CN111537640A - Multipurpose VOC (volatile organic compound) combined detection method - Google Patents
Multipurpose VOC (volatile organic compound) combined detection method Download PDFInfo
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- CN111537640A CN111537640A CN202010420036.0A CN202010420036A CN111537640A CN 111537640 A CN111537640 A CN 111537640A CN 202010420036 A CN202010420036 A CN 202010420036A CN 111537640 A CN111537640 A CN 111537640A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/16—Injection
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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
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/38—Flow patterns
- G01N30/46—Flow patterns using more than one column
- G01N30/461—Flow patterns using more than one column with serial coupling of separation columns
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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
- G01N30/48—Sorbent materials therefor
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/64—Electrical detectors
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/64—Electrical detectors
- G01N2030/642—Electrical detectors photoionisation detectors
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/40—Capture or disposal of greenhouse gases of CO2
Abstract
The embodiment of the invention provides a multipurpose VOC combined detection method, which comprises the following steps: a. collecting gas: feeding the gas to be detected into a detection device through an air inlet pump; b. primary cold trap treatment: the gas to be measured enters a primary cold trap arranged in a primary electric refrigeration chamber, and water and VOC in the gas to be measured are left; when the volume of the gas to be detected reaches the requirement, pushing the primary cold trap into a primary electric heating chamber, raising the temperature of the primary cold trap, and expelling the VOC gas; c. secondary cold trap treatment: b, enabling the VOC gas obtained in the step b to enter a secondary cold trap arranged in a secondary electric refrigerating chamber, condensing the VOC gas, pushing the secondary cold trap into a secondary electric heating chamber after the volume of the gas reaches the required volume, increasing the temperature of the secondary cold trap, and expelling the VOC gas; gc analysis: c, enabling the obtained VOC gas to enter an analytical column, and separating and qualifying the VOC gas; and e, PID analysis: the VOC gas inflow from the GC was quantitatively detected using PID. Meanwhile, the invention has the characteristic of simplifying operation.
Description
Technical Field
The invention relates to the technical field of automobiles, in particular to a multipurpose VOC combined detection method.
Background
Due to the ecological requirements of environmental protection and health, the VOC detection is increasingly required in various occasions such as the atmosphere, the indoor environment, the interior of a vehicle and the like. The existing detection means mainly comprise laboratory fixed equipment, and have the disadvantages of large volume, long time, high requirement and complex detection procedure. The accuracy and stability of the portable detection equipment are poor. The development of a novel multipurpose detection device solves the problem of the existing detection device very urgently.
The invention patent of an olfactory enhancer based on a preconcentration principle concentrates gas in an electronic semiconductor refrigeration and heating mode to evaluate odor, but only first-level concentration is carried out and only used for evaluating odor. The invention patent of on-line atmosphere pre-concentration device only has first-level concentration, the effect is limited, and the invention patent does not have the capacity of back-end gas separation and quantitative and qualitative detection of gas. The three-stage cold trap preconcentration detection method of the laboratory uses three-stage cold concentration and liquid nitrogen cooling, and has large volume, portability and expensive equipment.
Disclosure of Invention
The VOC's mentioned in the present invention: volatile organic compounds, commanding organic compounds; GC: GasChromatography, gas chromatography; PID: photo ionization Detector, which refers to a photo ionization Detector; tenax: Tenax-TA is a 2, 6-diphenylfuran porous polymer resin.
The invention provides a multipurpose VOC joint detection method, which at least solves the problems of large equipment volume and complex operation in the prior art.
