CN113533599A - Underwater SVOCs analysis device and method - Google Patents
Underwater SVOCs analysis device and method Download PDFInfo
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- CN113533599A CN113533599A CN202110877171.2A CN202110877171A CN113533599A CN 113533599 A CN113533599 A CN 113533599A CN 202110877171 A CN202110877171 A CN 202110877171A CN 113533599 A CN113533599 A CN 113533599A
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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
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
Abstract
The invention provides an underwater SVOCs analysis device and a method, wherein the underwater SVOCs analysis device comprises a multi-way valve, a chromatographic column and an extraction unit, one end of the extraction unit is respectively communicated with a port of the multi-way valve and a sample inlet pipe, and the other end of the extraction unit is communicated with the port of the multi-way valve; further comprising: the sample introduction unit is used for positively feeding a water sample into the extraction unit and enabling the water sample to repeatedly move in the extraction unit in a positive direction and a reverse direction; two ends of the cutting unit are respectively communicated with the ports of the multi-way valve, and the hydrophobic material is arranged in the cutting unit; when the multi-way valve is switched to the first state, carrier gas enters the extraction unit through the multi-way valve and is discharged from the multi-way valve, and when the multi-way valve is switched to the second state, the carrier gas sequentially enters the extraction unit and the cutting unit through the multi-way valve and is discharged from the multi-way valve; the temperature control unit is used for heating the extraction unit, refrigerating and heating the cutting unit. The invention has the advantages of accurate analysis and the like.
Description
Technical Field
The invention relates to the field of water quality analysis, in particular to an SVOCs (singular value optical storage and data acquisition) analysis device and method in water.
Background
The detection of organic pollutants in surface water and even water source areas in China is very common, and most of the pollutants are derived from artificial pollution mainly comprising industrial three wastes, agricultural pesticides and domestic sewage in agriculture. In 2002, China issued 'surface water environmental quality standards' (GB3838-2002), 109 pollutants are stipulated, wherein the pollutants comprise 69 organic indexes such as volatile organic pollutants, semi-volatile organic pollutants, pesticides, petroleum hydrocarbon and the like; in 2006, the sanitary Standard for Drinking Water (GB-5749-2006) was issued again, and the standard increased the organic index to 48 items. Among the series of organic pollutants, semi-volatile organic compounds (SVOCs) have the characteristics of low concentration, various types, large chemical property difference and the like, so that great challenges are brought to the pretreatment of samples, and the research workers pay attention to the SVocs. In recent years, serious water pollution events caused by deliberate stealing and discharging of industrial wastewater are quite common, and automatic water quality monitoring can play a significant role in pollution early warning.
The automatic pretreatment mode of the SVOCs in water has the following two modes:
1. the liquid desorption method is used together with LC, a switching system, an automatic sampler, a valve, a pump and other devices are needed in the process, and a large amount of organic solvent is needed to be used as an eluting agent and a mobile phase in the analysis process. The mobile phase generally adopts solvents such as water, acetonitrile, methanol and the like, and in the online monitoring process, the solvent addition period is frequent, and the use cost of the mobile phase is high, so that the strategy is not suitable for being applied to the online monitoring process.
2. In combination with GC, Gerstel and marks have related work and commercial solutions in terms of automation, and the automation process is realized by means of thermal desorption, and the automation of the work is not independent of the industrial assistant of "mechanical arm". A series of processes such as extraction, blow-drying, thermal desorption, aging and the like are realized through the grabbing of a mechanical arm, the cost of the mechanical arm is high, meanwhile, the currently commonly used SPME fiber or SPME ARROW is introduced into a sample in a sample introduction mode of piercing a GC sample inlet spacer, the replacement cycle of the spacer and the extraction fiber is frequent, and the method is still mainly used in a laboratory and is still not suitable for on-site on-line monitoring. How to realize a flow path like a liquid desorption mode (only a few electromagnetic valves and a ten-way valve are needed to be switched, so that the cost is relatively low) is also a difficulty in later research.
At present, a series of processes such as extraction, blow-drying, thermal desorption, aging and the like are mainly realized by 'grabbing' of a mechanical arm, such as the SPME ARROW technology of Agilent and the HiSorb stirring rod technology of Marks company. The analysis method is realized by switching the flow path, and the environmental monitoring equipment of the SVOCs in the water of Hunan force adopts the flow path switching mode to realize the extraction and analysis of the SVOCs substances in the water. In addition, the research on the online analysis of the SVOCs in the automatic water realized by the way of switching the flow path is less.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides an underwater SVOCs analysis device.
