CN112697902A - Quantitative analysis method for volatile organic compounds - Google Patents
Quantitative analysis method for volatile organic compounds Download PDFInfo
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- CN112697902A CN112697902A CN202011435633.7A CN202011435633A CN112697902A CN 112697902 A CN112697902 A CN 112697902A CN 202011435633 A CN202011435633 A CN 202011435633A CN 112697902 A CN112697902 A CN 112697902A
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- 238000000034 method Methods 0.000 title claims abstract description 35
- 238000004445 quantitative analysis Methods 0.000 title abstract description 16
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- 238000004817 gas chromatography Methods 0.000 claims abstract description 26
- 238000001514 detection method Methods 0.000 claims abstract description 19
- 238000012360 testing method Methods 0.000 claims abstract description 16
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- 239000007789 gas Substances 0.000 claims description 48
- QWTDNUCVQCZILF-UHFFFAOYSA-N isopentane Chemical compound CCC(C)C QWTDNUCVQCZILF-UHFFFAOYSA-N 0.000 claims description 46
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- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims description 23
- NHTMVDHEPJAVLT-UHFFFAOYSA-N Isooctane Chemical compound CC(C)CC(C)(C)C NHTMVDHEPJAVLT-UHFFFAOYSA-N 0.000 claims description 23
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- JVSWJIKNEAIKJW-UHFFFAOYSA-N dimethyl-hexane Natural products CCCCCC(C)C JVSWJIKNEAIKJW-UHFFFAOYSA-N 0.000 claims description 23
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- 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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas 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
- G01N2030/042—Standards
- G01N2030/047—Standards external
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Abstract
The invention discloses a quantitative analysis method of volatile organic compounds, which comprises the following steps: s1, pretreatment of a test sample; s2, qualitative detection: qualitatively analyzing a plurality of main components of the volatile organic gas in the expandable microspheres obtained in the step S1 by using a gas chromatography-mass spectrometer; s3, preparing a mixed standard working solution; s4, quantitative detection: and under the same conditions, respectively injecting the mixed standard working solution prepared in the step S3 and the volatile organic compound gas in the headspace bottle obtained through post-treatment in the step S1, performing gas chromatography test, collecting data and analyzing. The method is simple, convenient and quick, the analysis is quick, the result is accurate, the detection result obtained by the method can provide reference for the transportation of the expandable microsphere product, and the expandable microsphere product is ensured to be safer in the transportation process.
Description
Technical Field
The invention relates to the field of chemical products, in particular to a quantitative analysis method for volatile organic compounds.
Background
The heat expandable microsphere is a polymer particle which has a core-shell structure and can expand when heated, the core of the microsphere is liquid low-boiling-point alkane or other compounds, and the shell of the microsphere is a thermoplastic polymer with good barrier property and capable of preventing substances in the core from leaking. The shell of the microsphere is hard at normal temperature; when the microsphere is heated, the internal substance is vaporized or decomposed to generate pressure, and the macromolecular shell layer is softened, so that the microsphere can show good expansion performance if the pressure generated by the inner core is properly matched with the thermoplasticity of the outer shell.
VOCs are acronyms for volatile organic compounds (Volatile organic communications). Generally refers to an organic compound which is easy to volatilize at normal temperature, but the definition in the environmental protection sense refers to an active volatile organic compound, namely a volatile organic compound which can generate harm. The main components of VOC are: hydrocarbons, halogenated hydrocarbons, oxygen hydrocarbons and nitrogen hydrocarbons, which include: benzene series, organic chloride, freon series, organic ketone, amine, alcohol, ether, ester, acid and petroleum hydrocarbon compound. More common are benzene, toluene, xylene, ethylbenzene, styrene, formaldehyde, TVOC (C6-C16 alkane), ketones, and the like. These compounds are characterized by being volatile and hydrophilic, and are widely used in the industrial fields of footwear, toys, paints and inks, adhesives, cosmetics, interior and automobile decoration materials, and the like. VOC has great influence on human health, when the VOC in a room reaches a certain concentration, people can feel headache, nausea, vomiting, hypodynamia and the like in a short time, and can be convulsion and coma in severe cases, and the liver, the kidney, the brain and the nervous system of people can be injured, so that serious consequences such as hypomnesis and the like can be caused, and even cancer can be possibly caused.
At present, no relevant report for testing the VOC content of the expandable microspheres exists.
Disclosure of Invention
The invention aims to provide a quantitative analysis method for volatile organic compounds, which is simple, convenient and quick, has quick analysis and accurate result, and can provide reference for cargo transportation of expandable microsphere products and ensure that the expandable microsphere products are safer in the transportation process.
