CN112816310A - Detection device and method for semi-volatile organic compounds based on solid-phase extraction - Google Patents
Detection device and method for semi-volatile organic compounds based on solid-phase extraction Download PDFInfo
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- CN112816310A CN112816310A CN202011617415.5A CN202011617415A CN112816310A CN 112816310 A CN112816310 A CN 112816310A CN 202011617415 A CN202011617415 A CN 202011617415A CN 112816310 A CN112816310 A CN 112816310A
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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
- G01N1/4055—Concentrating samples by solubility techniques
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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
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/24—Suction devices
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
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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
- G01N1/4055—Concentrating samples by solubility techniques
- G01N2001/4061—Solvent extraction
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Abstract
The invention provides a detection device and a detection method for semi-volatile organic compounds based on solid-phase extraction, wherein the detection device for semi-volatile organic compounds based on solid-phase extraction comprises a closed sample cell and an analyzer; the first switching module is used for enabling the inlet of the processing pool to be selectively communicated with the outlet of the sample pool and the carrier gas; the closed treatment tank is provided with an inlet, an outlet and an opening, the opening is suitable for inserting a solid phase micro-extraction kit, and an extraction piece arranged on the solid phase micro-extraction kit is positioned in the treatment tank; the heating unit is used for heating the sample cell and the processing cell; a second switching module is connected to the outlet for selectively communicating the outlet with the pump and the analyzer. The invention has the advantages of low cost, accuracy and the like.
Description
Technical Field
The invention relates to organic matter detection, in particular to a device and a method for detecting semi-volatile organic matters based on solid-phase extraction.
Background
The solid phase microextraction technology has been widely applied to analysis of semi-volatile organic compounds (SVOCs), but most of them adopts manual sample injection mode, and the manual sample injection of solid phase microextraction is most commonly Supelco sample injection kit, and said sample injection kit is convenient and easy to use, and can change the extraction fibre according to the property of tested object, but said manual sample injection kit has need of three processes of extraction, sample injection and ageing when making sample analysis, and the manual sample injection mode and solid phase microextraction technology design can determine that the analysis result can produce large difference due to different operators. Need artificial six times of plugs at extraction, advance kind and ageing three process, not only can lead to the analysis result to receive the operation number of times influence of plug, the repeatability is poor, also can make extremely easily remain in the steel pipe protective sheath of handle because the thin garrulous of the shock insulator that the plug brought out of, influences the fibre durability. Meanwhile, in the extraction process, as the extraction fibers are directly inserted above the water sample, the volatilized water vapor can occupy adsorption sites on the fibers, so that the analysis result is influenced.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a detection device for semi-volatile organic compounds based on solid-phase extraction.
The purpose of the invention is realized by the following technical scheme:
the detection device for the semi-volatile organic compound based on the solid-phase extraction comprises a closed sample cell and an analyzer; the detection device further comprises:
a first switching module for selectively communicating an inlet of a process cell with an outlet of the sample cell and a carrier gas;
a closed treatment cell having an inlet, an outlet and an opening adapted for insertion of a solid phase microextraction kit, an extraction element disposed on said solid phase microextraction kit being located within said treatment cell;
a heating unit for heating the sample cell and the processing cell;
a second switching module connected to the outlet for selectively communicating the outlet with the pump and the analyzer.
The invention also aims to provide a detection method of semi-volatile organic compounds based on solid-phase extraction, which is realized by the following technical scheme:
the detection method of the semi-volatile organic compound based on the solid phase extraction comprises the following steps:
the first switching module and the second switching module are switched, carrier gas enters the treatment pool through the first switching module, and gas in the treatment pool is replaced and discharged from the second switching module and the pump;
heating the sample in the sample cell to release semi-volatile organic compounds;
the first switching module is switched, the semi-volatile organic compounds are discharged from the sample pool, enter the processing pool through the first switching module and are extracted by an extracting piece inserted into the processing pool;
heating the treatment tank, and desorbing the target substance on the extraction element;
the first switching module and the second switching module are switched, and carrier gas enters the processing pool through the first switching module, carries the desorbed target substance, and enters the analysis instrument through the second switching module.
Compared with the prior art, the invention has the beneficial effects that:
1. automation;
by utilizing the technical scheme, the automatic extraction, desorption and sample introduction processes of pretreatment by utilizing the solid phase microextraction kit are realized through the switching of the first switching module and the second switching module, and the repeatability of the solid phase microextraction manual sample introduction kit is improved;
2. the service life is long;
after the extraction piece such as the extraction fiber is inserted into the treatment tank, the extraction, desorption and sample injection are automatically carried out, thereby avoiding unnecessary damage of the extraction fiber caused by repeated plugging and unplugging and prolonging the service life;
3. the detection is accurate;
set up the dewatering module between the import of first switching module and processing pond, gas must pass through the dewatering step before getting into the processing pond for the gas that gets into in the processing pond does not contain the moisture, greatly reduced steam to extraction fibre adsorption performance's influence, ensured the accuracy that detects.
