CN112964509A - Natural water sample in-situ suction filtration and solid phase extraction integrated operation system and operation method thereof - Google Patents
Natural water sample in-situ suction filtration and solid phase extraction integrated operation system and operation method thereof Download PDFInfo
- Publication number
- CN112964509A CN112964509A CN202110286749.7A CN202110286749A CN112964509A CN 112964509 A CN112964509 A CN 112964509A CN 202110286749 A CN202110286749 A CN 202110286749A CN 112964509 A CN112964509 A CN 112964509A
- Authority
- CN
- China
- Prior art keywords
- liquid
- cylinder
- solid
- phase extraction
- water sample
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- 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
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
- G01N1/14—Suction devices, e.g. pumps; Ejector devices
-
- 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
-
- 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
- G01N1/34—Purifying; Cleaning
-
- 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
-
- 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
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
- G01N1/14—Suction devices, e.g. pumps; Ejector devices
- G01N2001/1418—Depression, aspiration
- G01N2001/1427—Positive displacement, piston, peristaltic
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Hydrology & Water Resources (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention relates to an integrated operation system and an operation method for in-situ suction filtration and solid-phase extraction of a natural water sample, wherein the integrated operation system comprises a Buchner funnel, a suction filter cylinder, an activation liquid bottle, a washing liquid bottle, a first vacuum-pumping cylinder, a second vacuum-pumping cylinder, a solid-liquid extraction column, a rack, a four-way joint, a three-way joint and the like, wherein the four-way joint and the three-way joint are arranged in the rack. The integrated operation system is small, exquisite, flexible and convenient in structure and convenient to carry, so that the integrated operation system can be brought to a natural water taking point to perform water sample collection, water sample suction filtration and solid phase extraction operation on site, the functions of field suction filtration and solid phase extraction on natural water samples such as rivers, lakes or underground water and the like are realized, the timeliness of sample treatment is ensured, and the data reliability and accuracy of water sample monitoring are improved. The operation method of the invention utilizes a set of system for water sample suction filtration and solid phase extraction, and can be completed at one time, the operation steps are simple, the working efficiency is improved, and no pollution harm is generated to the environment.
Description
Technical Field
The invention relates to a water sample in-situ suction filtration system, in particular to a natural water sample in-situ suction filtration and solid phase extraction integrated operation system and an operation method thereof.
Background
Surface water such as rivers and lakes, and ground water contain various organic and inorganic components in nature, and these components contain even complicated pollutants. In the present day, whether the analysis of the macro-substances in the water sample or the analysis of the key pollutants, the water sample is usually collected into the laboratory and then the pretreatment work is performed. The pretreatment includes a suction filtration step. The suction filtration is to remove impurity components contained in a water sample and to realize solid-liquid separation. Substances (such as antibiotics, hormones and the like) which are small in content and difficult to extract in a water sample can be extracted by carrying out solid-phase extraction. The solid phase extraction is mainly used for separating, purifying and concentrating a sample, namely, a solid adsorbent is adopted to adsorb target compounds (such as antibiotics, hormones and the like) in a liquid sample, so that the target compounds are separated from matrix and interfering substances of the liquid sample, and then an eluent (such as methanol and the like) is used for elution so as to achieve the purpose of separating and enriching the target compounds.
At present, both the suction filtration operation and the solid phase extraction operation are carried out in a laboratory, so that a sample needs to be taken away from the natural environment and returned to the laboratory for operation, and the method belongs to an ex-situ treatment mode. The process of bringing the water sample back to the laboratory can affect the in-situ characteristic state of the water sample, and the deterioration or variation of components in the sample can be caused due to the fact that the sample cannot be processed in time, so that the accuracy of data in experimental analysis is reduced.
Disclosure of Invention
The invention aims to provide an in-situ suction filtration and solid-phase extraction integrated operation system for a natural water sample and an operation method thereof, so as to solve the problem of reduced analysis data accuracy caused by poor timeliness of water sample transmission and difficulty in maintaining an in-situ characteristic state of the water sample.
