CN111220812A - Automatic sample purification and pollution-free sample introduction method - Google Patents
Automatic sample purification and pollution-free sample introduction method Download PDFInfo
- Publication number
- CN111220812A CN111220812A CN201811404970.2A CN201811404970A CN111220812A CN 111220812 A CN111220812 A CN 111220812A CN 201811404970 A CN201811404970 A CN 201811404970A CN 111220812 A CN111220812 A CN 111220812A
- Authority
- CN
- China
- Prior art keywords
- sample
- way valve
- valve
- cleaning
- sample injection
- 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
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N35/10—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices
- G01N35/1004—Cleaning sample transfer 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
- G01N1/34—Purifying; Cleaning
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Engineering & Computer Science (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention relates to a practical pollution-free sample feeding, cleaning and eluting method in organic pollutant sample analysis and purification equipment, which realizes pollution-free sample feeding and sequential elution of a purification column by a set of liquid pump and a plurality of valve control units.
Description
Technical Field
The invention belongs to the technical field of organic pollutant sample analysis and purification, and relates to a pollution-free sample introduction method of an automatic organic pollutant purification device.
Background
The analysis of ultra trace toxic organic pollutants requires sample purification to reduce the interference of interfering substances on the analysis result, such as the analysis of persistent organic pollutants of dioxin and polychlorinated biphenyl. Since the manual chromatography column purification consumes a lot of manpower and time, and it is difficult to ensure the reproducibility, some enterprises have developed automatic sample purification apparatuses one after another.
The existing automatic purification equipment mainly comprises an automatic purifier of American FMS company, an automatic purifier of Beijing prilatake company and an automatic purifier of Germany Dextech. The products of FMS company and Pritake company generally adopt the technology of single liquid pump sample introduction and purification, and the method of the sample is sent into the purification system after being sucked by the liquid pump, and certain cross contamination exists because of the dead volume of the pump. German Dextech company adopts two sets of pumps, wherein one set of pump is used for sucking samples into a quantitative tube, the quantitative tube is used for sampling samples through the second set of pump, and the other set of pump is used for purification driving.
Disclosure of Invention
The invention aims to develop an automatic sample purification and pollution-free sample introduction method, which realizes quantitative tube sample introduction and purification driving by utilizing a set of pumps. The method has the advantages of simple equipment and no cross contamination.
The technical scheme includes that the sample automatic purification pollution-free sample introduction device comprises a six-position valve, a six-way valve, a four-way valve, a large-volume quantitative tube, a self-cleaning sample introduction needle, a liquid pump, a purification column and a pipeline. Selecting the type of the absorption solvent and the absorption sample through a six-position valve; controlling the sample suction and the suction of the sample injection needle and the sample bottle cleaning solution through a six-way valve; controlling the sample sucked into the quantitative tube to enter the purifying column through the six-way valve to complete purification; the direction of the solvent is controlled by the four-way valve, so that the cleaning of the sample injection needle and the sample bottle cleaning solution, the sample loading of the purification column and the elution of different solvents are completed.
The principle of the invention is shown in figure 1. The device comprises a sample injection needle (7), a conduit (9), a self-cleaning pipeline (8), a solvent spray outlet (11) of the self-cleaning pipeline, a dosing pipe (13), a liquid pump (18), a solvent (25), a one-inlet-six-outlet multi-position valve (M0) (also called as a flow path selector or a flow divider, wherein the one inlet refers to a common interface), a two-position four-way valve (M2), a two-position six-way valve (M1) and a purification column (26).
An automatic purifying and pollution-free sample introduction method for a sample adopts a device comprising a sample introduction needle, a self-cleaning pipeline, a solvent ejection port of the self-cleaning pipeline, a quantitative tube, a liquid pump, a multi-position valve (M0) with one inlet and six outlets, a two-position four-way valve (M2), a two-position six-way valve (M1) and a purifying column.
The one-inlet six-outlet multi-position valve (M0) comprises an outlet and a port with 19-24 positions, the two-position four-way valve (M2) comprises a port with 14-17 positions, and the two-position six-way valve (M1) comprises a port with 1-6 positions.