In order to achieve the purpose, the invention adopts the technical scheme that:
the method for quantitatively analyzing the volatile organic compounds comprises the following steps:
s1, pretreatment of a test sample: placing expandable microspheres into a headspace bottle, recording the mass of the expandable microspheres, tightly covering the headspace bottle by using a jaw bottle cap, forming a sealed space inside the headspace bottle, and placing the headspace bottle in an oven at the temperature of at least 50 ℃ for more than 14 days to obtain volatile organic gas in the expandable microspheres;
s2, qualitative detection: qualitatively analyzing a plurality of main components of the volatile organic gas in the expandable microspheres obtained in the step S1 by using a gas chromatography-mass spectrometer;
s3, preparation of a mixed standard working solution: pure substances of a plurality of main components of volatile organic gas in the expandable microspheres detected in the step S2 are used as standard substances, and are dissolved in a solvent after being mixed to prepare a series of mixed standard working solutions with different concentrations;
s4, quantitative detection: and under the same conditions, respectively injecting the mixed standard working solution prepared in the step S3 and the volatile organic compound gas in the headspace bottle obtained through post-treatment in the step S1, performing gas chromatography test, collecting data and analyzing.
Preferably, in S1, the filling amount of the expandable microspheres is 50% of the volume of the headspace bottle.
Preferably, in S2, the volatile organic compounds in the expandable microspheres include isopentane, isooctane, ethanol and acrylonitrile.
Preferably, in S3, the solvent is toluene.
Preferably, in S4, the sample injection manner of the mixed standard working solution is automatic or manual, and the sample injection amount is 0.1 μ L.
Preferably, in S4, the sample injection manner of the volatile organic compound gas is automatic or manual, and the sample injection amount is 1 ml.
Preferably, in S2, the gas chromatography conditions are: temperature programming is carried out, the temperature of a sample inlet is 200 ℃, and the sample introduction mode is shunting; the chromatographic column adopts a polyethylene glycol chromatographic column with the model of TG-WAXMS; the carrier gas is nitrogen, and the constant current mode is adopted; the detector adopted is a hydrogen flame ionization detector; the solvent delay of the mass spectrometer used in conjunction with the gas chromatograph was set to 0min, and the Scan ion Scan range was 29-500 amu; in S4, the gas chromatography conditions were: temperature programming is carried out, the temperature of a sample inlet is 200 ℃, and the sample introduction mode is shunting; the chromatographic column adopts a polyethylene glycol chromatographic column with the model of TG-WAXMS; the carrier gas is nitrogen, and the constant current mode is adopted; the detector used was a hydrogen flame ionization detector.
Preferably, in S2 and S4, the temperature rising program adopted by the gas chromatograph is: the initial temperature is 35-50 ℃, and the holding time is 3-5 min; then increased to 200 ℃ at a rate of 10 ℃/min.
Preferably, the size of the chromatography column in S2 and S4 is 30m 0.32mm 0.25 μm each.
Preferably, the split ratio is 30 in both S2 and S4; the flow rate of the nitrogen gas was 1.2 ml/min.
Preferably, the hydrogen flame ionization detectors used in S2 and S4 both have an analysis temperature of 220 ℃, a hydrogen flow rate of 35ml/min and an air flow rate of 350 ml/min.
By adopting the technical scheme, compared with the prior art, the invention has the following technical effects:
the method provided by the invention can be used for detecting the main VOC components in the microspheres without diluting a sample or a standard solution, can be used for testing various VOC components such as isopentane, isooctane, ethanol, acrylonitrile and other VOC substances at one time, and is simple, convenient and rapid, and accurate in result. In the standard curve test of the standard liquid, a liquid sample introduction method is adopted, so that the defect of difficult sampling when a gas standard sample is used is avoided, and meanwhile, the accuracy of a quantitative method can be ensured.
Drawings
FIG. 1 is a gas chromatogram of a sample of example 1 according to the present invention.