The invention is realized by the following steps: an integrated operating system of in-situ suction filtration and solid-phase extraction of a natural water sample comprises:
the Buchner funnel is arranged at the upper end of the system;
the pumping filter cylinder is arranged on the bracket, the upper port of the pumping filter cylinder is connected with the outlet of the Buchner funnel, the lower port of the pumping filter cylinder is connected with a liquid outlet pipe, the liquid outlet pipe is connected with a first valve, and the pumping filter cylinder is connected with a first interface which is used for being in butt joint with a manual vacuum pump;
the four-way joint is arranged in the bracket, a first port of the four-way joint is connected with the liquid outlet pipe, a second port of the four-way joint is used for matching with an upper port of the solid-liquid extraction column, a third port of the four-way joint is connected with the first inserting pipe, and a fourth port of the four-way joint is connected with the second inserting pipe;
the tee joint is arranged in the bracket and is positioned below the tee joint, and a first port of the tee joint is used for matching with a lower port of the solid-liquid extraction column;
the free end of the first intubation is inserted into the activating liquid bottle, and a second valve is connected to the first intubation;
the free end of the second intubation is inserted into the shower lotion bottle, and the second intubation is connected with a sixth valve;
the first vacuum pumping cylinder is provided with a second port for butting with the manual vacuum pump, the cylinder wall of the first vacuum pumping cylinder is provided with a liquid inlet and a liquid outlet, a pipeline connected to the liquid inlet is connected with the second port of the tee joint, and the liquid outlet is connected with a fourth valve; and
and the second vacuum-pumping cylinder is provided with a wide-mouth sealing cover, a liquid-pumping pipeline penetrates through the sealing cover, the external end of the liquid-pumping pipeline is connected with a third port of the tee joint, and a third port for butting with a manual vacuum pump is arranged on the second vacuum-pumping cylinder.
The invention also includes:
the solid-liquid extraction column is arranged between the four-way joint and the three-way joint in the bracket and is used for extracting solid-phase substances in a water sample; and
and the liquid collecting bottle is placed in the second vacuumizing cylinder, and the free end of the liquid pumping pipeline is inserted into the liquid collecting bottle and is used for collecting eluent which flows through the solid-liquid extraction column to elute the solid-phase extraction substances.
The invention also includes:
and the manual vacuum pump is matched and connected with each interface in the system according to the process requirements and is used for finishing various operations including suction filtration, activation, leaching, solid-phase extraction and elution.
The first interface is arranged on the upper part of the side wall of the filter cartridge to prevent filtrate from flowing out of the filter cartridge and being incapable of filtering filtrate with enough volume; and a volume scale line is marked on the side wall of the pumping filter cylinder so as to control the collection amount of the filtrate during the pumping filtration operation.
The invention can also be realized as follows: an integrated operation method of in-situ suction filtration and solid-phase extraction of a natural water sample comprises the following steps:
a. preparing the natural water sample in-situ suction filtration and solid phase extraction integrated operation system, bringing the system to a natural water taking point to be detected, and collecting a natural water sample on site;
b. system rinsing: firstly, a solid-phase extraction column is not installed, a first valve on a liquid outlet pipe is closed, a part of a collected water sample is taken out and injected into a Buchner funnel, the water sample passes through the Buchner funnel and a suction filter cylinder to rinse the Buchner funnel and the suction filter cylinder, and after rinsing is finished, the first valve is opened to discharge rinsing liquid;
c. water sample suction filtration: closing a first valve on the liquid outlet pipe, putting filter paper into the buchner funnel, installing a manual vacuum pump on a first connector on the suction filter cylinder, carrying out vacuum pumping operation on the suction filter cylinder, and simultaneously injecting the collected water sample into the buchner funnel so that the water sample enters the suction filter cylinder in a suction filtration state to complete water sample suction filtration operation;
d. activation of the solid phase extraction column: installing the solid phase extraction column between a four-way joint and a three-way joint in a bracket to form an air tightness channel, opening a communication channel between an activation liquid bottle and the four-way joint and a communication channel between a first vacuumizing cylinder and the three-way joint, and closing other channels, installing a manual vacuum pump on a second interface on the first vacuumizing cylinder, and vacuumizing the first vacuumizing cylinder to enable the activation liquid in the activation liquid bottle to flow through the solid phase extraction column to perform activation operation; after the activation of the solid phase extraction column is completed, discharging waste liquid entering the first vacuum-pumping cylinder;
e. leaching the solid phase extraction column: opening a communication passage between the stranguria liquid bottle and the four passages, maintaining the communication passage between the first vacuumizing cylinder and the three passages to be in an open state, closing other passages, keeping a manual vacuum pump on a second interface, vacuumizing the first vacuumizing cylinder, and enabling the leacheate in the stranguria liquid bottle to flow through the solid-phase extraction column to perform leaching operation; after the leaching of the solid-phase extraction column is finished, discharging waste liquid entering the first vacuum-pumping cylinder;
f. extracting a water sample: opening a first valve on a liquid outlet pipe of the suction filtration cylinder, maintaining a communication passage between the first vacuum-pumping cylinder and the tee joint to be in an open state, closing other passages, maintaining a manual vacuum pump on a second interface, and performing vacuum-pumping operation on the first vacuum-pumping cylinder to enable a water sample subjected to suction filtration in the suction filtration cylinder to flow through a solid-phase extraction column to perform solid-phase extraction operation on the water sample; after the solid phase extraction operation is finished, discharging waste liquid entering the first vacuum-pumping cylinder;
g. elution of solid phase extract material: the liquid collecting bottle is placed into a second vacuumizing cylinder, the free end of a liquid pumping pipeline is inserted into the liquid collecting bottle, a sealing cover of the liquid collecting bottle is covered, a communication channel of an activation liquid bottle and a four-way connector and a communication channel of the second vacuumizing cylinder and a three-way connector are opened, other channels are closed, a manual vacuum pump is installed on a third interface on the second vacuumizing cylinder, vacuumizing operation is carried out on the second vacuumizing cylinder, the activation liquid in the activation liquid bottle flows through a solid-phase extraction column, elution operation is carried out on solid-phase extraction substances attached to the solid-phase extraction column, and eluent enters the liquid collecting bottle.
