CN112945656A - Simple and portable online enrichment device and method - Google Patents
Simple and portable online enrichment device and method Download PDFInfo
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- CN112945656A CN112945656A CN201911266823.8A CN201911266823A CN112945656A CN 112945656 A CN112945656 A CN 112945656A CN 201911266823 A CN201911266823 A CN 201911266823A CN 112945656 A CN112945656 A CN 112945656A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/405—Concentrating samples by adsorption or absorption
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/42—Low-temperature sample treatment, e.g. cryofixation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
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Abstract
The invention discloses a simple and portable online enrichment device and a simple and portable online enrichment method. The method of the invention realizes enrichment detection of low-concentration or trace organic matters in the environment by combining the device with a flight time mass spectrum detection instrument through the principle of low-temperature enrichment and high-temperature analysis, improves the detection sensitivity of the instrument and widens the detection range. The device has the characteristics of small volume, simple composition, low cost and convenient carrying, and can be widely applied to online analysis and detection of gas samples in laboratories and field environments.
Description
Technical Field
The invention is mainly applied to the analysis of low-concentration organic matters in the environment, and particularly relates to a device and a method for enriching and detecting trace organic matters in the environment. The device has the characteristics of small volume, simple composition, low cost and convenient carrying, and can be widely applied to analysis and detection of gas samples in laboratories and field environments.
Background
With the continuous development of social economy, human beings continuously emit a large amount of organic pollutants including various volatile organic compounds to the natural environment depending on the existence in the production and living processes, and the toxic and harmful substances are commonly present in the atmosphere, water and soil environment, so that sudden environmental pollution accidents frequently occur. Therefore, the detection and research of organic substances in the environment are receiving wide attention. For the evaluation of pollution accidents, the traditional off-line analysis method comprises the procedures of on-site sampling, sample pretreatment, laboratory analysis and the like. The whole process is time-consuming and labor-consuming, and the pollution condition which changes rapidly is difficult to master, so that the emergency treatment requirement is difficult to meet. Meanwhile, the content of some organic matters in the environment is low, and the detection sensitivity of an analytical instrument is low, so that the requirements cannot be met during direct analysis.
Proper sample pretreatment can effectively improve the detection sensitivity and the analysis range of the instrument, and generally comprises adsorption tube sampling, container sampling, air bag sampling, solid-phase microextraction technology, membrane sample introduction technology and the like. The technologies and the methods need to be analyzed after pretreatment, belong to off-line technologies, and cannot reflect the real-time change process of organic matters in ambient air. The analysis range of membrane sample injection is limited, only substances with similar structures and performances can be analyzed, and the membrane replacement is complex. Therefore, based on the low-temperature enrichment-high-temperature desorption principle, the simple portable online enrichment device is developed. The gas is trapped on the cooled surface by reducing the temperature to be below the boiling point of a target object, and then the sample is analyzed after being heated, so that the detection sensitivity of the instrument is effectively improved, and the qualitative and quantitative analysis of low-concentration or trace organic matters in the environment is realized.
Disclosure of Invention
The invention is mainly applied to detecting low-concentration or trace organic matters in the environment after enriching, and adopts the following technical scheme:
a simple and portable online enrichment device and method comprises a halogen lamp, a fixing plate, glass wool, an enrichment tube semiconductor refrigerating sheet and a time-of-flight mass spectrometer. The halogen lamp is arranged at a position right above the center of the enrichment pipe, and the enrichment pipe is arranged on the fixing plate. Enrichment materials are filled in the enrichment pipe, and the different kinds of enrichment materials are separated by glass wool. The semiconductor refrigerating sheet is tightly attached to the fixing plate and arranged below the enrichment pipe. The time-of-flight mass spectrometer is connected to the outlet end of the enrichment pipe. The distance between the halogen lamp and the enrichment pipe is as close as possible, a groove is formed in the fixing plate and used for placing the enrichment pipe, and the size of the groove is slightly larger than that of the enrichment pipe, so that the enrichment pipe can be replaced conveniently. Two ends of the enrichment pipe are provided with two connectors which are respectively an air inlet and a carrier gas port. The center of the semiconductor refrigerating sheet, the center of the halogen lamp and the center of the enrichment tube are on the same axis.
When low-temperature enrichment is carried out, the semiconductor refrigerating piece is electrified, gas is adsorbed by the enrichment material through the enrichment pipe, and the semiconductor refrigerating piece is closed after the low-temperature enrichment is carried out for a certain time. And (3) turning on a halogen lamp for heating, analyzing the adsorbed sample at high temperature, carrying the sample by carrier gas, carrying the sample into time-of-flight mass spectrometry, turning off the halogen lamp after analysis is finished, and turning on a semiconductor refrigerating sheet for cooling.