Detailed Description
The invention is further described with reference to the following drawings and specific examples, which are not intended to be limiting.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
Example 1
The quantitative analysis method for volatile organic compounds provided by the embodiment comprises the following steps:
s1, pretreatment of a test sample: placing expandable microspheres into a headspace bottle, wherein the addition amount of the expandable microspheres accounts for 50% of the volume of the headspace bottle, weighing by a balance, recording the mass of the expandable microspheres to be 5.0945g, tightly covering the headspace bottle by using a jaw bottle cap, forming a sealed space inside the headspace bottle, and placing in an oven at the temperature of 50 ℃ for 14 days to obtain volatile organic gas in the expandable microspheres;
s2, qualitative detection: adopting a gas chromatography-mass spectrometer, wherein the gas chromatography conditions are as follows: the temperature raising procedure is that the initial temperature is 40 ℃, the temperature is kept for 5min, then the temperature is raised to 200 ℃ at the speed of 10 ℃/min, the temperature of a sample inlet is 200 ℃, the sample feeding mode is split flow, and the split flow ratio is 30; the sample introduction mode is flow splitting; the chromatographic column adopts a polyethylene glycol chromatographic column with the model of TG-WAXMS, and the specification of the chromatographic column is 30m x 0.32mm x 0.25 mu m; the carrier gas is nitrogen, and the constant-current mode is 1.2 ml/min; the detector is a hydrogen flame ionization detector, the analysis temperature of the hydrogen flame ionization detector is 220 ℃, the flow rate of the used hydrogen is 35ml/min, and the flow rate of the air is 350 ml/min; setting the solvent delay of a mass spectrometer to be 0min, and scanning the Scan ions to be 29-500 amu; qualitatively analyzing a plurality of main components of volatile organic gas in the expandable microspheres obtained in the step S1, wherein the volatile organic gas in the expandable microspheres comprises isopentane, isooctane, ethanol and acrylonitrile;
s3, preparation of a mixed standard working solution: mixing pure standard substances of isopentane, isooctane, ethanol and acrylonitrile, dissolving the mixture into toluene to prepare a series of mixed standard working solutions with a series of concentrations, wherein the concentrations of the isopentane in the mixed standard working solutions with the series of concentrations are respectively 0.005, 0.01, 0.025, 0.05 and 0.1g/ml, the concentrations of the isooctane in the mixed standard working solutions with the series of concentrations are respectively 0.0025, 0.005, 0.01, 0.025 and 0.05g/ml, the concentrations of the ethanol in the mixed standard working solutions with the series of concentrations are respectively 0.005, 0.01, 0.025, 0.05 and 0.1g/ml, and the concentrations of the acrylonitrile in the mixed standard working solutions with the series of concentrations are respectively 0.01, 0.02, 0.05, 0.1 and 0.2 g/ml;
s4, quantitative detection: under the same conditions, respectively transferring 5ml to 20ml of the mixed standard working solution with the series of concentrations into a headspace bottle, tightly covering the headspace bottle with a headspace bottle cap, setting the sample injection amount to be 0.1 mu L by adopting a gas chromatography Saimei fly Trace1300, a CombipAL automatic sample injector and a liquid injector, collecting data, determining a standard curve, and solving the slope and the intercept; taking out the headspace bottle after the pretreatment (placing in a 50 ℃ oven for 14 days) is finished, placing the headspace bottle on a gas chromatography Sammer fly Trace1300, a CombipAl automatic sample injector, using a gas injector, setting the sample volume to be 1ml, collecting data, and checking the concentration of the component to be detected from a standard curve according to the signal of the component to be detected or calculating by using a regression equation; wherein, the gas chromatography conditions are as follows: the temperature raising procedure is that the initial temperature is 40 ℃, the temperature is kept for 5min, then the temperature is raised to 200 ℃ at the speed of 10 ℃/min, the temperature of a sample inlet is 200 ℃, the sample feeding mode is split flow, and the split flow ratio is 30; the sample introduction mode is flow splitting; the chromatographic column adopts a polyethylene glycol chromatographic column with the model of TG-WAXMS, and the specification of the chromatographic column is 30m x 0.32mm x 0.25 mu m; the carrier gas is nitrogen, and the constant-current mode is 1.2 ml/min; the detector used is a hydrogen flame ionization detector, the analysis temperature of the hydrogen flame ionization detector is 220 ℃, the flow rate of the used hydrogen is 35ml/min, and the flow rate of the air is 350 ml/min.
And (4) analyzing results: the results show that the major VOC species are all able to form an effective separation. And (4) carrying out quantitative analysis on the detection result by an external standard method of gas chromatography. Calculating the concentration (g/ml) of each substance through a standard curve equation of an external standard method of each substance, and obtaining the content of different volatile organic compounds in the microspheres by using a formula (1):
wherein, w is the content of volatile organic compounds in the microspheres, and the content is mu g/g;
c-concentration of each substance, g/ml, obtained using a standard curve;
m-mass of microsphere sample placed in the headspace bottle.