The self-cleaning pipeline is a pipeline with openings at two ends, the lower outlet end of the self-cleaning pipeline is welded with the sample injection needle, and more than 2 solvent spray outlets of the self-cleaning pipeline are arranged at the bottom end of the self-cleaning pipeline; the sample injection needle passes through the self-cleaning pipeline, and the sample injection needle penetrates from the inlet to the bottom.
The solvent inlet of the liquid pump is connected with a common interface of a one-inlet six-outlet multi-position valve (M0), and the solvent outlet of the liquid pump is connected with the 16 position of a two-position four-way valve (M2); the 17 th bit of the two-position four-way valve (M2) is connected with the 5 th bit of the two-position six-way valve (M1); 6 of the two-position six-way valve (M1) is connected with the purifying column; 1 and 4 positions of the two-position six-way valve (M1) are respectively connected with two ends of the quantitative tube; 2 bits of the two-position six-way valve (M1) are connected with a conduit of the sample injection needle; the 3 position of the two-position six-way valve (M1) is connected with the 19 position of a one-in six-out multi-position valve (M0); the self-cleaning pipeline of the sample injection needle is connected with the 15 th position of the two-position four-way valve (M2) through a guide pipe; more than two different solvents are respectively connected to more than two positions of 20, 21, 22, 23 and 24 of the one-in six-out multi-position valve (M0).
The sample is injected without pollution without flowing through the liquid pump by the valve control and the quantitative tube, and the automatic cleaning of the injection needle and the sequential elution of a plurality of elution solvents of the purifying column are completed simultaneously.
The sample injection method has the advantages that the sample injection is pollution-free: the sample is sucked into the quantitative tube, and the sample in the quantitative tube is introduced into the purifying column through valve switching, so that the sample does not need to pass through a liquid pump; the system can finish the automatic cleaning of the sample injection needle and the sample bottle by switching the flow path through the valve, and the cleaning liquid is sucked into the quantitative tube.
The sample injection method has the following functions of eluting a plurality of solvents of the purifying column: and selecting an elution solvent through a six-position valve, and sequentially finishing the loading and the sequential elution of the purification column.
In the sample injection method, in the first stage, a sample injection needle is inserted into a liquid sample, and the 1-2 position communication, the 3-4 position communication and the 1-4 position communication of a two-position six-way valve (M1) are communicated with a quantitative tube; a six-in, multi-position valve (M0) in position 19; and 16-17 positions of the two-position four-way valve (M2) are communicated. At the moment, the liquid pump operates, the extracted sample enters the quantitative tube through the sample injection needle and the two-position six-way valve (M1), the flow rate of the liquid pump is set according to the capacity of the quantitative tube, and the extraction of the sample is finished after the sample liquid completely enters the quantitative tube.
And in the second stage, a one-inlet six-outlet multi-position valve (M0) is positioned at the position of 20 and can extract the solvent 1, the 15-16 positions of the two-position four-way valve (M2) are communicated, a liquid pump operates to extract the solvent 1 to enter a self-cleaning pipeline of the sample injection needle, and the solvent is sprayed out from the self-cleaning pipeline to clean the outer wall of the sample injection needle and the inner wall of the sample bottle. And after the cleaning is finished, the first-stage flow is operated again, the cleaning liquid is sucked into the quantitative tube, and the second-stage cleaning flow and the first-stage sample injection flow are operated repeatedly for more than three times in sequence to finish the extraction of the sample and the cleaning of the sample injection needle and the sample injection pipeline.
In the third stage, after the sample is extracted, the one-inlet six-outlet multi-position valve (M0) is sequentially positioned at more than two of the positions 20, 21, 22, 23 and 24 for extracting different leaching solutions, and the 1-6 position and the 4-5 position of the two-position six-way valve (M1) are adjusted to be communicated; and (3) connecting 16-17 positions of the two-position four-way valve (M2), operating the liquid pump at the moment, pumping the solvent into the quantitative tube, driving the liquid sample in the quantitative tube to enter the purification column, and finishing the subsequent solvent elution and purification.