To solve the above technical problem, an embodiment of the present invention provides the following solutions:
a multipurpose VOC combined detection method comprises the following steps:
a. collecting gas: feeding the gas to be detected into a detection device through an air inlet pump;
b. primary cold trap treatment: the gas to be measured enters a primary cold trap arranged in a primary electric refrigeration chamber, water and VOC in the gas to be measured are left, and carbon dioxide is released; when the volume of the gas to be detected entering the primary cold trap reaches the requirement, automatically pushing the primary cold trap into a primary electric heating chamber, raising the temperature of the primary cold trap to 240 ℃ by adjusting a temperature raising program, and expelling the VOC gas and water vapor;
c. secondary cold trap treatment: b, enabling the VOC gas and the water vapor obtained in the step b to enter a secondary cold trap arranged in a secondary electric refrigeration chamber, condensing the VOC gas and the water vapor, automatically pushing the secondary cold trap into a secondary electric heating chamber after the volume of the gas entering the secondary cold trap reaches the required volume, heating the temperature of the secondary cold trap to 10-60 ℃ by adjusting a heating program, and expelling the VOC gas out;
gc analysis: c, enabling the obtained VOC gas to enter an analytical column, and separating and qualifying the VOC gas;
and e, PID analysis: the VOC gas inflow from the GC was quantitatively detected using PID.
Optionally, in the step b, the internal temperature of the primary cold trap placed in the primary electric refrigerating chamber is 30-55 ℃.
Optionally, in the step c, the internal temperature of the secondary cold trap disposed in the secondary electric refrigerating chamber is ≦ 130 ℃.
Optionally, in the step b, an adsorbent is filled inside the primary cold trap.
Optionally, in the step b, the adsorbent is formed by mixing silica gel, activated carbon and Tenax.
Optionally, in the step c, the secondary cold trap is an empty trap.
Optionally, in the step d, the analytical column is formed by connecting a polar chromatographic column and a non-polar chromatographic column in series.
Optionally, the lengths of the polar chromatographic column and the nonpolar chromatographic column are both ≧ 30 m.
Optionally, in the step b, the primary electric refrigerating chamber and the primary electric warming chamber are in a common chamber or a different chamber.
Optionally, in the step c, the primary electric refrigerating chamber and the primary electric warming chamber are in a common chamber or a different chamber.
The scheme of the invention at least comprises the following beneficial effects:
the scheme of the invention realizes the effects of reduced equipment volume, short detection time, low environmental requirement, complete device function and accurate result; the device is suitable for various scenes in the air, indoors, in the vehicle and the like, can be used for VOC and odor detection, analysis and control, and has wide application range; can be customized according to laboratory fixed equipment and portable mobile equipment; meanwhile, the cost of the detection equipment is reduced.
Drawings
FIG. 1 is a schematic view of a first structure of a heating chamber and a cooling chamber of a detection device used in a multi-purpose VOC combined detection method provided by the invention;
FIG. 2 is a schematic view of a second structure of the heating chamber and the cooling chamber of the detection device used in the multi-purpose VOC combined detection method provided by the invention;
FIG. 3 is a schematic view of a third structure of the detection device used in the multi-purpose VOC combined detection method, wherein the heating chamber and the cooling chamber are arranged in different chambers;
fig. 4 is a schematic structural diagram of the detection device used in the multi-purpose VOC combined detection method with the same heating chamber and cooling chamber.
Detailed Description
Exemplary embodiments of the present disclosure will be described in more detail below with reference to the accompanying drawings. While exemplary embodiments of the present disclosure are shown in the drawings, it should be understood that the present disclosure may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art.
As shown in fig. 1 to 4, the present invention provides a multi-purpose VOC combined detection method, comprising the following steps:
a. collecting gas: feeding the gas to be detected into a detection device through an air inlet pump;
b. primary cold trap treatment: the gas to be detected enters a primary cold trap arranged in a primary electric refrigerating chamber, an adsorbent is filled in the primary cold trap, the adsorbent is a mixture of silica gel, activated carbon and Tenax, and impurities, peculiar smell and the like are adsorbed; the internal temperature of the primary cold trap is 30 ℃ below zero; water and VOC in the gas to be detected are left, and carbon dioxide is released; when the volume of the gas to be detected entering the first-stage cold trap reaches the requirement, automatically pushing the first-stage cold trap into a first-stage electric heating chamber, raising the temperature of the first-stage cold trap to 200 ℃ by adjusting a temperature raising program, and expelling the VOC gas and water vapor out;
c. secondary cold trap treatment: the VOC gas and the water vapor obtained in the step b enter a secondary cold trap arranged in a secondary electric refrigerating chamber, the secondary cold trap is an empty trap, and the temperature in the secondary cold trap is 130 ℃ below zero; condensing VOC gas and water vapor, automatically pushing the secondary cold trap into a secondary electric heating chamber when the volume of the gas entering the secondary cold trap reaches the required volume, and heating the temperature of the secondary cold trap to 10 ℃ by adjusting a heating program to expel the VOC gas;
gc analysis: c, enabling the VOC gas obtained in the step c to enter an analytical column, wherein the analytical column is formed by connecting a polar chromatographic column and a non-polar chromatographic column in series; separating and determining the nature of the VOC gas; and recording the information of retention time, peak area, sequence and the like of each gas. For more complete separation, the length of both the polar and non-polar columns was 30 m.