And VOC volume fraction (%) calculation formula (2):
v is volume fraction of volatile organic compounds in the microspheres,%;
c-concentration of each substance, g/ml, obtained using a standard curve;
ρ -relative density of each VOC substance (air 1), kg/m3。
(the relative gas densities of isopentane, isooctane, ethanol, and acrylonitrile were 2.48, 3.9, 1.59, and 1.83kg/m, respectively3。)
Example 1 the results are shown in table 1:
TABLE 1
| VOC example 1 | Concentration c (g/ml) | Content w (μ g/g) | Volume fraction v (%) |
| Isopentane | 0.070652213 | 23.57616295 | 0.284887956 |
| Isooctane | 0.017559723 | 5.859560069 | 0.04502493 |
| Ethanol | 0.011341703 | 3.78464917 | 0.071331466 |
| Acrylonitrile | 0.163394777 | 54.52372567 | 0.892867632 |
Example 2
The quantitative analysis method for volatile organic compounds provided by the embodiment comprises the following steps:
s1, pretreatment of a test sample: placing expandable microspheres into a headspace bottle, wherein the addition amount of the expandable microspheres accounts for 50% of the volume of the headspace bottle, weighing by a balance, recording the mass of the expandable microspheres to be 4.8844g, tightly covering the headspace bottle by using a jaw bottle cap, forming a sealed space inside the headspace bottle, and placing in an oven at the temperature of 50 ℃ for 14 days to obtain volatile organic gas in the expandable microspheres;
s2, qualitative detection: adopting a gas chromatography-mass spectrometer, wherein the gas chromatography conditions are as follows: the temperature raising procedure is that the initial temperature is 35 ℃, the temperature is kept for 5min, then the temperature is raised to 200 ℃ at the speed of 10 ℃/min, the temperature of a sample inlet is 200 ℃, the sample feeding mode is split flow, and the split flow ratio is 30; the sample introduction mode is flow splitting; the chromatographic column adopts a polyethylene glycol chromatographic column with the model of TG-WAXMS, and the specification of the chromatographic column is 30m x 0.32mm x 0.25 mu m; the carrier gas is nitrogen, and the constant-current mode is 1.2 ml/min; the detector is a hydrogen flame ionization detector, the analysis temperature of the hydrogen flame ionization detector is 220 ℃, the flow rate of the used hydrogen is 35ml/min, and the flow rate of the air is 350 ml/min; setting the solvent delay of a mass spectrometer to be 0min, and scanning the Scan ions to be 29-500 amu; qualitatively analyzing a plurality of main components of volatile organic gas in the expandable microspheres obtained in the step S1, wherein the volatile organic gas in the expandable microspheres comprises isopentane, isooctane, ethanol and acrylonitrile;
s3, preparation of a mixed standard working solution: mixing pure standard substances of isopentane, isooctane, ethanol and acrylonitrile, dissolving the mixture into toluene to prepare a series of mixed standard working solutions with a series of concentrations, wherein the concentrations of the isopentane in the mixed standard working solutions with the series of concentrations are respectively 0.005, 0.01, 0.025, 0.05 and 0.1g/ml, the concentrations of the isooctane in the mixed standard working solutions with the series of concentrations are respectively 0.0025, 0.005, 0.01, 0.025 and 0.05g/ml, the concentrations of the ethanol in the mixed standard working solutions with the series of concentrations are respectively 0.005, 0.01, 0.025, 0.05 and 0.1g/ml, and the concentrations of the acrylonitrile in the mixed standard working solutions with the series of concentrations are respectively 0.01, 0.02, 0.05, 0.1 and 0.2 g/ml;
s4, quantitative detection: under the same conditions, the mixed standard working solutions with the series of concentrations are respectively extracted by a 1 mu L sample injection needle by hand to 0.1 mu L for the Sammer fly Trace1300 gas chromatography test, data are collected, a standard curve is determined, and the slope and the intercept are calculated; taking out the headspace bottle after the pretreatment (placing in a 50 ℃ oven for 14 days) is finished, manually extracting 1ml of gas above the headspace bottle by using a 1ml sample injection needle, collecting data, and finding out the concentration of the component to be detected from a standard curve according to the signal of the component to be detected or calculating by using a regression equation; wherein, the gas chromatography conditions are as follows: the temperature raising procedure is that the initial temperature is 35 ℃, the temperature is kept for 5min, then the temperature is raised to 200 ℃ at the speed of 10 ℃/min, the temperature of a sample inlet is 200 ℃, the sample feeding mode is split flow, and the split flow ratio is 30; the sample introduction mode is flow splitting; the chromatographic column adopts a polyethylene glycol chromatographic column with the model of TG-WAXMS, and the specification of the chromatographic column is 30m x 0.32mm x 0.25 mu m; the carrier gas is nitrogen, and the constant-current mode is 1.2 ml/min; the detector used is a hydrogen flame ionization detector, the analysis temperature of the hydrogen flame ionization detector is 220 ℃, the flow rate of the used hydrogen is 35ml/min, and the flow rate of the air is 350 ml/min.