Drawings
The disclosure of the present invention will become more readily understood with reference to the accompanying drawings. As is readily understood by those skilled in the art: these drawings are only for illustrating the technical solutions of the present invention and are not intended to limit the scope of the present invention. In the figure:
FIG. 1 is a schematic structural diagram of an apparatus for detecting semi-volatile organic compounds based on solid-phase extraction according to an embodiment of the present invention.
Detailed Description
Fig. 1 and the following description depict alternative embodiments of the invention to teach those skilled in the art how to make and reproduce the invention. Some conventional aspects have been simplified or omitted for the purpose of teaching the present invention. Those skilled in the art will appreciate that variations or substitutions from these embodiments will be within the scope of the invention. Those skilled in the art will appreciate that the features described below can be combined in various ways to form multiple variations of the invention. Thus, the present invention is not limited to the following alternative embodiments, but is only limited by the claims and their equivalents.
Example 1:
fig. 1 is a schematic structural diagram of an apparatus for detecting semi-volatile organic compounds based on solid-phase extraction according to an embodiment of the present invention, as shown in fig. 1, the apparatus for detecting semi-volatile organic compounds based on solid-phase extraction includes:
closed sample cells and analyzers, these components being prior art in the field;
a first switching module for selectively communicating an inlet of a process cell with an outlet of the sample cell and a carrier gas;
a closed treatment cell having an inlet, an outlet and an opening adapted for insertion of a solid phase microextraction kit 11, an extraction element provided on said solid phase microextraction kit 11 being located within said treatment cell;
a heating unit for heating the sample cell and the processing cell;
a second switching module connected to the outlet for selectively communicating the outlet with the pump and the analyzer.
In order to prevent moisture from entering the processing tank to affect extraction, the detection device further comprises:
and the water removal module is arranged between the first switching module and an inlet of the treatment pool.
In order to achieve harmless emission, further, the detection device further comprises:
a purifier disposed downstream of the pump.
In order to increase the release rate of the semi-volatile organic compounds, further, the detection device further comprises:
an agitator for agitating gas within the sample cell.
To achieve desorption, further, the detection device further includes:
a valve disposed between the outlet of the treatment basin and the second switching module.
The detection method of the solid-phase extraction-based semi-volatile organic compound according to the embodiment of the present invention, that is, the working method of the detection apparatus according to the embodiment of the present invention, includes:
the first switching module and the second switching module are switched, so that carrier gas enters the treatment pool through the first switching module, the gas in the treatment pool is replaced, and the gas is discharged from the second switching module and the pump;
heating the sample in the sample cell to release semi-volatile organic compounds;
the first switching module is switched, the semi-volatile organic compounds are discharged from the sample pool, enter the processing pool through the first switching module and are extracted by an extracting piece inserted into the processing pool;
heating the treatment tank, and desorbing the target substance on the extraction element;
the first switching module and the second switching module are switched, and carrier gas enters the processing pool through the first switching module, carries the desorbed target substance, and enters the analysis instrument through the second switching module.
In order to prevent water vapor from entering the processing pool to influence extraction, carrier gas and semi-volatile organic compounds discharged from the sample pool enter the processing pool after physical dehydration.
In order to achieve desorption, furthermore, during desorption, a valve provided between the treatment cell and the second switching module is closed.
Example 2:
an application example of the device and the method for detecting semi-volatile organic compounds based on solid-phase extraction in embodiment 1 of the present invention.
In this application example, as shown in fig. 1, the first switching module and the second switching module adopt two-position three-way valves; the carrier gas passes through the filter and the flow controller and then is connected with the first switching module; a physical dehydrator is arranged between the first switching module and the inlet of the treatment pool; a valve is arranged between the outlet of the treatment pool and the second switching module; one outlet of the second switching module is communicated with the analyzer, and the other outlet of the second switching module is communicated with the pump and the purifier; the solid phase micro-extraction kit 11 is inserted into the treatment tank, the sealing is kept between the kit and the treatment tank, the extraction piece is arranged at the bottom end of the kit, and extraction fibers are adopted; agitation is used to agitate the sample within the sample cell.