And c, maintaining the suction filtration operation of the step c until the liquid level of the filtrate in the suction filtration cylinder reaches the position of the preset volume scale mark on the suction filtration cylinder.
When the waste liquid entering the first vacuumizing cylinder pollutes and harms the environment, the waste liquid bottle is used for collecting the discharged waste liquid and bringing the waste liquid back to a laboratory for harmless treatment.
In the step f, according to the indication number of a negative pressure meter attached to the manual vacuum pump, the force and the frequency of the vacuumizing operation are adjusted, so that the liquid flow rate in the water sample extraction process accords with the maximum extraction efficiency of the solid-phase extraction column.
And (g) after the elution operation in the step g is finished, taking the liquid collecting bottle out of the second vacuumizing cylinder, covering the liquid collecting bottle, sticking a label, and taking the liquid collecting bottle back to a laboratory for physical and chemical analysis.
The integrated operation system is small, exquisite and flexible in structure and convenient to carry, so that the integrated operation system can be brought to a natural water taking point to carry out water sample collection, water sample suction filtration and solid phase extraction operation on site, the function of real-time detection on natural water samples such as rivers, lakes or underground water is realized, the timeliness of sample treatment is ensured, the phenomena of organic matter volatilization and the like possibly caused by long-distance carrying of the water samples are avoided, and the data reliability and accuracy of water sample monitoring are improved. The operation method of the invention utilizes a set of system for water sample suction filtration and solid phase extraction, and can be completed at one time, the operation steps are simple, the working efficiency is improved, and no pollution harm is generated to the environment.
Drawings
FIG. 1 is a schematic diagram of an integrated operating system according to the present invention.
Fig. 2 is a schematic view of the structure of the manual vacuum pump.
In the figure: 1. buchner funnel, 2, first interface, 3, take out and strain the section of thick bamboo, 4, first valve, 5, cross, 6, second valve, 7, activation liquid bottle, 8, first intubate, 9, third interface, 10, the second section of thick bamboo of taking out a vacuum, 11, the collecting flask, 12, third valve, 13, tee bend, 14, solid-phase extraction post, 15, fourth valve, 16, fifth valve, 17, the first section of thick bamboo of taking out a vacuum, 18, drench liquid bottle, 19, the second intubate, 20, the second interface, 21, the sixth valve, 22, support, 23, manual vacuum pump, 24, negative pressure table, 25, liquid suction pipeline.
Detailed Description
As shown in figure 1, the natural water sample in-situ suction filtration and solid phase extraction integrated operation system comprises a Buchner funnel 1, a suction filtration cylinder 3, an activation liquid bottle 7, a leacheate bottle 18, a first vacuum-pumping cylinder 17, a second vacuum-pumping cylinder 10, a solid-liquid extraction column 14, a liquid collection bottle 11, a manual vacuum pump 23 (figure 2), a rack 22, a four-way joint 5, a three-way joint 13 and the like, wherein the four-way joint 5 and the three-way joint 13 are arranged in the rack 22.
The buchner funnel 1 is arranged at the upper end of the system; the suction filter cylinder 3 is arranged at the upper part of the bracket 22, the upper port of the suction filter cylinder is connected with the outlet of the Buchner funnel 1, the lower port of the suction filter cylinder is connected with a liquid outlet pipe, the liquid outlet pipe is connected with a first valve 4, and the suction filter cylinder 3 is connected with a first interface 2 for being in butt joint with a manual vacuum pump; the first connector 2 is arranged at the position, close to the top surface, of the upper part of the side wall of the suction filter cylinder, and a volume scale line is marked on the side wall of the suction filter cylinder 3.
The frame 22 is a cylindrical structure, the bottom surface of the top of the frame is provided with a connecting port connected with a liquid outlet pipe of the suction filtration cylinder, the first port of the cross joint 5 is connected with the connecting port to form a connecting passage with the liquid outlet pipe of the suction filtration cylinder, the second port of the cross joint 5 is vacant and used for being connected with the upper port of the solid-liquid extraction column 14, the third port of the cross joint 5 is connected with the first insertion pipe 8, and the fourth port of the cross joint 5 is connected with the second insertion pipe 19. The tee joint 13 is arranged in the bracket 22 and is positioned below the cross joint 5, and a first port of the tee joint is vacant and is used for being matched with a lower port of the solid-liquid extraction column 14.