And (4) analyzing results: the results show that the major VOC species are all able to form an effective separation. And (4) carrying out quantitative analysis on the detection result by an external standard method of gas chromatography. Calculating the concentration (g/ml) of each substance through a standard curve equation of an external standard method of each substance, and obtaining the content of different volatile organic compounds in the microspheres by using a formula (1):
wherein, w is the content of volatile organic compounds in the microspheres, and the content is mu g/g;
c-concentration of each substance, g/ml, obtained using a standard curve;
m-mass of microsphere sample placed in the headspace bottle.
And VOC volume fraction (%) calculation formula (2):
v is volume fraction of volatile organic compounds in the microspheres,%;
c-concentration of each substance, g/ml, obtained using a standard curve;
ρ -relative density of each VOC substance (air 1), kg/m3。
(the relative gas densities of isopentane, isooctane, ethanol, and acrylonitrile were 2.48, 3.9, 1.59, and 1.83kg/m, respectively3。)
Example 2 the results are shown in table 2:
TABLE 2
| VOC example 2 | Concentration c (g/ml) | Content w (μ g/g) | Volume fraction v (%) |
| Isopentane | 0.070488587 | 24.5333302 | 0.284228174 |
| Isooctane | 0.017781123 | 6.18866386 | 0.045592624 |
| Ethanol | 0.011614629 | 4.042434894 | 0.07304798 |
| Acrylonitrile | 0.170609263 | 59.38001552 | 0.932291057 |
Example 3
The quantitative analysis method for volatile organic compounds provided by the embodiment comprises the following steps:
s1, pretreatment of a test sample: placing expandable microspheres into a headspace bottle, wherein the addition amount of the expandable microspheres accounts for 50% of the volume of the headspace bottle, weighing by a balance, recording the mass of the expandable microspheres to be 5.0728g, tightly covering the headspace bottle by using a jaw bottle cap, forming a sealed space inside the headspace bottle, and placing in an oven at the temperature of 50 ℃ for 14 days to obtain volatile organic gas in the expandable microspheres;
s2, qualitative detection: adopting a gas chromatography-mass spectrometer, wherein the gas chromatography conditions are as follows: the temperature raising procedure is that the initial temperature is 50 ℃, the temperature is kept for 3min, then the temperature is raised to 200 ℃ at the speed of 10 ℃/min, the temperature of a sample inlet is 200 ℃, the sample feeding mode is split flow, and the split flow ratio is 30; the sample introduction mode is flow splitting; the chromatographic column adopts a polyethylene glycol chromatographic column with the model of TG-WAXMS, and the specification of the chromatographic column is 30m x 0.32mm x 0.25 mu m; the carrier gas is nitrogen, and the constant-current mode is 1.2 ml/min; the detector is a hydrogen flame ionization detector, the analysis temperature of the hydrogen flame ionization detector is 220 ℃, the flow rate of the used hydrogen is 35ml/min, and the flow rate of the air is 350 ml/min; setting the solvent delay of a mass spectrometer to be 0min, and scanning the Scan ions to be 29-500 amu; qualitatively analyzing a plurality of main components of volatile organic gas in the expandable microspheres obtained in the step S1, wherein the volatile organic gas in the expandable microspheres comprises isopentane, isooctane, ethanol and acrylonitrile;
s3, preparation of a mixed standard working solution: mixing pure standard substances of isopentane, isooctane, ethanol and acrylonitrile, dissolving the mixture into toluene to prepare a series of mixed standard working solutions with a series of concentrations, wherein the concentrations of the isopentane in the mixed standard working solutions with the series of concentrations are respectively 0.005, 0.01, 0.025, 0.05 and 0.1g/ml, the concentrations of the isooctane in the mixed standard working solutions with the series of concentrations are respectively 0.0025, 0.005, 0.01, 0.025 and 0.05g/ml, the concentrations of the ethanol in the mixed standard working solutions with the series of concentrations are respectively 0.005, 0.01, 0.025, 0.05 and 0.1g/ml, and the concentrations of the acrylonitrile in the mixed standard working solutions with the series of concentrations are respectively 0.01, 0.02, 0.05, 0.1 and 0.2 g/ml;
s4, quantitative detection: under the same conditions, the mixed standard working solutions with the series of concentrations are respectively extracted by a 1 mu L sample injection needle by hand to 0.1 mu L for the Sammer fly Trace1300 gas chromatography test, data are collected, a standard curve is determined, and the slope and the intercept are calculated; taking out the headspace bottle after the pretreatment (placing in a 50 ℃ oven for 14 days) is finished, manually extracting 1ml of gas above the headspace bottle by using a 1ml sample injection needle, collecting data, and finding out the concentration of the component to be detected from a standard curve according to the signal of the component to be detected or calculating by using a regression equation; wherein, the gas chromatography conditions are as follows: the temperature raising procedure is that the initial temperature is 50 ℃, the temperature is kept for 3min, then the temperature is raised to 200 ℃ at the speed of 10 ℃/min, the temperature of a sample inlet is 200 ℃, the sample feeding mode is split flow, and the split flow ratio is 30; the sample introduction mode is flow splitting; the chromatographic column adopts a polyethylene glycol chromatographic column with the model of TG-WAXMS, and the specification of the chromatographic column is 30m x 0.32mm x 0.25 mu m; the carrier gas is nitrogen, and the constant-current mode is 1.2 ml/min; the detector used is a hydrogen flame ionization detector, the analysis temperature of the hydrogen flame ionization detector is 220 ℃, the flow rate of the used hydrogen is 35ml/min, and the flow rate of the air is 350 ml/min.