The detection method of the semi-volatile organic compound based on the solid phase extraction in the embodiment specifically comprises the following steps:
the first switching module and the second switching module are switched, so that carrier gas sequentially passes through the filter, the flow controller, the first switching module and the dehydrator and enters the treatment pool, and gas in the treatment pool is replaced by the carrier gas without water vapor and is discharged from the second switching module, the pump and the purifier;
heating and stirring the sample in the sample cell to release semi-volatile organic compounds;
the first switching module is switched, the semi-volatile organic compounds are discharged from the sample pool, sequentially pass through the first switching module and the dehydrator, enter the treatment pool and are extracted by an extraction part inserted into the treatment pool;
closing the valve, heating the treatment tank, and desorbing the target substance on the extraction element;
the first switching module and the second switching module are switched, the valve is opened, and carrier gas sequentially passes through the filter, the flow controller, the first switching module and the dehydrator, enters the treatment tank, carries the desorbed target substance, and enters the analysis instrument through the second switching module.
Claims (9)
1. The detection device for the semi-volatile organic compound based on the solid-phase extraction comprises a closed sample cell and an analyzer; characterized in that, the detection device further comprises:
a first switching module for selectively communicating an inlet of a process cell with an outlet of the sample cell and a carrier gas;
a closed treatment cell having an inlet, an outlet and an opening adapted for insertion of a solid phase microextraction kit, an extraction element disposed on said solid phase microextraction kit being located within said treatment cell;
a heating unit for heating the sample cell and the processing cell;
a second switching module connected to the outlet for selectively communicating the outlet with the pump and the analyzer.
2. The apparatus for detecting semi-volatile organic compounds based on solid-phase extraction according to claim 1, further comprising:
and the water removal module is arranged between the first switching module and an inlet of the treatment pool.
3. The apparatus for detecting semi-volatile organic compounds based on solid-phase extraction according to claim 1, further comprising:
a purifier disposed downstream of the pump.
4. The apparatus for detecting semi-volatile organic compounds based on solid-phase extraction according to claim 1, further comprising:
an agitator for agitating gas within the sample cell.
5. The apparatus for detecting semi-volatile organic compounds based on solid phase extraction of claim 1, wherein the carrier gas is filtered and controlled to flow to the first switching module.
6. The apparatus for detecting semi-volatile organic compounds based on solid-phase extraction according to claim 1, further comprising:
a valve disposed between the outlet of the treatment basin and the second switching module.
7. The detection method of the semi-volatile organic compound based on the solid phase extraction comprises the following steps:
the first switching module and the second switching module are switched, carrier gas enters the treatment pool through the first switching module, and gas in the treatment pool is replaced and discharged from the second switching module and the pump;
heating the sample in the sample cell to release semi-volatile organic compounds;
the first switching module is switched, the semi-volatile organic compounds are discharged from the sample pool, enter the processing pool through the first switching module and are extracted by an extracting piece inserted into the processing pool;
heating the treatment tank, and desorbing the target substance on the extraction element;
the first switching module and the second switching module are switched, and carrier gas enters the processing pool through the first switching module, carries the desorbed target substance, and enters the analysis instrument through the second switching module.
8. The method for detecting semi-volatile organic compounds based on solid phase extraction of claim 7, wherein the carrier gas and the semi-volatile organic compounds discharged from the sample cell enter the processing cell after physical dehydration.
9. The method for detecting semi-volatile organic compounds based on solid-phase extraction of claim 7, wherein a valve disposed between the processing tank and the second switching module is closed during desorption.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011617415.5A CN112816310A (en) | 2020-12-31 | 2020-12-31 | Detection device and method for semi-volatile organic compounds based on solid-phase extraction |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011617415.5A CN112816310A (en) | 2020-12-31 | 2020-12-31 | Detection device and method for semi-volatile organic compounds based on solid-phase extraction |
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| CN112816310A true CN112816310A (en) | 2021-05-18 |
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| CN202011617415.5A Withdrawn CN112816310A (en) | 2020-12-31 | 2020-12-31 | Detection device and method for semi-volatile organic compounds based on solid-phase extraction |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104458999A (en) * | 2014-12-26 | 2015-03-25 | 力合科技（湖南）股份有限公司 | Automatic organism analyzer |
| CN107290189A (en) * | 2016-03-31 | 2017-10-24 | 庞英明 | A kind of portable multi-mode sampler |
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2020
- 2020-12-31 CN CN202011617415.5A patent/CN112816310A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104458999A (en) * | 2014-12-26 | 2015-03-25 | 力合科技（湖南）股份有限公司 | Automatic organism analyzer |
| CN107290189A (en) * | 2016-03-31 | 2017-10-24 | 庞英明 | A kind of portable multi-mode sampler |
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Application publication date: 20210518 |