Drawings
FIG. 1 is a flow diagram of a non-contaminating sample injection circuit of an automatic purification system;
FIG. 2 is an integrated drawing of a needle and a self-cleaning channel.
Detailed Description
The invention is further described below with reference to fig. 1 and 2.
The solvent inlet of the liquid pump 18 is connected with the outlet (common interface) of a one-inlet six-outlet multi-position valve (M0), and the solvent outlet of the liquid pump 18 is connected with the 16 position of a two-position four-way valve (M2); the 17 th bit of the two-position four-way valve (M2) is connected with the 5 th bit of the two-position six-way valve (M1); 6 of the two-position six-way valve (M1) is connected with the purifying column 26; 1 and 4 positions of the two-position six-way valve (M1) are respectively connected with two ends of the quantitative pipe 13; 2 positions of the two-position six-way valve (M1) are connected with a conduit 10 of the sample injection needle 7; the 3 position of the two-position six-way valve M1 is connected with the 19 position of a one-in six-out multi-position valve (M0); a self-cleaning pipeline 8 of the sample injection needle is connected with the 15 th position of a two-position four-way valve (M2) through a guide pipe 9, and 11 is a solvent ejection port of the self-cleaning pipeline; the 20, 21, 22, 23 and 24 positions of a one-in six-out multi-position valve (M0) are respectively connected with different solvents.
In the first stage, a sample injection needle 7 is inserted into a liquid sample 12, and the 1-2 position, the 3-4 position and the 1-4 position of a two-position six-way valve (M1) are communicated with a quantification tube 13; a six-in, multi-position valve (M0) in position 19; and 16-17 positions of the two-position four-way valve (M2) are communicated. At this time, the liquid pump 18 operates, the extracted sample enters the quantitative tube 13 through the sample injection needle 7 and the two-position six-way valve (M1), the flow rate of the liquid pump 18 is set according to the capacity of the quantitative tube, and the extraction of the sample is finished after the sample liquid completely enters the quantitative tube 13.
In the second stage, a one-inlet six-outlet multi-position valve (M0) is positioned at the position of 20 and can extract solvent 1, the 15-16 positions of the two-position four-way valve (M2) are communicated, a liquid pump 18 operates, the extracted solvent 1 enters a cleaning pipeline 8 of the sample injection needle, and the solvent is sprayed out from the cleaning pipeline 8 to clean the outer wall of the sample injection needle and the inner wall of the sample bottle. After the cleaning is finished, the first-stage flow is operated again, the cleaning liquid is sucked into the quantitative tube 13, the second-stage cleaning flow and the first-stage sample injection flow are operated repeatedly for more than three times in sequence, and the extraction of the sample and the cleaning of the sample injection needle and the sample injection pipeline are finished.
In the third stage, after the sample is extracted, the one-inlet six-outlet multi-position valve (M0) is sequentially positioned at the positions of 20, 21 and 22 to extract different leaching solutions, and the 1-6 position and the 4-5 position of the two-position six-way valve (M1) are adjusted to be communicated; and (3) connecting 16-17 positions of the two-position four-way valve (M2), operating the liquid pump at the moment, pumping the solvent 25 into the quantitative tube 13, driving the liquid sample in the quantitative tube into the purification column 26, and finishing the subsequent solvent elution and purification.