And (4) analyzing results: the results show that the major VOC species are all able to form an effective separation. And (4) carrying out quantitative analysis on the detection result by an external standard method of gas chromatography. Calculating the concentration (g/ml) of each substance through a standard curve equation of an external standard method of each substance, and obtaining the content of different volatile organic compounds in the microspheres by using a formula (1):
wherein, w is the content of volatile organic compounds in the microspheres, and the content is mu g/g;
c-concentration of each substance, g/ml, obtained using a standard curve;
m-mass of microsphere sample placed in the headspace bottle.
And VOC volume fraction (%) calculation formula (2):
v is volume fraction of volatile organic compounds in the microspheres,%;
c-concentration of each substance, g/ml, obtained using a standard curve;
ρ -relative density of each VOC substance (air 1), kg/m3。
(the relative gas densities of isopentane, isooctane, ethanol, and acrylonitrile were 2.48, 3.9, 1.59, and 1.83kg/m, respectively3。)
Example 3 the results are shown in table 3:
TABLE 3
| VOC example 3 | Concentration c (g/ml) | Content w (μ g/g) | Volume fraction v (%) |
| Isopentane | 0.070324961 | 23.56734623 | 0.283568392 |
| Isooctane | 0.016895521 | 5.662037891 | 0.043321849 |
| Ethanol | 0.011887555 | 3.983764941 | 0.074764494 |
| Acrylonitrile | 0.16700202 | 55.96582442 | 0.912579345 |
Example 4
The quantitative analysis method for volatile organic compounds provided by the embodiment comprises the following steps:
s1, pretreatment of a test sample: placing expandable microspheres into a headspace bottle, wherein the addition amount of the expandable microspheres accounts for 50% of the volume of the headspace bottle, weighing by a balance, recording the mass of the expandable microspheres to be 4.7636g, tightly covering the headspace bottle by using a jaw bottle cap, forming a sealed space inside the headspace bottle, and placing in an oven at the temperature of 50 ℃ for 14 days to obtain volatile organic gas in the expandable microspheres;
s2, qualitative detection: adopting a gas chromatography-mass spectrometer, wherein the gas chromatography conditions are as follows: the temperature raising procedure is that the initial temperature is 40 ℃, the temperature is kept for 4min, then the temperature is raised to 200 ℃ at the speed of 10 ℃/min, the temperature of a sample inlet is 200 ℃, the sample feeding mode is split flow, and the split flow ratio is 30; the sample introduction mode is flow splitting; the chromatographic column adopts a polyethylene glycol chromatographic column with the model of TG-WAXMS, and the specification of the chromatographic column is 30m x 0.32mm x 0.25 mu m; the carrier gas is nitrogen, and the constant-current mode is 1.2 ml/min; the detector is a hydrogen flame ionization detector, the analysis temperature of the hydrogen flame ionization detector is 220 ℃, the flow rate of the used hydrogen is 35ml/min, and the flow rate of the air is 350 ml/min; setting the solvent delay of a mass spectrometer to be 0min, and scanning the Scan ions to be 29-500 amu; qualitatively analyzing a plurality of main components of volatile organic gas in the expandable microspheres obtained in the step S1, wherein the volatile organic gas in the expandable microspheres comprises isopentane, isooctane, ethanol and acrylonitrile;
s3, preparation of a mixed standard working solution: mixing pure standard substances of isopentane, isooctane, ethanol and acrylonitrile, dissolving the mixture into toluene to prepare a series of mixed standard working solutions with a series of concentrations, wherein the concentrations of the isopentane in the mixed standard working solutions with the series of concentrations are respectively 0.005, 0.01, 0.025, 0.05 and 0.1g/ml, the concentrations of the isooctane in the mixed standard working solutions with the series of concentrations are respectively 0.0025, 0.005, 0.01, 0.025 and 0.05g/ml, the concentrations of the ethanol in the mixed standard working solutions with the series of concentrations are respectively 0.005, 0.01, 0.025, 0.05 and 0.1g/ml, and the concentrations of the acrylonitrile in the mixed standard working solutions with the series of concentrations are respectively 0.01, 0.02, 0.05, 0.1 and 0.2 g/ml;