The purpose of the invention is realized by the following technical scheme:
the underwater SVOCs analysis device comprises a multi-way valve, a chromatographic column and an extraction unit, wherein one end of the extraction unit is respectively communicated with a port of the multi-way valve and a sample inlet pipe, and the other end of the extraction unit is communicated with the port of the multi-way valve; the subaqueous SVOCs analytical equipment still includes:
the sample introduction unit is used for positively feeding a water sample into the extraction unit and enabling the water sample to move in the extraction unit repeatedly in a positive direction and a reverse direction;
the two ends of the cutting unit are respectively communicated with the ports of the multi-way valve, and a hydrophobic material is arranged in the cutting unit; when the multi-way valve is switched to the first state, carrier gas enters the extraction unit through the multi-way valve and is discharged from the multi-way valve, and when the multi-way valve is switched to the second state, the carrier gas sequentially enters the extraction unit and the cutting unit through the multi-way valve and is discharged from the multi-way valve;
and the temperature control unit is used for heating the extraction unit, refrigerating and heating the cutting unit.
The invention also aims to provide an SVOCs analysis method in water, and the invention aims to be realized by the following technical scheme:
an in-water SVOCs analysis method, comprising the steps of:
(A1) the sample introduction unit is used for sending the water sample to the extraction unit in the forward direction and enabling the water sample to move repeatedly in the forward direction and the reverse direction in the extraction unit, and the SVOCs in the water sample are extracted by the extraction unit;
discharging the water sample in the extraction unit;
(A2) disconnecting the extraction unit and the sample introduction unit, switching the multi-way valve to a first state, and allowing purge gas to enter the extraction unit by using the multi-way valve to discharge water vapor in the extraction unit;
(A3) the multi-way valve is switched to a second state, the extraction unit is heated, the cutting unit is refrigerated, carrier gas enters the extraction unit by using the multi-way valve, SVOCs and gaseous water of the extraction unit are discharged and enter the cutting unit, and the SVOCs and the gaseous water are focused in the cutting unit;
(A4) the multi-way valve is switched to a second state, the cutting unit is heated, carrier gas sequentially enters the extraction unit and the cutting unit by using the multi-way valve, water vapor in the cutting unit is carried out, and the SVOCs are focused in the cutting unit;
(A5) the multi-way valve is switched to a third state, the cutting unit is heated, carrier gas enters the cutting unit by using the multi-way valve, carries the SVOCs released in the cutting unit, is discharged and enters a chromatographic column;
(A6) and (4) enabling the components separated by the chromatographic column to enter a detector so as to obtain the content of SVOCs in the water sample.
Compared with the prior art, the invention has the beneficial effects that:
1. the analysis is accurate and the sensitivity is high;
the SVOCs in the water sample are analyzed by combining the technologies of extraction, transfer, focusing, cutting and desorption, so that the SVOCs in the water sample are accurately extracted and separated; (ii) a
The water sample repeatedly moves forwards and directionally in the extraction unit, so that the SVOCs in the water sample are fully extracted, and the analysis accuracy is further improved;
the cutting unit is refrigerated and heated, so that the focusing of the SVOCs and the separation of the SVOCs and water vapor are effectively realized, and the accuracy and the sensitivity of the SVOCs analysis are improved;
2. automation;
the pump, the switching module and the temperature control unit are automatically controlled, so that automatic analysis of SVOCs in a water sample is realized, manual intervention is not needed, and the analysis efficiency is improved.
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 diagram of an underwater SVOCs analysis apparatus according to an embodiment of the present invention;
FIG. 2 is another schematic diagram of an underwater SVOCs analysis apparatus according to an embodiment of the present invention;
FIG. 3 is a flow chart of a method for analyzing SVOCs in water according to an embodiment of the present invention.