The device small in size, conveniently carry, easy operation combine time of flight mass spectrometry to carry out analysis and detection, select different enrichment modes to different experimental conditions, have improved the sensitivity and the detection range of instrument greatly. The device and the method can realize the enrichment and the re-detection of low-concentration or trace compounds in the environment.
Drawings
FIG. 1 is a schematic diagram of a simple portable online enrichment apparatus and method; the device comprises a halogen lamp, a fixing plate 2, glass wool 3, an enrichment tube 4, a semiconductor refrigeration piece 5 and a time-of-flight mass spectrometer 6.
Detailed Description
The invention relates to a device which sequentially comprises a halogen lamp, a fixed plate, glass wool, an enrichment tube semiconductor refrigerating sheet and a time-of-flight mass spectrometer from left to right. The halogen lamp is arranged at a position right above the center of the enrichment pipe, and the enrichment pipe is arranged on the fixing plate. Enrichment materials are filled in the enrichment pipe, and the different kinds of enrichment materials are separated by glass wool. The semiconductor refrigerating sheet is tightly attached to the fixing plate and arranged below the enrichment pipe. The time-of-flight mass spectrometer is connected to the outlet end of the enrichment pipe. The distance between the halogen lamp and the enrichment pipe is as close as possible, a groove is formed in the fixing plate and used for placing the enrichment pipe, and the size of the groove is slightly larger than that of the enrichment pipe, so that the enrichment pipe can be replaced conveniently. Two ends of the enrichment pipe are provided with two connectors which are respectively an air inlet and a carrier gas port. The center of the semiconductor refrigerating sheet, the center of the halogen lamp and the center of the enrichment tube are on the same axis.
The enrichment device detection comprises two processes of low-temperature enrichment and high-temperature analysis, gas is adsorbed by an enrichment material after passing through an enrichment pipe after the semiconductor refrigeration piece is electrified, and the semiconductor refrigeration piece is closed after low-temperature enrichment for a certain time. And (3) turning on a halogen lamp for heating, analyzing the adsorbed sample at high temperature, carrying the sample by carrier gas, performing flight time mass spectrometry, and turning off the halogen lamp and turning on a semiconductor refrigerating sheet for rapid cooling after analysis.
The carrier gas can be connected during laboratory analysis, a sample analyzed at high temperature is carried to the time-of-flight mass spectrum, and if the flow of the carrier gas is larger than the sample input amount of the instrument, redundant gas is discharged through a tail gas port; otherwise, the tail gas port is sealed.
The operation is simpler in field analysis, and a carrier gas is not needed to carry the sample to the time-of-flight mass spectrum. And sealing the carrier gas inlet during enrichment, sealing the tail gas inlet after the enrichment is finished, and directly sucking the sample into an instrument for analysis by using a time-of-flight mass spectrum negative pressure sample injection mode for the sample analyzed at high temperature. And directly replacing the new enrichment tube after the single analysis is finished.
Claims (7)
1. The utility model provides a simple and easy portable online enrichment device which characterized in that:
the device comprises a halogen lamp (1), a heat conduction fixing plate (2), glass wool (3), an enrichment tube (4), a semiconductor refrigeration piece (5) and a time-of-flight mass spectrometer (6);
the halogen lamp (1) is arranged at a position right above the middle part of the enrichment pipe (4), and the enrichment pipe (4) is arranged on the heat conduction fixing plate (2); enrichment materials are filled in the enrichment pipe (3), and the semiconductor refrigerating sheet (6) is tightly attached to the lower surface of the fixing plate and arranged right below the middle part of the enrichment pipe (4); the cold end of the semiconductor refrigerating sheet (6) is attached to the lower surface of the heat conducting fixing plate below the middle part of the enrichment pipe (4), and the time-of-flight mass spectrometer (6) is connected to the outlet end of the enrichment pipe (4).
2. The simple portable online enrichment device of claim 1, wherein:
the heat conduction fixing plate (2) is provided with a groove, the left end and the right end of the groove are communicated with the left end face and the right end face of the heat conduction fixing plate, the groove is used for placing the enrichment pipe (4), the width of the groove is slightly larger than the radial size of the enrichment pipe (4), and the enrichment pipe (4) can be replaced conveniently; two ports are arranged at two ends of the enrichment pipe (4), one end of the enrichment pipe is respectively provided with an air inlet and a carrier gas port, and the other end of the enrichment pipe is respectively provided with a tail gas port and a flight time mass spectrometer (6) port; the geometric center of the cold end of the semiconductor refrigerating sheet (5) is on the same axis with the geometric center of the halogen lamp (1) and the geometric center of the enrichment material of the enrichment pipe (4).