s4, quantitative detection: under the same conditions, respectively transferring 5ml to 20ml of the mixed standard working solution with the series of concentrations into a headspace bottle, tightly covering the headspace bottle with a headspace bottle cap, setting the sample injection amount to be 0.1 mu L by adopting a gas chromatography Saimei fly Trace1300, a CombipAL automatic sample injector and a liquid injector, collecting data, determining a standard curve, and solving the slope and the intercept; taking out the headspace bottle after the pretreatment (placing in a 50 ℃ oven for 14 days) is finished, placing the headspace bottle on a gas chromatography Sammer fly Trace1300, a CombipAl automatic sample injector, using a gas injector, setting the sample volume to be 1ml, collecting data, and checking the concentration of the component to be detected from a standard curve according to the signal of the component to be detected or calculating by using a regression equation; wherein, the gas chromatography conditions are as follows: the temperature raising procedure is that the initial temperature is 40 ℃, the temperature is kept for 4min, then the temperature is raised to 200 ℃ at the speed of 10 ℃/min, the temperature of a sample inlet is 200 ℃, the sample feeding mode is split flow, and the split flow ratio is 30; the sample introduction mode is flow splitting; the chromatographic column adopts a polyethylene glycol chromatographic column with the model of TG-WAXMS, and the specification of the chromatographic column is 30m x 0.32mm x 0.25 mu m; the carrier gas is nitrogen, and the constant-current mode is 1.2 ml/min; the detector used is a hydrogen flame ionization detector, the analysis temperature of the hydrogen flame ionization detector is 220 ℃, the flow rate of the used hydrogen is 35ml/min, and the flow rate of the air is 350 ml/min.
And (4) analyzing results: the results show that the major VOC species are all able to form an effective separation. And (4) carrying out quantitative analysis on the detection result by an external standard method of gas chromatography. Calculating the concentration (g/ml) of each substance through a standard curve equation of an external standard method of each substance, and obtaining the content of different volatile organic compounds in the microspheres by using a formula (1):
wherein, w is the content of volatile organic compounds in the microspheres, and the content is mu g/g;
c-concentration of each substance, g/ml, obtained using a standard curve;
m-mass of microsphere sample placed in the headspace bottle.
And VOC volume fraction (%) calculation formula (2):
v is volume fraction of volatile organic compounds in the microspheres,%;
c-concentration of each substance, g/ml, obtained using a standard curve;
ρ -relative density of each VOC substance (air 1), kg/m3。
(the relative gas densities of isopentane, isooctane, ethanol, and acrylonitrile were 2.48, 3.9, 1.59, and 1.83kg/m, respectively3。)
Example 4 the results are shown in table 4:
TABLE 4
| VOC example 4 | Concentration c (g/ml) | Content w (μ g/g) | Volume fraction v (%) |
| Isopentane | 0.08969451 | 32.0095448 | 0.361671413 |
| Isooctane | 0.022019173 | 7.8580474 | 0.056459419 |
| Ethanol | 0.010542303 | 3.762262982 | 0.066303796 |
| Acrylonitrile | 0.155709545 | 55.56852509 | 0.850871829 |
In the analytical method of the present invention, in order to measure volatile organic compounds in the expandable microspheres, volatile low-boiling-point substances in the microspheres are volatilized as completely as possible. Referring to the contents of the Association's handbook on the recommendation, test and Standard for transportation of dangerous goods' (Small orange book), the substance to be tested was filled in a bottle at a rate of 50% by volume, left at a temperature of at least 50 ℃ for 14 days, and then analyzed for the concentration of flammable gas using a gas chromatograph.