Detailed Description
Fig. 1-3 and the following description depict alternative embodiments of the invention to teach those skilled in the art how to make and use the invention. Some conventional aspects have been simplified or omitted for the purpose of explaining the technical solution of 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. 1-2 schematically show a schematic structural diagram of an underwater SVOCs analyzing apparatus according to an embodiment of the present invention, as shown in fig. 1-2, the underwater SVOCs analyzing apparatus includes:
the device comprises a multi-way valve 11, a chromatographic column 21 and a detector 31, wherein the port of the multi-way valve 11 is communicated with the chromatographic column 21 and the detector 31 in sequence;
the extraction unit 41 is used for extracting SVOCs of water samples, one end of the extraction unit 41 is respectively communicated with the port of the multi-way valve 11 and the sample inlet pipe 12, and the other end of the extraction unit 41 is communicated with the port of the multi-way valve 11;
a sample introduction unit, such as a combination of a pump and a valve, for feeding the water sample into the extraction unit 41 in a forward direction and repeatedly moving the water sample in the extraction unit 41 in the forward and reverse directions;
the two ends of the cutting unit 51 are respectively communicated with the ports of the multi-way valve 11, and a hydrophobic material is arranged in the cutting unit 51; when the multi-way valve 11 is switched to the first state, the carrier gas enters the extraction unit 41 (without passing through the cutting unit 51) through the multi-way valve 11 and is discharged from the multi-way valve 11, and when the multi-way valve 11 is switched to the second state, the carrier gas sequentially enters the extraction unit 41 and the cutting unit 51 through the multi-way valve 11 and is discharged from the multi-way valve 11;
a temperature control unit for heating the extraction unit 41, and refrigerating and heating the cutting unit 51.
In order to realize sufficient extraction of SVOCs in the water sample, further, the sample injection unit comprises:
a first switching module 61, the first switching module 16 being used to selectively communicate one end of the extraction unit 41 with a port of the multi-way valve 11 and a second switching module 62;
a second switching module 62, wherein the second switching module 62 is used for enabling the pump 71 to selectively communicate the sampling pipe 12 with the first switching module 61;
a pump 71, said pump 71 being used to pump and push out water samples.
In order to prevent the SOVCs in the water sample from adversely affecting the pump, further, the sample injection unit further comprises:
a reservoir 81, said reservoir 81 being arranged on the line between said pump 71 and the second switching module 62.
FIG. 3 is a flow chart schematically showing an in-water SVOCs analysis method according to an embodiment of the present invention, and as shown in FIG. 3, the in-water SVOCs analysis method includes the steps of:
(A1) the sample introduction unit is used for sending the water sample to the extraction unit 41 in the forward direction, and enabling the water sample to move repeatedly in the forward direction and the reverse direction in the extraction unit 41, wherein the SVOCs in the water sample are extracted by the extraction unit 41, as shown in fig. 1;
discharging the water sample in the extraction unit 41;
(A2) disconnecting the extraction unit 41 and the sample injection unit, switching the multi-way valve 11 to the first state, introducing purge gas into the extraction unit 41 by using the multi-way valve 11, and discharging water vapor in the extraction unit 41 (without entering the cutting unit 51), as shown in fig. 1;
(A3) the multi-way valve 11 is switched to the second state, the extraction unit 41 and the cooling cutting unit 51 are heated, the carrier gas enters the extraction unit 41 by using the multi-way valve 11, the SVOCs and the gaseous water discharged from the extraction unit 41 enter the cutting unit 51, and the SVOCs and the gaseous water are focused in the cutting unit 51, as shown in FIG. 2;
(A4) the multi-way valve 11 is switched to a second state, the cutting unit 51 is heated, the carrier gas enters the extraction unit 41 and the cutting unit 51 in sequence by using the multi-way valve 11, the water vapor in the cutting unit 51 is carried out, and the SVOCs are focused in the cutting unit 51, as shown in FIG. 2;
(A5) the multi-way valve 11 is switched to a third state, the cutting unit 51 is heated, the carrier gas enters the cutting unit 51 by using the multi-way valve 11, carries the SVOCs released from the cutting unit 51, is discharged, and enters the chromatographic column 21, as shown in FIG. 1;
(A6) and the components separated by the chromatographic column 21 enter a detector 31, so that the content of SVOCs in the water sample is obtained.
In order to realize sufficient extraction of SVOCs in the water sample, further, in step (a1), the operation mode of the sample injection unit includes the steps of:
(B1) the second switching module 62 is switched, the sample inlet pipe 12 is communicated with the pump 71 through the second switching module 62, and the pump 71 extracts a water sample;
(B2) the first switching module 61 and the second switching module 62 are switched, the pump 71 pushes the water sample, the water sample sequentially passes through the second switching module 62 and the first switching module 61 and enters the extraction unit 41, and the SVOCs in the water sample are extracted;
(B3) the pump 71 repeatedly pumps out the water sample in the extraction unit 41 and pushes the water sample back into the extraction unit 41, so that the SVOCs in the water sample are extracted;
(B4) the pump 71 pumps out the water sample in the extraction unit 41 and discharges the water sample.