And e, PID analysis: quantitatively detecting the VOC gas flowing in from the GC by using PID; the information of retention time, peak area, order, etc. of each gas was recorded.
The scheme of the invention realizes the effects of reduced equipment volume, short detection time, low environmental requirement, complete device function and accurate result, and has wide application range.
As an alternative embodiment of the present invention, the present invention provides a multipurpose VOC combined detection method, comprising the steps of:
a. collecting gas: feeding the gas to be detected into a detection device through an air inlet pump;
b. primary cold trap treatment: the gas to be detected enters a primary cold trap arranged in a primary electric refrigerating chamber, an adsorbent is filled in the primary cold trap, the adsorbent is a mixture of Tenax and other adsorbents, and impurities, peculiar smell and the like are adsorbed by selecting the type of the adsorbent according to the requirement; the internal temperature of the primary cold trap is 55 ℃ below zero; water and VOC in the gas to be detected are left, and carbon dioxide is released; when the volume of the gas to be detected entering the first-stage cold trap reaches the requirement, automatically pushing the first-stage cold trap into a first-stage electric heating chamber, raising the temperature of the first-stage cold trap to 240 ℃ by adjusting a temperature raising program, and expelling the VOC gas and water vapor out;
c. secondary cold trap treatment: the VOC gas and the water vapor obtained in the step b enter a secondary cold trap arranged in a secondary electric refrigerating chamber, the secondary cold trap is an empty trap, and the temperature in the secondary cold trap is 130 ℃ below zero; condensing the VOC gas and water vapor, automatically pushing the secondary cold trap into a secondary electric heating chamber when the volume of the gas entering the secondary cold trap reaches the required volume, and heating the temperature of the secondary cold trap to 60 ℃ by adjusting a heating program to expel the VOC gas;
gc analysis: c, enabling the VOC gas obtained in the step c to enter an analytical column, wherein the analytical column is formed by connecting a polar chromatographic column and a non-polar chromatographic column in series; separating and determining the nature of the VOC gas; and recording the information of retention time, peak area, sequence and the like of each gas. For more complete separation, the length of both the polar and non-polar columns was 35 m.
And e, PID analysis: quantitatively detecting the VOC gas flowing in from the GC by using PID; the information of retention time, peak area, order, etc. of each gas was recorded.
As an alternative embodiment of the present invention, the present invention provides a multipurpose VOC combined detection method, comprising the steps of:
a. collecting gas: feeding the gas to be detected into a detection device through an air inlet pump;
b. primary cold trap treatment: the gas to be detected enters a primary cold trap arranged in a primary electric refrigerating chamber, an adsorbent is filled in the primary cold trap, the adsorbent is a mixture of silica gel, activated carbon and Tenax, and impurities, peculiar smell and the like are adsorbed; the internal temperature of the primary cold trap is minus 40 ℃; water and VOC in the gas to be detected are left, and carbon dioxide is released; when the volume of the gas to be detected entering the first-stage cold trap reaches the requirement, automatically pushing the first-stage cold trap into a first-stage electric heating chamber, raising the temperature of the first-stage cold trap to 220 ℃ by adjusting a temperature raising program, and expelling the VOC gas and water vapor out;
c. secondary cold trap treatment: the VOC gas and the water vapor obtained in the step b enter a secondary cold trap arranged in a secondary electric refrigerating chamber, the secondary cold trap is an empty trap, and the temperature in the secondary cold trap is 130 ℃ below zero; condensing the VOC gas and water vapor, automatically pushing the secondary cold trap into a secondary electric heating chamber when the volume of the gas entering the secondary cold trap reaches the required volume, and heating the temperature of the secondary cold trap to 20 ℃ by adjusting a heating program to expel the VOC gas;
gc analysis: c, enabling the VOC gas obtained in the step c to enter an analytical column, wherein the analytical column is formed by connecting a polar chromatographic column and a non-polar chromatographic column in series; separating and determining the nature of the VOC gas; and recording the information of retention time, peak area, sequence and the like of each gas. For more complete separation, the length of both the polar and non-polar columns was 40 m.