The analysis method uses a gas chromatography-mass spectrometer GCMS to qualitatively analyze VOC main components; according to the result of qualitative analysis, an external standard method is adopted for determination in quantitative analysis. Meanwhile, referring to the document of 'calibration of gas concentration by liquid marking line of gas chromatograph', it is found that under the same operating conditions, the absolute mass of a certain substance entering the instrument is in direct proportion to the peak area of a chromatographic peak generated by the substance. Under the condition that the operating parameters of the instrument are the same and the absolute mass of a certain substance entering the chromatographic column is the same, the sample introduction mode of the gas chromatograph, namely liquid sample introduction and gas sample introduction, is changed, and the peak areas of the finally obtained chromatographic peaks are the same. Therefore, when the quantitative analysis is carried out by adopting an external standard method, the liquid standard series samples are directly adopted for sample injection, and then a standard curve is made for subsequent sample analysis.
While the invention has been 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.
Claims (11)
1. The method for quantitatively analyzing the volatile organic compounds is characterized by comprising the following steps of:
s1, pretreatment of a test sample: placing expandable microspheres into a headspace bottle, recording the mass of the expandable microspheres, tightly covering the headspace bottle by using a jaw bottle cap, forming a sealed space inside the headspace bottle, and placing the headspace bottle in an oven at the temperature of at least 50 ℃ for more than 14 days to obtain volatile organic gas in the expandable microspheres;
s2, qualitative detection: qualitatively analyzing a plurality of main components of the volatile organic gas in the expandable microspheres obtained in the step S1 by using a gas chromatography-mass spectrometer;
s3, preparation of a mixed standard working solution: pure substances of a plurality of main components of volatile organic gas in the expandable microspheres detected in the step S2 are used as standard substances, and are dissolved in a solvent after being mixed to prepare a series of mixed standard working solutions with different concentrations;
s4, quantitative detection: and under the same conditions, respectively injecting the mixed standard working solution prepared in the step S3 and the volatile organic compound gas in the headspace bottle obtained through post-treatment in the step S1, performing gas chromatography test, collecting data and analyzing.
2. The method for quantitatively analyzing volatile organic compounds according to claim 1, wherein the filling amount of said expandable microspheres is 50% by volume of said headspace bottle at S1.
3. The method for quantitatively analyzing volatile organic compounds according to claim 1, wherein in S2, the volatile organic compounds in the expandable microspheres include isopentane, isooctane, ethanol and acrylonitrile.
4. The method for quantitatively analyzing volatile organic compounds according to claim 1, wherein the solvent used in S3 is toluene.
5. The method for quantitatively analyzing volatile organic compounds according to claim 1, wherein the mixed standard working solution is automatically or manually injected in S4 in an amount of 0.1 μ L.
6. The method for quantitatively analyzing volatile organic compounds according to claim 1, wherein in S4, the volatile organic compound gas is automatically or manually injected in an amount of 1 ml.
7. The method for quantitatively analyzing volatile organic compounds according to claim 1, wherein the gas chromatography conditions in S2 are as follows: temperature programming is carried out, the temperature of a sample inlet is 200 ℃, and the sample introduction mode is shunting; the chromatographic column adopts a polyethylene glycol chromatographic column with the model of TG-WAXMS; the carrier gas is nitrogen, and the constant current mode is adopted; the detector adopted is a hydrogen flame ionization detector; the solvent delay of the mass spectrometer used in conjunction with the gas chromatograph was set to 0min, and the Scan ion Scan range was 29-500 amu; in S4, the gas chromatography conditions were: temperature programming is carried out, the temperature of a sample inlet is 200 ℃, and the sample introduction mode is shunting; the chromatographic column adopts a polyethylene glycol chromatographic column with the model of TG-WAXMS; the carrier gas is nitrogen, and the constant current mode is adopted; the detector used was a hydrogen flame ionization detector.
8. The method for quantitatively analyzing volatile organic compounds according to claim 7, wherein the temperature rising program used in the gas chromatography in both of S2 and S4 is: the initial temperature is 35-50 ℃, and the holding time is 3-5 min; then increased to 200 ℃ at a rate of 10 ℃/min.
9. The method of claim 7, wherein the size of the chromatographic columns in each of S2 and S4 is 30m 0.32mm 0.25 μm.
10. The method for quantitatively analyzing volatile organic compounds according to claim 7, wherein the split ratios of both of S2 and S4 are 30; the flow rate of the nitrogen gas was 1.2 ml/min.
11. The method of claim 7, wherein the hydrogen flame ionization detector has a temperature of 220 ℃, a flow rate of 35ml/min hydrogen gas, and a flow rate of 350ml/min air in each of S2 and S4.
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