The activating liquid bottle 7 is filled with activating liquid (such as methanol), the free end of the first cannula 8 is inserted into the activating liquid bottle to form a suction pipe, and a communication passage between the four-way joint 5 and the activating liquid bottle 7 is formed. A second valve 6 is connected to the first cannula 8. The leacheate bottle 18 is filled with leacheate (such as ultrapure water), and the free end of the second cannula 19 is inserted into the leacheate bottle to form a suction pipe, and a communication passage between the four-way joint 5 and the leacheate bottle 18 is formed. A sixth valve 21 is connected to the second cannula 19.
A second interface 20 for butting with a manual vacuum pump is arranged on the first vacuum-pumping cylinder 17, a liquid inlet and a liquid outlet are arranged on the cylinder wall of the first vacuum-pumping cylinder, and a pipeline connected with the liquid inlet is connected with a second interface of the tee joint 13 to form a communication passage between the tee joint 13 and the first vacuum-pumping cylinder 17; a fourth valve 15 is connected to the liquid outlet. The second vacuum-pumping cylinder 10 is in a wide-mouth bottle structure and is provided with a wide-mouth sealing cover, a liquid pumping pipeline 25 is connected to the sealing cover in a penetrating manner, and the external connection end of the liquid pumping pipeline 25 is connected with the third port of the tee joint 13 to form a communication passage between the tee joint 13 and the second vacuum-pumping cylinder 10. A third port 9 for interfacing with a manual vacuum pump is provided on the second vacuum cylinder 10.
The solid-liquid extraction column 14 can be installed between the second port of the four-way joint 5 and the first port of the three-way joint 13 in the bracket 22, and a sealing ring is arranged at the joint to form an airtight connection. The liquid collecting bottle 11 may be placed in the second vacuum-pumping cylinder 10, and after the liquid collecting bottle is placed, the free end of the liquid pumping pipeline 25 should be inserted therein to collect the eluent flowing through the solid-liquid extraction column.
As shown in fig. 2, the manual vacuum pump 23 is a conventional apparatus, and is connected with a negative pressure gauge 22 for displaying the negative pressure value in the vacuum container in real time. The manual vacuum pump 23 can be connected with each interface in the system according to the process requirements to complete various operations such as suction filtration, activation, leaching, solid phase extraction, elution and the like.
The operation method of the natural water sample in-situ suction filtration and solid phase extraction integrated system comprises the following steps:
firstly, preparing a set of natural water sample in-situ suction filtration and solid phase extraction integrated operation system, bringing the system to a natural water taking point to be detected, and collecting a natural water sample on site.
II, a rinsing system: and (3) closing the first valve 4, taking out a part of the collected water sample under the condition that no filter paper is placed in the solid-phase extraction column 14 and the Buchner funnel 1, injecting the part into the Buchner funnel 1, and rinsing the Buchner funnel 1 and the suction filtration cylinder 3 by the water sample through the Buchner funnel 1 and the suction filtration cylinder 2. After rinsing is completed, the first valve 4 is opened to discharge the rinse solution.
Thirdly, water sample suction filtration: closing a first valve 4 on the liquid outlet pipe, putting and paving filter paper with the diameter consistent with the inner diameter of the bottom of an inner cavity of a Buchner funnel 1 in the Buchner funnel 1, tightly butting a pipe orifice of a manual vacuum pump 23 with a first interface 2 on a suction filtration cylinder 3, vacuumizing the suction filtration cylinder 3 by the manual vacuum pump 23, and simultaneously injecting the collected water sample into the Buchner funnel 1 to ensure that the water sample in the Buchner funnel 1 enters the suction filtration cylinder 3 in a suction filtration state; when the liquid level of the filtrate reaches the preset volume scale position on the suction filter cylinder 3, no water sample is injected, so that the water sample suction filtration operation is completed.
Fourthly, activating the solid phase extraction column: the solid phase extraction column 14 is arranged between the four-way joint 5 and the three-way joint 13 in the bracket 22, and the joints of the two are provided with sealing rings to ensure the air tightness of the connection. Opening the second valve 6 and the fifth valve 16 to open a communication passage between the activation liquid bottle 7 and the four-way valve 5 and a communication passage between the first vacuum-pumping cylinder 17 and the three-way valve 13; the first valve 4, the fourth valve 15, the sixth valve 21, and the third valve 12 are closed to shut off the other passages. The activating solution bottle 7 is filled with the activating solution which is preferably the same liquid as the liquid in the solid phase extraction column 14. The nozzle of the manual vacuum pump 23 is closely abutted with the second interface 20 on the first vacuum cylinder 17, and the manual vacuum pump 23 is used for performing vacuum pumping operation on the first vacuum cylinder 17. At this time, the activation solution in the activation solution bottle 7 enters the solid phase extraction column 14 through the first cannula 8 and the four-way valve 5 for activation operation, and then enters the first vacuum cylinder 17 through the three-way valve 13. After the activation operation of the solid phase extraction column is finished, the fourth valve 15 is opened, the waste liquid entering the vacuum cylinder 17 is discharged into a waste liquid bottle and is carried back to a laboratory for harmless treatment.
