, an extraction solvent (the same as the extraction solvent in the embodiment 1 of the invention) is added until the filter membrane is completely immersed, and ultrasonic extraction is carried out for 3 times, each time for 15 minutes.
(1) Standard solution preparation
Normal paraffin mixed standard (Sigma-Aldrich, USA) and polycyclic aromatic hydrocarbon mixed standard (Sigma-Aldrich, USA) are directly purchased at concentrations of 500. mu.g/uL and 2000. mu.g/uL respectively, and the two stock solutions are diluted to 1ng/uL respectively with n-hexane solution (chromatographically pure, TEDIA, USA). In the experiment, a blank quartz filter membrane is adopted for a standard recovery rate experiment, and normal alkane and polycyclic aromatic hydrocarbon mixed standard solution with the concentration of 1ng/uL is used as an extract to be extracted.
(2) Compared with the traditional ultrasonic extraction pretreatment method
By comparing the ASE extraction pretreatment method with the traditional ultrasonic extraction pretreatment method, the experimental parameters of 4 groups of ASE extraction pretreatment methods are determined, and are shown in Table 1.
TABLE 1 4 sets of Experimental parameters for ASE extraction pretreatment method
A group of the 4 groups of ASE extraction pretreatment method experimental parameters with the most reasonable recovery rate of the mixed standard substances (specifically shown in the table 2) is selected as the optimal experimental conditions of the ASE extraction pretreatment method.
TABLE 2 ASE Pre-extraction treatment method Standard mixture recovery (%)
| Name of mixed standard substance | Group 1 | |
|
|
| Normal alkane mixed standard | 53-123 | 255-343 | 162-448 | 163-377 |
| Polycyclic aromatic hydrocarbon mixed standard | 55-119 | 332-592 | 225-418 | 151-514 |
As can be seen from the data in table 2, the recovery rates of the two mixed standard substances under the experimental parameters in the 1 st group are most reasonable, so the experimental parameters in the 1 st group are selected as the experimental conditions of the optimal ASE extraction pretreatment method, that is, the extraction temperature: 100 ℃; static extraction time: 3 min; cycle number: 2 times; flush volume: 50 percent; purging time: 60s, consistent with the ASE extraction parameters adopted by the invention.
Under the optimal experimental conditions of the ASE extraction pretreatment method, two pretreatment methods of ASE extraction and traditional ultrasonic extraction are respectively adopted to carry out mixed standard recovery experiments (each group is provided with 4 repeated samples), and the comparative data of the recovery rates of the mixed standard of the two pretreatment methods are shown in the table 3.
TABLE 3 comparison of recovery (%) of the mixed standard substance between the ASE pre-extraction method and the conventional ultrasonic pre-extraction method
As can be seen from the data in Table 3, compared with the traditional ultrasonic extraction pretreatment method, the ASE extraction pretreatment method of the invention has better overall recovery rate of the two mixed standard substances, and shows that the ASE extraction pretreatment method of the invention has higher efficiency for extracting organic components in atmospheric particulates.
Although the invention has been described in detail above with reference to a general description and specific examples, it will be apparent to one skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (7)
1. A pretreatment method for efficiently extracting organic components from atmospheric particulates is characterized by comprising the following steps:
(1) collecting a sample: before collecting a sample, the flow of the sampler needs to be corrected, a filter membrane clamp and an adsorbent sleeve are sequentially installed and connected with the sampler, the sampling flow is adjusted, and the sampling is started;
(2) extracting a sample: taking a certain amount of quartz filter membrane, shearing, placing in an extraction tank with a cellulose membrane at the bottom layer, adding diatomite, mixing with the quartz filter membrane sample, placing in the extraction tank, adding an extraction solvent for extraction, and taking out the extract after extraction is finished;
(3) and (3) analyzing the extract: concentrating the extract liquor in the step (2) to be nearly dry by using a rotary evaporator and a nitrogen blower, performing derivatization reaction by using N, O-bistrimethylsilyl-trifluoroacetamide, and directly analyzing by using GC/MS.
2. The pretreatment method for efficiently extracting organic components from atmospheric particulates according to claim 1, wherein in the step (1), a quartz filter membrane is adopted to collect PM (particulate matter) in a sample2.5Particulate matter, the flow rate of the collected sample is 1.3m3min-1。
3. The pretreatment method for efficiently extracting organic components from atmospheric particulates according to claim 1, wherein in the step (1), the sample is collected and then stored at a temperature below 4 ℃ in a dark place.
4. The pretreatment method for efficiently extracting organic components from atmospheric particulates according to claim 1, wherein the sample extracted in the step (2) is an ASE350 rapid solvent extractor; the extraction apparatus comprises a solvent bottle, a pump, a gas circuit, a heating furnace chamber, a stainless steel extraction tank and a collection bottle.
5. The pretreatment method for efficiently extracting organic components from atmospheric particulates according to claim 1, wherein the specific operation method of the sample extraction in the step (2) comprises the following steps: manually loading the sample collected in the step (1) into an extraction pool of an ASE350 rapid solvent extraction instrument, placing the extraction pool on a disc type conveying device, conveying the extraction pool into a heating furnace chamber by the disc type conveying device, connecting the extraction pool with a collection bottle with a relative number, conveying the extraction solvent to the extraction pool by a pump, heating and pressurizing the extraction pool in the heating furnace chamber, carrying out static extraction at a set temperature and pressure, adding a small amount of cleaning solvent into the extraction pool for multiple times, automatically introducing the extraction liquid into the collection bottle through a filter membrane, purging the extraction pool and a pipeline by nitrogen, and completely introducing the extraction liquid into the collection bottle to be analyzed.
6. The pretreatment method for efficiently extracting organic components from atmospheric particulates according to claim 5, wherein the extraction parameters of the extraction cell comprise the following: extracting solvent: mixed solution of dichloromethane and methanol in a volume ratio of 2:1, system pressure: 1500psi, extraction temperature: static extraction time at 100 ℃: 3min, cycle number: 2 times, volume of wash: 50%, purge time: for 60 s.
7. The pretreatment method for efficiently extracting organic components from atmospheric particulates according to claim 1, wherein the GC/MS analysis conditions in the step (3) are as follows: (1) the gas chromatography-mass spectrometer adopts Agilent 7890A, and the tandem mass spectrometer adopts Agilent 5975C;
a chromatographic column: HP-5MS capillary column, the specification is: 30 m.times.0.25 mm.times.0.25 μm; temperature of the column oven: maintaining at 50 deg.C for 2 min, heating to 120 deg.C at 15 deg.C per minute, heating to 300 deg.C at 5 deg.C per minute, and maintaining for 16 min; mobile phase type: a mixed solution of dichloromethane and methanol with a volume ratio of 2: 1; the flow rate of the mobile phase: 1 mL/min; sample introduction amount of a sample to be analyzed: 2 μ L.
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