3. The simple portable online enrichment device of claim 1, wherein:
the enrichment pipe (3) is filled with more than 2 different kinds of enrichment materials, the different kinds of enrichment materials are separated by glass wool (3), and two ends of the enrichment materials are plugged by the glass wool (3).
4. The simple portable online enrichment device of claim 1, wherein: the enrichment tube (4) is in the illumination range of the halogen lamp (1).
5. A method of detection using the apparatus of any of claims 1 to 4, wherein:
the detection of the enrichment device comprises two processes of low-temperature enrichment and high-temperature analysis, gas passes through the enrichment pipe (4) after the semiconductor refrigerating sheet (5) is electrified and is adsorbed by an enrichment material, and the semiconductor refrigerating sheet (5) is closed after low-temperature enrichment for a certain time; and (2) turning on the halogen lamp (1) to heat, resolving the adsorbed sample at high temperature, carrying the sample into a time-of-flight mass spectrometry (6) through a carrier gas, turning off the halogen lamp (1) after the analysis is finished, and simultaneously turning on the semiconductor refrigerating sheet (5) to rapidly cool.
6. The detection method according to claim 1, characterized in that:
the carrier gas can be connected during laboratory analysis, a sample analyzed at high temperature is carried to the time-of-flight mass spectrum (6), and if the flow of the carrier gas is larger than the sample input amount of an instrument, redundant gas is discharged through a tail gas port; otherwise, the tail gas port is sealed.
7. The detection method according to claim 1, characterized in that:
the operation is simpler in the field analysis, and a carrier gas is not needed to carry the sample to the time-of-flight mass spectrum (6); sealing a carrier gas inlet during enrichment, sealing a tail gas inlet after the enrichment is finished, and directly sucking a sample analyzed at high temperature into an instrument for analysis by utilizing a time-of-flight mass spectrum (6) negative pressure sample injection mode; and directly replacing the new enrichment tube after the single analysis is finished.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911266823.8A CN112945656A (en) | 2019-12-11 | 2019-12-11 | Simple and portable online enrichment device and method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911266823.8A CN112945656A (en) | 2019-12-11 | 2019-12-11 | Simple and portable online enrichment device and method |
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| CN112945656A true CN112945656A (en) | 2021-06-11 |
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| CN201911266823.8A Pending CN112945656A (en) | 2019-12-11 | 2019-12-11 | Simple and portable online enrichment device and method |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1867982A2 (en) * | 2006-06-15 | 2007-12-19 | SLS Micro Technology GmbH | Miniaturised gas chromatography analytic device with sample enrichment |
| CN102749302A (en) * | 2012-07-31 | 2012-10-24 | 宁波市环境监测中心 | Portable Fourier infrared spectrum detection device and detection method thereof |
| CN106645770A (en) * | 2015-11-03 | 2017-05-10 | 中国科学院大连化学物理研究所 | An on-line detector capable of continuous sample injection and application thereof |
| CN206546349U (en) * | 2017-01-16 | 2017-10-10 | 北京雪迪龙科技股份有限公司 | A kind of low concentration VOCs is enriched with resolver |
| CN109865309A (en) * | 2017-12-01 | 2019-06-11 | 中国科学院大连化学物理研究所 | A kind of enrichment of volatile organic trace compounds low temperature and Thermal desorption integration cold-trap |
| CN209264371U (en) * | 2018-09-21 | 2019-08-16 | 上海卫星装备研究所 | Volatile organic matter enriching apparatus based on semiconductor chilling plate |
-
2019
- 2019-12-11 CN CN201911266823.8A patent/CN112945656A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1867982A2 (en) * | 2006-06-15 | 2007-12-19 | SLS Micro Technology GmbH | Miniaturised gas chromatography analytic device with sample enrichment |
| CN102749302A (en) * | 2012-07-31 | 2012-10-24 | 宁波市环境监测中心 | Portable Fourier infrared spectrum detection device and detection method thereof |
| CN106645770A (en) * | 2015-11-03 | 2017-05-10 | 中国科学院大连化学物理研究所 | An on-line detector capable of continuous sample injection and application thereof |
| CN206546349U (en) * | 2017-01-16 | 2017-10-10 | 北京雪迪龙科技股份有限公司 | A kind of low concentration VOCs is enriched with resolver |
| CN109865309A (en) * | 2017-12-01 | 2019-06-11 | 中国科学院大连化学物理研究所 | A kind of enrichment of volatile organic trace compounds low temperature and Thermal desorption integration cold-trap |
| CN209264371U (en) * | 2018-09-21 | 2019-08-16 | 上海卫星装备研究所 | Volatile organic matter enriching apparatus based on semiconductor chilling plate |
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Application publication date: 20210611 |