And fifthly, leaching the solid phase extraction column: opening a sixth valve 21 to open a communication passage between the leacheate bottle 18 and the four-way valve 5; meanwhile, the communication path between the first vacuum cylinder 17 and the tee 13 is maintained in an open state. The first valve 4, the fourth valve 15, the second valve 6, and the third valve 12 are closed to shut off the other passages. The rinse solution bottle 18 contains a rinse solution (e.g., ultrapure water). The manual vacuum pump 23 is still connected to the second port 20 of the first vacuum cylinder 17, and the first vacuum cylinder 17 is vacuumized by the manual vacuum pump 23. At this time, the eluent in the eluent bottle 18 enters the solid-phase extraction column 14 through the second cannula 19 and the four-way valve 5, performs an elution operation, and then enters the first vacuuming cylinder 17 through the three-way valve 13. After the washing operation of the solid phase extraction column is completed, the fifth valve 16 and the sixth valve 21 are closed, and the manual vacuum pump 23 is removed. If the leacheate has no pollution to the environment, the fourth valve 15 on the liquid outlet of the first vacuum-pumping cylinder 17 can be opened to directly discharge waste liquid; if the mixed solution of ultrapure water and other compounds is used as the leacheate, the leacheate needs to be discharged into a waste liquid bottle and taken back to a laboratory for harmless treatment due to certain pollution damage to the environment.
Sixthly, extracting a water sample: opening a first valve 4 on a liquid outlet pipe of the suction filtration cylinder, and maintaining a communication passage between a first vacuum-pumping cylinder 17 and a tee joint 13 in an open state; the second valve 6, the third valve 12, the fourth valve 15, and the sixth valve 21 are closed to close the other passages. The manual vacuum pump 23 is held by the second port 20, and performs a vacuum pumping operation on the first vacuum cylinder 17. At this time, the water sample pumped in the pumping filtration cylinder 3 enters the solid phase extraction column 14 through the four-way valve 5, and then flows into the first vacuum pumping cylinder 17 to perform the solid phase extraction operation of the water sample. In the process, an operator can observe the indication value on the negative pressure meter 24 on the manual vacuum pump 23 and adjust the force and frequency of the vacuumizing operation so as to ensure that the flow rate of the liquid in the water sample extraction process conforms to the maximum extraction efficiency of the solid-phase extraction column. After the solid-phase extraction of the water sample is completed, the fourth valve 15 on the liquid outlet of the first vacuum-pumping cylinder can be opened to directly discharge the waste liquid in view of the fact that the extracted waste liquid has no pollution hazard to the environment.
Seventhly, eluting the solid-phase extraction substance: the liquid collecting bottle 11 is put into the second vacuum cylinder 10, and the free end of the liquid extracting pipe 25 is inserted into the liquid collecting bottle 11, and the sealing cover on the liquid collecting bottle 11 is covered. Then, opening the second valve 6 and the third valve 12, and opening a communication passage of the activation liquid bottle and the four-way valve and a communication passage of the second vacuum-pumping cylinder and the three-way valve; the first valve 4, the fourth valve 15, the fifth valve 16, and the sixth valve 21 are closed to shut off the other passages. The nozzle of the manual vacuum pump 23 is closely abutted with the third interface 9 on the second vacuum cylinder 10, and the second vacuum cylinder 10 is vacuumized by the manual vacuum pump 23. At this time, the activating solution in the activating solution bottle 7 enters the solid phase extraction column 14 through the first cannula 8 and the four-way joint 5, and the solid phase extraction substance attached to the solid phase extraction column is eluted; under the continuous vacuum pumping operation, the eluent passes through the tee joint 13 and the liquid pumping line 25 to enter the liquid collecting bottle 11 provided in the second vacuum cylinder 10. After the elution operation is finished, the liquid collecting bottle 11 is taken out of the second vacuum-pumping cylinder 10, the sealing cover of the liquid collecting bottle is covered, the label is pasted, and the liquid collecting bottle is taken back to a laboratory for physical and chemical analysis.