To prevent SOVCs in the sample water from adversely affecting the pump, further, in the sample water pumped by the pump 71, the sample water enters the container 81 between the pump 71 and the second switching module 62.
In order to reduce the structural complexity of the multi-way valve 11, further, in steps (a2) - (a4), gas or liquid is discharged from the same port of the multi-way valve 11.
Example 2:
an application example of the SVOCs analysis apparatus and method according to embodiment 1 of the present invention.
In this application, as shown in fig. 1-2, the pump 71 employs an automatically controlled syringe pump, which also has a waste discharge port; a container 81 is arranged between the pump 71 and the second switching module 62 to buffer water samples; the first switching module 61 and the second switching module 62 respectively adopt an electromagnetic three-way valve, and the multi-way valve 11 adopts a ten-way valve; the extraction unit 41 is internally provided with a PDMS adsorbing material; the cutting unit 51 has a hydrophobic material therein; the temperature control unit comprises a heating module and a temperature control module, the heating module is used for automatically heating the extraction unit 41, and the temperature control module is used for automatically heating and refrigerating the cutting unit 51; the column 21 was an LTM column, and the detector 31 was a mass spectrometer.
As shown in fig. 3, the underwater SVOCs analysis method of the present application example includes the steps of:
(A1) the sample introduction unit is used for sending the water sample to the extraction unit 41 in a forward direction, and enabling the water sample to move repeatedly in the extraction unit 41 in the forward direction and the reverse direction, and the SVOCs in the water sample are extracted by the extraction unit 41, as shown in fig. 1, the specific method is as follows:
(B1) the second switching module 62 is switched automatically, the sampling pipe 12 is communicated with the pump 71 through the second switching module 62, the pump 71 automatically pumps water samples, and the water samples enter the container 81;
(B2) the first switching module 61 and the second switching module 62 are automatically switched, the pump 71 pushes the water sample, the water sample discharged from the container 81 sequentially passes through the second switching module 62 and the first switching module 61 and enters the extraction unit 41, and the SVOCs in the water sample are extracted;
(B3) the pump 71 repeatedly pumps out the water sample in the extraction unit 41 and pushes the water sample back into the extraction unit 41, so that the SVOCs in the water sample are extracted;
(B4) the pump 71 automatically pumps out the water sample in the extraction unit 41 and discharges the water sample through the waste discharge port;
(A2) the connection between the extraction unit 41 and the sample injection unit is automatically disconnected, that is, the first switching module 61 is automatically switched, the multi-way valve 11 is switched to the first state, purge gas (from the port 4 of the multi-way valve) sequentially enters the first switching module 61 and the extraction unit 41 through the multi-way valve 11, and water vapor in the extraction unit 41 is discharged from the port 1 of the multi-way valve 11 (without entering the cutting unit 51), as shown in fig. 1;
(A3) the multi-way valve 11 is switched to a second state, the heating module heats the extraction unit 41, the temperature control module refrigerates the cutting unit 51, carrier gas (from a port 4 of the multi-way valve) sequentially enters the first switching module 61 and the extraction unit 41 by using the multi-way valve 11, SVOCs and gaseous water discharged from the extraction unit 41 enter the cutting unit 51, the SVOCs and the gaseous water are focused in the cutting unit 51, and finally the SVOCs and the gaseous water are discharged from a port 1 of the multi-way valve 11, as shown in FIG. 2;
(A4) the multi-way valve 11 is switched to a second state, the cutting unit 51 is heated to room temperature, carrier gas (from a multi-way valve port 4) enters the first switching module 61, the extraction unit 41 and the cutting unit 51 in sequence by using the multi-way valve 11, water vapor in the cutting unit 51 is carried out, and finally is discharged from a multi-way valve 11 port 1, and SVOCs are still focused in the cutting unit 51, as shown in FIG. 2;
(A5) the multi-way valve 11 is switched to a third state, the cutting unit 51 is heated to room temperature, carrier gas (from the multi-way valve port 7) enters the cutting unit 51 by using the multi-way valve 11, and SVOCs released from the cutting unit 51 are carried out and discharged into the chromatographic column 21, as shown in FIG. 1;
(A6) and the components separated by the chromatographic column 21 enter a detector 31, so that the content of SVOCs in the water sample is obtained.
In the above embodiment, the first switching module and the second switching module both use electromagnetic three-way valves, and the multi-way valve uses a ten-way valve, but may also be other valve banks.