And e, PID analysis: quantitatively detecting the VOC gas flowing in from the GC by using PID; the information of retention time, peak area, order, etc. of each gas was recorded.
The scheme of the invention is suitable for various scenes required in the atmosphere, indoors, in a vehicle and the like, and can be used for VOC and odor detection, analysis and control; can be customized according to laboratory fixed equipment and portable mobile equipment; meanwhile, the cost of the detection equipment is reduced.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. A multipurpose VOC combined detection method is characterized by comprising the following steps:
a. collecting gas: feeding the gas to be detected into a detection device through an air inlet pump;
b. primary cold trap treatment: the gas to be measured enters a primary cold trap arranged in a primary electric refrigeration chamber, water and VOC in the gas to be measured are left, and carbon dioxide is released; when the volume of the gas to be detected entering the primary cold trap reaches the requirement, pushing the primary cold trap into a primary electric heating chamber, and raising the temperature of the primary cold trap to 240 ℃ by adjusting a temperature raising program to expel the VOC gas and water vapor;
c. secondary cold trap treatment: b, enabling the VOC gas and the water vapor obtained in the step b to enter a secondary cold trap arranged in a secondary electric refrigeration chamber, condensing the VOC gas and the water vapor, pushing the secondary cold trap into a secondary electric heating chamber after the volume of the gas entering the secondary cold trap reaches the required volume, heating the temperature of the secondary cold trap to 10-60 ℃ by adjusting a heating program, and expelling the VOC gas;
gc analysis: c, enabling the obtained VOC gas to enter an analytical column, and separating and qualifying the VOC gas;
and e, PID analysis: the VOC gas inflow from the GC was quantitatively detected using PID.
2. The method for multipurpose VOC joint detection of claim 1, wherein in step b, the internal temperature of said primary cold trap placed in said primary electric refrigerator is-30-55 ℃.
3. The method for multipurpose VOC joint detection of claim 2, wherein in step c, the internal temperature of said secondary cold trap placed in said secondary electric refrigeration chamber is ≦ 130 ℃.
4. The multipurpose VOC joint detection method according to claim 3, wherein in the step b, an adsorbent is filled in the primary cold trap.
5. The method for multipurpose joint VOC detection as claimed in claim 4, wherein in step b, said adsorbent is a mixture of silica gel, activated carbon and Tenax.
6. The method for multipurpose VOC joint detection of claim 5 wherein in step c, said secondary cold trap is an empty trap.
7. The method for multipurpose joint VOC detection as claimed in claim 6, wherein in step d, said analytical column is composed of a polar chromatographic column and a non-polar chromatographic column connected in series.
8. The multi-purpose VOC joint detection method according to claim 7, wherein the polar chromatography column and the non-polar chromatography column are each ≧ 30m in length.
9. The method for the combined detection of multipurpose VOCs as claimed in any one of claims 1 to 8, wherein in step b, said primary electric cooling chamber and said primary electric warming chamber are co-chamber or separate chamber.
10. The method for the combined detection of multipurpose VOCs as claimed in any one of claims 1 to 8, wherein in step c, said primary electric cooling chamber and said primary electric warming chamber are co-chamber or separate chamber.
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