Claims (9)
1. The utility model provides an integrated operating system of natural world water sample normal position suction filtration and solid-phase extraction which characterized by includes:
the Buchner funnel is arranged at the upper end of the system;
the pumping filter cylinder is arranged on the bracket, the upper port of the pumping filter cylinder is connected with the outlet of the Buchner funnel, the lower port of the pumping filter cylinder is connected with a liquid outlet pipe, the liquid outlet pipe is connected with a first valve, and the pumping filter cylinder is connected with a first interface which is used for being in butt joint with a manual vacuum pump;
the four-way joint is arranged in the bracket, a first port of the four-way joint is connected with the liquid outlet pipe, a second port of the four-way joint is used for matching with an upper port of the solid-liquid extraction column, a third port of the four-way joint is connected with the first inserting pipe, and a fourth port of the four-way joint is connected with the second inserting pipe;
the tee joint is arranged in the bracket and is positioned below the tee joint, and a first port of the tee joint is used for matching with a lower port of the solid-liquid extraction column;
the free end of the first intubation is inserted into the activating liquid bottle, and a second valve is connected to the first intubation;
the free end of the second intubation is inserted into the shower lotion bottle, and the second intubation is connected with a sixth valve;
the first vacuum pumping cylinder is provided with a second port for butting with the manual vacuum pump, the cylinder wall of the first vacuum pumping cylinder is provided with a liquid inlet and a liquid outlet, a pipeline connected to the liquid inlet is connected with the second port of the tee joint, and the liquid outlet is connected with a fourth valve; and
and the second vacuum-pumping cylinder is provided with a wide-mouth sealing cover, a liquid-pumping pipeline penetrates through the sealing cover, the external end of the liquid-pumping pipeline is connected with a third port of the tee joint, and a third port for butting with a manual vacuum pump is arranged on the second vacuum-pumping cylinder.
2. The integrated operating system for in-situ suction filtration and solid-phase extraction of a natural water sample according to claim 1, further comprising:
the solid-liquid extraction column is arranged between the four-way joint and the three-way joint in the bracket and is used for extracting solid-phase substances in a water sample; and
and the liquid collecting bottle is placed in the second vacuumizing cylinder, and the free end of the liquid pumping pipeline is inserted into the liquid collecting bottle and is used for collecting eluent which flows through the solid-liquid extraction column to elute the solid-phase extraction substances.
3. The natural water sample in-situ suction filtration and solid phase extraction integrated operation system according to claim 2, further comprising:
and the manual vacuum pump is matched and connected with each interface in the system according to the process requirements and is used for finishing various operations including suction filtration, activation, leaching, solid-phase extraction and elution.
4. The integrated operating system for in-situ suction filtration and solid-phase extraction of a natural water sample according to claim 3, wherein the first interface is arranged at the upper part of the side wall of the suction filtration cylinder, and a volume scale line is marked on the side wall of the suction filtration cylinder.
5. An integrated operation method of in-situ suction filtration and solid-phase extraction of a natural water sample is characterized by comprising the following steps:
a. preparing the natural water sample in-situ suction filtration and solid phase extraction integrated operation system as claimed in any one of claims 1 to 4, bringing the system to a natural water taking point to be detected, and collecting a natural water sample on site;
b. system rinsing: firstly, a solid-phase extraction column is not installed, a first valve on a liquid outlet pipe is closed, a part of a collected water sample is taken out and injected into a Buchner funnel, the water sample passes through the Buchner funnel and a suction filter cylinder to rinse the Buchner funnel and the suction filter cylinder, and after rinsing is finished, the first valve is opened to discharge rinsing liquid;
c. water sample suction filtration: closing a first valve on the liquid outlet pipe, putting filter paper into the buchner funnel, installing a manual vacuum pump on a first connector on the suction filter cylinder, carrying out vacuum pumping operation on the suction filter cylinder, and simultaneously injecting the collected water sample into the buchner funnel so that the water sample enters the suction filter cylinder in a suction filtration state;
d. activation of the solid phase extraction column: installing the solid phase extraction column between a four-way joint and a three-way joint in a bracket to form an air tightness channel, opening a communication channel between an activation liquid bottle and the four-way joint and a communication channel between a first vacuumizing cylinder and the three-way joint, and closing other channels, installing a manual vacuum pump on a second interface on the first vacuumizing cylinder, and vacuumizing the first vacuumizing cylinder to enable the activation liquid in the activation liquid bottle to flow through the solid phase extraction column to perform activation operation; after the activation of the solid phase extraction column is completed, discharging waste liquid entering the first vacuum-pumping cylinder;
e. leaching the solid phase extraction column: opening a communication passage between the stranguria liquid bottle and the four passages, maintaining the communication passage between the first vacuumizing cylinder and the three passages to be in an open state, closing other passages, keeping a manual vacuum pump on a second interface, vacuumizing the first vacuumizing cylinder, and enabling the leacheate in the stranguria liquid bottle to flow through the solid-phase extraction column to perform leaching operation; after the leaching of the solid-phase extraction column is finished, discharging waste liquid entering the first vacuum-pumping cylinder;
f. extracting a water sample: opening a first valve on a liquid outlet pipe of the suction filtration cylinder, maintaining a communication passage between the first vacuum-pumping cylinder and the tee joint to be in an open state, closing other passages, maintaining a manual vacuum pump on a second interface, and performing vacuum-pumping operation on the first vacuum-pumping cylinder to enable a water sample subjected to suction filtration in the suction filtration cylinder to flow through a solid-phase extraction column to perform solid-phase extraction operation on the water sample; after the solid phase extraction operation is finished, discharging waste liquid entering the first vacuum-pumping cylinder;
g. elution of solid phase extract material: the liquid collecting bottle is placed into a second vacuumizing cylinder, the free end of a liquid pumping pipeline is inserted into the liquid collecting bottle, a sealing cover of the liquid collecting bottle is covered, a communication channel of an activation liquid bottle and a four-way connector and a communication channel of the second vacuumizing cylinder and a three-way connector are opened, other channels are closed, a manual vacuum pump is installed on a third interface on the second vacuumizing cylinder, vacuumizing operation is carried out on the second vacuumizing cylinder, the activation liquid in the activation liquid bottle flows through a solid-phase extraction column, elution operation is carried out on solid-phase extraction substances attached to the solid-phase extraction column, and eluent enters the liquid collecting bottle.