Claims (4)
1. A sample automatic purification pollution-free sample introduction method is characterized in that:
the adopted device comprises a sample injection needle (7), a self-cleaning pipeline (8), a solvent spray outlet (11) of the self-cleaning pipeline, a quantitative pipe (13), a liquid pump (18), a multi-position valve (M0) with one inlet and six outlets, a two-position four-way valve (M2), a two-position six-way valve (M1) and a purification column (26);
the one-inlet six-outlet multi-position valve (M0) comprises an outlet and a port with 19-24 positions, the two-position four-way valve (M2) comprises a port with 14-17 positions, and the two-position six-way valve (M1) comprises a port with 1-6 positions;
the self-cleaning pipeline is a pipeline with openings at two ends, the lower outlet end of the self-cleaning pipeline is welded with the sample injection needle (7), and the bottom end of the self-cleaning pipeline is provided with more than 2 solvent spray outlets (11) of the self-cleaning pipeline; the sample injection needle penetrates through the self-cleaning pipeline and penetrates from the inlet to the bottom;
the solvent inlet of the liquid pump (18) is connected with a common interface of a one-inlet six-outlet multi-position valve (M0), and the solvent outlet of the liquid pump (18) is connected with the 16 position of a two-position four-way valve (M2); the 17 th bit of the two-position four-way valve (M2) is connected with the 5 th bit of the two-position six-way valve (M1); 6 of the two-position six-way valve (M1) is connected with the purifying column (26); 1 and 4 positions of the two-position six-way valve (M1) are respectively connected with two ends of the quantitative pipe (13); 2 bits of the two-bit six-way valve (M1) are connected with a conduit (10) of the sample injection needle (7); the 3 position of the two-position six-way valve (M1) is connected with the 19 position of a one-in six-out multi-position valve (M0); a self-cleaning pipeline (8) of the sample injection needle is connected with the 15 th position of the two-position four-way valve (M2) through a guide pipe (9); more than two different solvents are respectively connected to more than two positions of 20, 21, 22, 23 and 24 of the multi-position valve (M0) with one inlet and six outlets;
the sample is injected without pollution without flowing through the liquid pump by the valve control and the quantitative tube, and the automatic cleaning of the injection needle and the sequential elution of a plurality of elution solvents of the purifying column are completed simultaneously.
2. The sample injection method according to claim 1, characterized in that: pollution-free sample injection: the sample is sucked into the quantitative tube, and the sample in the quantitative tube is introduced into the purifying column through valve switching, so that the sample does not need to pass through a liquid pump; the system can finish the automatic cleaning of the sample injection needle and the sample bottle by switching the flow path through the valve, and the cleaning liquid is sucked into the quantitative tube.
3. The sample injection method according to claim 1, characterized in that: the purification column has a plurality of solvent elution functions: and selecting an elution solvent through a six-position valve, and sequentially finishing the loading and the sequential elution of the purification column.
4. A sample introduction method according to any of claims 1-3, characterized in that:
in the first stage, a sample injection needle (7) is inserted into a liquid sample (12), and the 1-2 position, the 3-4 position and the 1-4 position of a two-position six-way valve (M1) are communicated with a quantification tube (13); a six-in, multi-position valve (M0) in position 19; 16-17 positions of a two-position four-way valve (M2) are communicated; at the moment, the liquid pump (18) operates, the extracted sample enters the quantitative tube (13) through the sample injection needle (7) and the two-position six-way valve (M1), the flow rate of the liquid pump (18) is set according to the capacity of the quantitative tube, and the extraction of the sample is finished after the sample liquid completely enters the quantitative tube (13);
in the second stage, a one-inlet six-outlet multi-position valve (M0) is positioned at the position of 20 and can extract a solvent 1(25), the 15-16 positions of a two-position four-way valve (M2) are communicated, a liquid pump (18) operates to extract the solvent 1 to enter a self-cleaning pipeline (8) of a sample injection needle, and the solvent is sprayed out from the self-cleaning pipeline (8) to clean the outer wall of the sample injection needle and the inner wall of a sample bottle; after cleaning, the first-stage flow is operated again, cleaning liquid is sucked into the quantitative tube (13), and the second-stage cleaning flow and the first-stage sample injection flow are operated repeatedly for more than three times in sequence to finish the extraction of samples and the cleaning of the sample injection needle and the sample injection pipeline;