Claims (10)
1. The underwater SVOCs analysis device comprises a multi-way valve, a chromatographic column and an extraction unit, wherein one end of the extraction unit is respectively communicated with a port of the multi-way valve and a sample inlet pipe, and the other end of the extraction unit is communicated with the port of the multi-way valve; characterized in that, aquatic SVOCs analytical equipment still includes:
the sample introduction unit is used for positively feeding a water sample into the extraction unit and enabling the water sample to move in the extraction unit repeatedly in a positive direction and a reverse direction;
the two ends of the cutting unit are respectively communicated with the ports of the multi-way valve, and a hydrophobic material is arranged in the cutting unit; when the multi-way valve is switched to the first state, carrier gas enters the extraction unit through the multi-way valve and is discharged from the multi-way valve, and when the multi-way valve is switched to the second state, the carrier gas sequentially enters the extraction unit and the cutting unit through the multi-way valve and is discharged from the multi-way valve;
and the temperature control unit is used for heating the extraction unit, refrigerating and heating the cutting unit.
2. The underwater SVOCs analyzing apparatus of claim 1, wherein the sample injection unit comprises:
a first switching module for selectively communicating one end of the extraction unit with a port of the multi-way valve and a second switching module;
the second switching module is used for enabling the pump to be selectively communicated with the sampling pipe and the first switching module;
a pump for pumping and pushing out the water sample.
3. The underwater SVOCs analyzing apparatus of claim 2, wherein the sample injection unit further comprises:
a reservoir disposed on the conduit between the pump and the second switching module.
4. The underwater SVOCs analyzing apparatus of claim 2, wherein the multi-way valve is a ten-way valve, and the first switching module and the second switching module are three-way valves, respectively.
5. The underwater SVOCs analysis apparatus of claim 1, wherein the extraction unit has PDMS adsorption material therein.
6. An in-water SVOCs analysis method, comprising the steps of:
(A1) the sample introduction unit is used for sending the water sample to the extraction unit in the forward direction and enabling the water sample to move repeatedly in the forward direction and the reverse direction in the extraction unit, and the SVOCs in the water sample are extracted by the extraction unit;
discharging the water sample in the extraction unit;
(A2) disconnecting the extraction unit and the sample introduction unit, switching the multi-way valve to a first state, and allowing purge gas to enter the extraction unit by using the multi-way valve to discharge water vapor in the extraction unit;
(A3) the multi-way valve is switched to a second state, the extraction unit is heated, the cutting unit is refrigerated, carrier gas enters the extraction unit by using the multi-way valve, SVOCs and gaseous water of the extraction unit are discharged and enter the cutting unit, and the SVOCs and the gaseous water are focused in the cutting unit;
(A4) the multi-way valve is switched to a second state, the cutting unit is heated, carrier gas sequentially enters the extraction unit and the cutting unit by using the multi-way valve, water vapor in the cutting unit is carried out, and the SVOCs are focused in the cutting unit;
(A5) the multi-way valve is switched to a third state, the cutting unit is heated, carrier gas enters the cutting unit by using the multi-way valve, carries the SVOCs released in the cutting unit, is discharged and enters a chromatographic column;
(A6) and (4) enabling the components separated by the chromatographic column to enter a detector so as to obtain the content of SVOCs in the water sample.
7. The underwater SVOCs analysis method of claim 6, wherein in step (A1), the sample injection unit operates in a manner comprising the steps of:
(B1) the second switching module switches, the sample injection pipe is communicated with the pump through the second switching module, and a water sample is pumped and extracted by the pump;
(B2) the first switching module and the second switching module are switched, the pump pushes a water sample, the water sample sequentially passes through the second switching module and the first switching module and enters the extraction unit, and the SVOCs in the water sample are extracted;
(B3) the pump repeatedly pumps out the water sample in the extraction unit and pushes the water sample back into the extraction unit, and SVOCs in the water sample are extracted;
(B4) and pumping out the water sample in the extraction unit by the pump and discharging the water sample.
8. The in-water SVOCs analysis method of claim 6 or 7, wherein in said pumping of the sample of water, the sample of water enters a container between the pump and the second switching module.
9. The aquatic SVOCs analysis method as claimed in claim 6, wherein in steps (a2) - (a4), gas or liquid is discharged from the same port of said multi-way valve.
10. The aquatic SVOCs analysis method as claimed in claim 7, wherein in the step (a2), the moisture discharged from the extraction unit does not enter the cutting unit.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103675154A (en) * | 2013-12-30 | 2014-03-26 | 力合科技（湖南）股份有限公司 | Online pretreatment method and online pretreatment device of SVOCs (Semi Volatile Organic Compounds) in water |
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