6. The method of claim 5, wherein the suction filtration operation of step c is maintained until the filtrate level in the suction filtration cartridge reaches the predetermined volumetric graduation marks on the suction filtration cartridge.
7. The method as claimed in claim 5, wherein when the waste liquid introduced into the first vacuum-pumping cylinder is harmful to environment, the waste liquid bottle is used to collect the discharged waste liquid and carry it back to the laboratory for harmless treatment.
8. The operating method as claimed in claim 5, wherein in step f, the force and frequency of the vacuum pumping operation are adjusted according to the indication of the negative pressure gauge attached to the manual vacuum pump, so that the liquid flow rate in the water sample extraction process meets the maximum extraction efficiency of the solid phase extraction column.
9. The method as claimed in claim 5, wherein the elution step g is completed by removing the vial from the second vacuum drum, covering the second vacuum drum, labeling the vial, and returning the vial to the laboratory for physical and chemical analysis.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110286749.7A CN112964509B (en) | 2021-03-17 | 2021-03-17 | Natural water sample in-situ suction filtration and solid phase extraction integrated operation system and operation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110286749.7A CN112964509B (en) | 2021-03-17 | 2021-03-17 | Natural water sample in-situ suction filtration and solid phase extraction integrated operation system and operation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112964509A true CN112964509A (en) | 2021-06-15 |
| CN112964509B CN112964509B (en) | 2023-03-03 |
Family
ID=76279039
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110286749.7A Active CN112964509B (en) | 2021-03-17 | 2021-03-17 | Natural water sample in-situ suction filtration and solid phase extraction integrated operation system and operation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112964509B (en) |
Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5345809A (en) * | 1989-06-09 | 1994-09-13 | Research Corporation Technologies, Inc. | Explosive detection screening system |
| JP2004175801A (en) * | 2002-11-28 | 2004-06-24 | Polimeri Europa Spa | Integrated method for producing phenol from benzene while using by-product in circulating way |
| CN102109505A (en) * | 2009-12-23 | 2011-06-29 | 中国科学院生态环境研究中心 | Pretreatment method for purifying extract liquor |
| CN202777921U (en) * | 2012-09-21 | 2013-03-13 | 北京莱伯泰科仪器有限公司 | Multifunctional solid-phase extraction device and multifunctional solid-phase extraction system |
| CN103787466A (en) * | 2014-01-24 | 2014-05-14 | 中南大学 | Pulse enrichment device and method for quick treatment of high-concentration heavy metal wastewater |
| CN204065037U (en) * | 2014-02-28 | 2014-12-31 | 中国农业科学院农产品加工研究所 | A kind of full-automatic matrix dispersive solid-phase extraction pre-treatment all-in-one |
| CN105251238A (en) * | 2015-11-13 | 2016-01-20 | 黑龙江省科学院科技孵化中心 | Solid phase extraction column capable of achieving negative pressure suction and using method |
| CN205670140U (en) * | 2016-04-20 | 2016-11-02 | 济南出入境检验检疫局检验检疫技术中心 | A kind of device that multiple samples can be carried out continuous pigment detection |
| CN106932516A (en) * | 2017-04-18 | 2017-07-07 | 蔡明红 | Original position ultrasound washing device and ultrasonic elution process based on SPE sampling column |
| CN107469425A (en) * | 2017-08-08 | 2017-12-15 | 中国地质科学院岩溶地质研究所 | A kind of Portable water sample step filters system |
| CN109932211A (en) * | 2019-04-11 | 2019-06-25 | 中国科学院海洋研究所 | Deep-sea multichannel original position fluid sampling filter and method based on ROV |
| CN110108517A (en) * | 2019-05-30 | 2019-08-09 | 中国地质科学院水文地质环境地质研究所 | A kind of in-situ acquisition filter device and its application method based on phreatic water |
| CN110501203A (en) * | 2019-08-05 | 2019-11-26 | 未名环境分子诊断(广东)有限公司 | The Preconcentration in-situ purification device and method of psychoactive drug substance in a kind of water environment |
-
2021
- 2021-03-17 CN CN202110286749.7A patent/CN112964509B/en active Active
Patent Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5345809A (en) * | 1989-06-09 | 1994-09-13 | Research Corporation Technologies, Inc. | Explosive detection screening system |