in the third stage, after the sample is extracted, the one-inlet six-outlet multi-position valve (M0) is sequentially positioned at more than two of the positions 20, 21, 22, 23 and 24 for extracting different leaching solutions, and the 1-6 position and the 4-5 position of the two-position six-way valve (M1) are adjusted to be communicated; and (3) connecting 16-17 positions of the two-position four-way valve (M2), operating the liquid pump at the moment, pumping the solvent (25) into the quantitative tube (13), driving the liquid sample in the quantitative tube to enter the purification column (26), and finishing the subsequent solvent elution and purification.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811404970.2A CN111220812B (en) | 2018-11-23 | 2018-11-23 | Automatic sample purification and pollution-free sample introduction method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811404970.2A CN111220812B (en) | 2018-11-23 | 2018-11-23 | Automatic sample purification and pollution-free sample introduction method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111220812A true CN111220812A (en) | 2020-06-02 |
| CN111220812B CN111220812B (en) | 2021-06-29 |
Family
ID=70828565
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811404970.2A Active CN111220812B (en) | 2018-11-23 | 2018-11-23 | Automatic sample purification and pollution-free sample introduction method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111220812B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001255315A (en) * | 2000-03-08 | 2001-09-21 | Shimadzu Corp | Liquid chromatograph |
| CN1527052A (en) * | 2003-03-05 | 2004-09-08 | 株式会社岛津制作所 | Automatic sampling device and method for washing needle thereof |
| CN101196497A (en) * | 2006-12-06 | 2008-06-11 | 株式会社岛津制作所 | Auto-sampler cleaning mechanism |
| CN105891391A (en) * | 2016-06-29 | 2016-08-24 | 天津博纳艾杰尔科技有限公司 | Automatic sampling device |
| CN206772913U (en) * | 2017-05-02 | 2017-12-19 | 维科托（北京）科技有限公司 | Liquid chromatogram atom spectrum combined system |
-
2018
- 2018-11-23 CN CN201811404970.2A patent/CN111220812B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001255315A (en) * | 2000-03-08 | 2001-09-21 | Shimadzu Corp | Liquid chromatograph |
| CN1527052A (en) * | 2003-03-05 | 2004-09-08 | 株式会社岛津制作所 | Automatic sampling device and method for washing needle thereof |
| CN101196497A (en) * | 2006-12-06 | 2008-06-11 | 株式会社岛津制作所 | Auto-sampler cleaning mechanism |
| CN105891391A (en) * | 2016-06-29 | 2016-08-24 | 天津博纳艾杰尔科技有限公司 | Automatic sampling device |
| CN206772913U (en) * | 2017-05-02 | 2017-12-19 | 维科托（北京）科技有限公司 | Liquid chromatogram atom spectrum combined system |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111220812B (en) | 2021-06-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104690047B (en) | A kind of liquid chromatograph sample intake passage cleans device | |
| US7347936B2 (en) | Liquid chromatograph | |
| EP2835636A1 (en) | Liquid chromotography device, liquid chromotography analysis process, and liquid chromotography analysis program | |
| CN103235074B (en) | High performance liquid chromatography online analysis method and application thereof | |
| CN104062170A (en) | Automatic online micro-scale sample dilution and mixing system and mixing method | |
| CN111220812B (en) | Automatic sample purification and pollution-free sample introduction method | |
| CN106546687B (en) | Miniaturized device for gel chromatography purification system and use method thereof | |
| CN217092185U (en) | Chromatography purification system | |
| CN203908855U (en) | Diluting and mixing device of automatic online sample and chromatographic analysis instrument | |
| CN108548879B (en) | Automatic change rapid detection equipment | |
| CN104062167A (en) | Automatic online sample dilution and mixing device and mixing method | |
| CN206557171U (en) | It is a kind of to be used for the automatic pretreating device of trace phenol in water | |
| CN114392583A (en) | Chromatographic purification system and purification method | |
| CN2832294Y (en) | Automatic flow path separating device | |
| CN103969388B (en) | Perchlorate's on-line monitoring system | |
| CN115616233A (en) | Online dilution device and method for flow injection analyzer | |
| CN115645986A (en) | Full-automatic solid phase extraction instrument | |
| CN203908852U (en) | Automatic online micro sample diluting and mixing system | |
| CN212459561U (en) | Double-channel ion chromatography detection system and sample injector with series double-valve structure | |
| CN212159315U (en) | Device for automatically enriching red tide toxins in concentrated seawater | |
| CN204892469U (en) | Wash integrated equipment of chromatographic column | |
| CN104569456B (en) | Injector | |
| CN203908853U (en) | Automatic online micro-sample diluting and mixing system | |
| CN106979985B (en) | Liquid chromatogram atomic spectrum combined system | |
| CN103901144B (en) | Automatic sampler |
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 |