| JP2004175801A (en) * | 2002-11-28 | 2004-06-24 | Polimeri Europa Spa | Integrated method for producing phenol from benzene while using by-product in circulating way |
| CN102109505A (en) * | 2009-12-23 | 2011-06-29 | 中国科学院生态环境研究中心 | Pretreatment method for purifying extract liquor |
| CN202777921U (en) * | 2012-09-21 | 2013-03-13 | 北京莱伯泰科仪器有限公司 | Multifunctional solid-phase extraction device and multifunctional solid-phase extraction system |
| CN103787466A (en) * | 2014-01-24 | 2014-05-14 | 中南大学 | Pulse enrichment device and method for quick treatment of high-concentration heavy metal wastewater |
| CN204065037U (en) * | 2014-02-28 | 2014-12-31 | 中国农业科学院农产品加工研究所 | A kind of full-automatic matrix dispersive solid-phase extraction pre-treatment all-in-one |
| CN105251238A (en) * | 2015-11-13 | 2016-01-20 | 黑龙江省科学院科技孵化中心 | Solid phase extraction column capable of achieving negative pressure suction and using method |
| CN205670140U (en) * | 2016-04-20 | 2016-11-02 | 济南出入境检验检疫局检验检疫技术中心 | A kind of device that multiple samples can be carried out continuous pigment detection |
| CN106932516A (en) * | 2017-04-18 | 2017-07-07 | 蔡明红 | Original position ultrasound washing device and ultrasonic elution process based on SPE sampling column |
| CN107469425A (en) * | 2017-08-08 | 2017-12-15 | 中国地质科学院岩溶地质研究所 | A kind of Portable water sample step filters system |
| CN109932211A (en) * | 2019-04-11 | 2019-06-25 | 中国科学院海洋研究所 | Deep-sea multichannel original position fluid sampling filter and method based on ROV |
| CN110108517A (en) * | 2019-05-30 | 2019-08-09 | 中国地质科学院水文地质环境地质研究所 | A kind of in-situ acquisition filter device and its application method based on phreatic water |
| CN110501203A (en) * | 2019-08-05 | 2019-11-26 | 未名环境分子诊断(广东)有限公司 | The Preconcentration in-situ purification device and method of psychoactive drug substance in a kind of water environment |
Non-Patent Citations (1)
| Title |
|---|
| 刘玲玲: "固相萃取/气相色谱－质谱法对土壤中有机氯农药的分析及基质效应研究", 《分析测试学报》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112964509B (en) | 2023-03-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN206369647U (en) | A kind of strand tidal beach wetland Sediment Pore Water sampler | |
| CN102895798B (en) | Simple semi-automatic chromatographic column | |
| CN101322885A (en) | Soil anaerobic leaching method and device thereof | |
| CN109855913A (en) | Underground water-borne radioactivity inert gas nucleic surveys year sampling system and its method of sampling | |
| CN105126385B (en) | Automatic liquid-liquid extraction device | |
| CN210720067U (en) | Rotatable serial-type earth pillar test device | |
| CN112964509B (en) | Natural water sample in-situ suction filtration and solid phase extraction integrated operation system and operation method thereof | |
| CN106932259A (en) | A kind of device for extracting soil hydrophobic DOM | |
| CN106872225A (en) | A kind of water sample pretreatment device and its application method | |
| CN2789754Y (en) | Extracting and purifying device | |
| CN203663496U (en) | Quick and convenient solid-phase extraction device using functional non-woven fabric membrane | |
| CN106834421B (en) | Full-automatic assembly line collection bacterium operating method and system towards the bottled powder test sample in XiLin | |
| CN105699131B (en) | A kind of Suction filtration device | |
| CN111795862A (en) | Device and method for sampling dioxin in water with automatic extraction function | |
| CN103007575A (en) | Rapid, simple and convenient solid phase extracting device applying functional non-woven fabric membrane | |
| CN204767597U (en) | Diaphragm type solid -phase extraction device | |
| CN100457272C (en) | Multi manifold vacuum device, solid phase extroction pipe, liquid phase extraction pipe and solid phosel solicd liquid phase negative pressure extraction instrument | |
| CN106893114B (en) | A kind of equipment for extracting soil humic acid full constituent | |
| CN106872231B (en) | Soil hydrophobic fulvic acid component extraction purification device | |
| CN203178108U (en) | Enriching device for semi-volatile organic compounds in underground water | |
| CN211357983U (en) | Small liquid filter | |
| CN216798794U (en) | Infusion bottle type large-volume sample introduction solid phase extraction device | |
| CN207371357U (en) | A kind of efficient isotopic separation device | |
| CN202267622U (en) | Filtration-solid-phase extraction combined device | |
| CN206876461U (en) | One kind detection pretreating device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |