CN211603025U - Capillary electrophoresis apparatus for water environment field monitoring - Google Patents
Capillary electrophoresis apparatus for water environment field monitoring Download PDFInfo
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- CN211603025U CN211603025U CN202020263182.2U CN202020263182U CN211603025U CN 211603025 U CN211603025 U CN 211603025U CN 202020263182 U CN202020263182 U CN 202020263182U CN 211603025 U CN211603025 U CN 211603025U
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- UELLBEZSKVQTLW-UHFFFAOYSA-N 1,1-bis(2-hydroxyethylamino)-2-(hydroxymethyl)propane-1,3-diol Chemical compound OCCNC(O)(C(CO)CO)NCCO UELLBEZSKVQTLW-UHFFFAOYSA-N 0.000 description 1
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Abstract
The utility model relates to a water sample pollutant monitoring technology field especially relates to a capillary electrophoresis apparatus for water environment on-the-spot monitoring, including sampling device, the quartz capillary and the detector of inner wall coating, sampling device includes air supply, first solenoid valve, peristaltic pump, filter head, liquid storage bottle, six-way valve, second solenoid valve, second buffer solution liquid storage bottle, buffer solution liquid storage chamber and three way connection; the outlet of the second electromagnetic valve is connected with a waste liquid discharge pipe, the left end of the quartz capillary is inserted from the right port of the three-way joint, the insertion depth is based on half of the distance between the left port and the right port of the three-way joint, a conductive needle connected with a grounding end is arranged in a pipeline between the left port of the three-way joint and the second electromagnetic valve, the detector is a non-contact conductivity detector, and a complete electrophoresis loop is formed between the conductive needle and a high-voltage end electrode.
Description
Technical Field
The utility model belongs to the technical field of water sample pollutant monitoring, especially, relate to a capillary electrophoresis apparatus for water environment on-the-spot monitoring.
Background
With the rapid development of social economy, a large amount of pollutants discharged by human beings enter a water body, so that the water quality is deteriorated, the ecological environment is damaged, and the normal life of the human beings is seriously influenced. The concentration of ionic compounds, particularly nitrate nitrogen, nitrite nitrogen, ammonia nitrogen and phosphate is one of important indexes reflecting the water quality and the health condition of an aquatic ecosystem. Therefore, monitoring of ionic compounds in a body of water becomes of particular importance. Water sample collection is usually carried out on site in the traditional method for water quality monitoring, and then collected samples are transported to a laboratory for water quality detection. The method has a plurality of problems, and the target object to be detected can be polluted or degraded in the transferring process, so that the pollutants in the collected water sample cannot be accurately determined qualitatively and quantitatively; the monitoring data amount is small, and the change rule of the environmental parameters cannot be truly reflected. In recent years, on-site analytical instruments have been widely used to monitor ionic compounds in water samples in real time. Most automated field instruments are based on electrochemical or colorimetric methods. In the case of electrochemical sensors, there is still a need to further improve selectivity and durability to accommodate long-term field applications. Although in-situ analysis of natural waters can be achieved by combining colorimetry with flow analysis techniques, the determination of each parameter requires a specific reaction to form a colored compound for spectrophotometric detection, and multiple parallel channels are required for the measurement of multiple analytes, resulting in a complex and expensive overall system. In the prior art, an ion chromatography or capillary electrophoresis-ultraviolet detection technology is adopted to simultaneously detect a plurality of ionic compounds in a water body, but the implemented equipment has large volume and high price, has high requirements on the operating environment, is generally used in a laboratory and is difficult to be used in various complicated water body sites to continuously monitor the water quality.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to provide a capillary electrophoresis apparatus for water environment field monitoring small, with low costs, adaptation scene are wide, the precision is high.
The technical scheme for realizing the purpose of the utility model is as follows,
a capillary electrophoresis apparatus for monitoring water environment on site comprises a sample introduction device, a quartz capillary tube with a coating on the inner wall and a detector, wherein the sample introduction device comprises a gas source, a first electromagnetic valve, a peristaltic pump, a filter head, a liquid storage bottle, a six-way valve, a second electromagnetic valve, a second buffer liquid storage bottle, a buffer liquid storage chamber and a three-way connector; the outlet of the gas source is respectively connected with the inlet of a first electromagnetic valve and the inlet of a liquid storage bottle through a pressure controller, the outlet of the first electromagnetic valve is communicated with the atmosphere, the peristaltic pump is connected with a six-way valve through a filter head, the outlet of the liquid storage bottle is connected with the upper port of a three-way joint after passing through the six-way valve, the left port of the three-way joint is connected with a second electromagnetic valve through a buffer liquid storage chamber, the outlet of the second electromagnetic valve is connected with a waste liquid discharge pipe, the left end of a quartz capillary tube is inserted from the right port of the three-way joint, the insertion depth is based on half of the distance between the left port and the right port of the three-way joint, the right port of the quartz capillary tube is connected with a second buffer liquid storage bottle, an electrode connected with a high-pressure end is arranged in the second buffer liquid storage bottle, a conductive needle connected with a grounding, when the electrophoresis device works, a complete electrophoresis loop is formed between the conductive needle head connected with the grounding end and the high-voltage end electrode.
Further, the left port of the quartz capillary tube is flush with the left port of the three-way joint.
Further, sampling device still includes the mixing coil pipe, the peristaltic pump is the binary channels peristaltic pump, and one of them passageway of binary channels peristaltic pump is equipped with the filter head, this passageway are water sample passageway, and another passageway is interior standard passageway, and water sample passageway and interior standard passageway are connected the entry of mixing coil pipe after merging, and the export of mixing coil pipe meets with six-way valve.
The capillary electrophoresis apparatus for the water environment field monitoring has the advantages of simple structure, small volume and convenient maintenance, is suitable for various complicated water environments to carry out field water quality monitoring, and has obvious economic benefit.
The use method of the capillary electrophoresis apparatus for the water environment field monitoring comprises the following steps:
s1, initializing the system, switching the six-way valve to the sampling state, mixing the water sample and the internal standard substance through the mixing coil, loading the mixture into the quantitative ring of the six-way valve, opening the second electromagnetic valve, closing the first electromagnetic valve, and driving the background buffer solution in the liquid storage bottle to flush the sample inlet of the quartz capillary by the output pressure of the gas source;
s2, switching the six-way valve to a sample injection state;
s3, driving the quantitative intra-annular water sample/internal standard substance mixed solution to flow into the three-way joint under the pressure of the gas source, and ensuring that the left port of the quartz capillary is immersed into the water sample/internal standard substance mixed solution;
s4, closing the second electromagnetic valve, switching the six-way valve to the sample loading state, and driving the water sample/internal standard substance mixed solution to be pressed into the quartz capillary by the pressure of the gas source;
s5, opening the second electromagnetic valve, flushing the conductive needle at the grounding end by the buffer solution in the air source pressure driving tube,
s6, closing the second electromagnetic valve, setting the output of the pressure controller of the gas source to be 0, opening the first electromagnetic valve, and releasing the pressure in the pipeline to ensure that the left port and the right port of the quartz capillary are balanced with the atmospheric pressure;
s7, inputting high-voltage direct current to the electrodes according to the separation requirement, wherein when cations are separated, the high-voltage end is connected with a direct current cathode, and the ground end is connected with a direct current anode; when separating anions, the high-voltage end is connected with a direct-current positive electrode, and the ground end is connected with a direct-current negative electrode; simultaneously, automatically triggering a non-contact conductivity detector to perform a data acquisition task in the electrophoretic separation process;
s8, closing the first electromagnetic valve, opening the second electromagnetic valve, and driving the background buffer solution flushing buffer solution storage chamber, the conductive needle and the grounding end by the air pressure output by the air source;
s9, closing the second electromagnetic valve, increasing the output pressure of the gas source, and driving the background buffer solution to rapidly flush the quartz capillary;
and S10, setting the output of the pressure controller of the air source to be 0, opening the first electromagnetic valve, releasing the pressure in the pipeline, and waiting for entering the next cycle.
The six-way valve is also called a six-way sample injection valve and is an existing product, the six-way valve is provided with a quantitative ring, when the sample loading state is switched, a detection sample enters the quantitative ring, and when the sample injection state is switched, the detection sample in the quantitative ring is output from the six-way valve.
The utility model discloses a capillary electrophoresis apparatus for water environment on-the-spot monitoring has following whole or partial technological effect: the device has the advantages of simple structure, small volume, convenient maintenance, suitability for various complex water environments for field water quality monitoring and obvious economic benefit; the capillary electrophoresis apparatus can measure anions and cations simultaneously, the obtained water quality parameters are multiple, and the capillary modified by the chemical coating can effectively inhibit electroosmotic flow, so that the anions and cations in the water environment can be detected simultaneously by switching the polarity of the high-voltage power supply; thirdly, the measurement precision is high, and the pneumatic shunting type automatic sample introduction is adopted, so that the sample introduction amount is accurately controlled between nL-pL; and fourthly, the stability is good, and the introduction of the internal standard substance enables the system to correct the analysis result in a complex environment, so that the stability of the system is enhanced.
Drawings
Fig. 1 is a schematic structural diagram of an embodiment of the present invention;
FIG. 2 is a schematic view of the internal structure of the three-way joint of FIG. 1;
FIG. 3 is a graph showing the trend of the typical anion concentration with the time of detection obtained by using the capillary electrophoresis apparatus of the embodiment of the present invention and the ion chromatography method in the same water area;
fig. 4 is a typical trend graph of cation concentration with time of detection obtained by the capillary electrophoresis apparatus of the embodiment of the present invention for the water area detection shown in fig. 3.
In the figure, 1: a gas source; 2: a pressure controller: 3: a first solenoid valve; 4: a liquid storage bottle; 5: a six-way valve; 6: a three-way joint; 7: a mixing coil; 8, a filter head; 9: a two-channel peristaltic pump; 10: a quartz capillary tube; 11: a non-contact conductivity detector; 12: a second buffer solution storage bottle; 13: a buffer solution storage chamber; 14: a ground terminal; 15: a high-voltage end; 16: a second solenoid valve.
Detailed Description
Referring to fig. 1 and 2, a capillary electrophoresis apparatus for monitoring water environment on site comprises a sample introduction device, a quartz capillary 10 with a coating on the inner wall and a detector, wherein the sample introduction device comprises a gas source 1, a first electromagnetic valve 3, a mixing coil 7, a two-channel peristaltic pump 9, a filter head 8, a liquid storage bottle 4, a six-way valve 5, a second electromagnetic valve 16, a second buffer liquid storage bottle 12, a buffer liquid storage chamber 13 and a three-way joint 6; an outlet of the gas source 1 is respectively connected with inlets of a first electromagnetic valve 3 and a liquid storage bottle 4 through a pressure controller 2, and an outlet of the first electromagnetic valve 3 is communicated with the atmosphere; one channel of the two-channel peristaltic pump 9 is provided with a filter head 8, the channel is a water sample channel, the other channel is an internal standard channel, the water sample channel and the internal standard channel are combined and then connected with the inlet of the mixing coil 7, the outlet of the mixing coil 7 is connected with the six-way valve 5, and the internal standard and the water sample are mixed and then detected so as to calibrate and eliminate the influence on the analysis result caused by the change of the detection environment and be beneficial to improving the accuracy of the analysis result; the outlet of the liquid storage bottle 4 is connected with the upper port of the three-way joint 6 after passing through the six-way valve 5, the left port of the three-way joint 6 is connected with a second electromagnetic valve 16 through a buffer liquid storage chamber 13, the outlet of the second electromagnetic valve 16 is connected with a waste liquid discharge pipe, the left end of the quartz capillary tube 10 is inserted from the right port of the three-way joint 6, the insertion depth is based on the half distance exceeding or equal to the left and right ports of the three-way joint 6, so as to ensure that the left port of the quartz capillary tube 10 is immersed in the detection sample liquid when the detection sample liquid enters the three-way joint 6, the left port of the quartz capillary tube 10 is flush with the left port of the three-way joint 6 in the embodiment, the arrangement is favorable for quick positioning when the quartz capillary tube 10 is replaced, the maintainability of the capillary electrophoresis apparatus is improved, the right port of the quartz capillary tube 10 is connected with, a conductive needle connected with a grounding terminal 14 is arranged in a pipeline between the left port of the three-way joint 6 and the second electromagnetic valve 16, a detector is externally connected to the middle part of the quartz capillary tube 10, the detector is a non-contact conductivity detector 11, when the electrophoresis apparatus works, a complete electrophoresis loop is formed between the conductive needle connected with the grounding terminal 14 and a high-voltage terminal 15 electrode,
the capillary electrophoresis apparatus for the water environment field monitoring has the advantages of simple structure, good maintainability and high detection precision, and is suitable for the field water environment water quality continuous monitoring.
The use method of the capillary electrophoresis apparatus comprises the following steps:
s1, initializing a system, switching the six-way valve 5 to a sample loading state, mixing the water sample and the internal standard substance through the mixing coil 7 under the action of a two-channel peristaltic pump, loading the mixture into a quantitative ring of the six-way valve 5, closing the first electromagnetic valve 3, opening the second electromagnetic valve 16, outputting 16 psi pressure by the air source 1 to drive the background buffer solution in the liquid storage bottle 4 to flush the sample inlet of the quartz capillary tube 10, and flushing for 15S;
s2, switching the six-way valve 5 to a sample injection state for 1S;
s3, driving the quantitative intra-annular water sample/internal standard substance mixed solution to flow into the three-way joint 6 under the pressure of the gas source 1, and ensuring that the left port of the quartz capillary is immersed into the water sample/internal standard substance mixed solution for 1S;
s4, closing the second electromagnetic valve 16, switching the six-way valve 5 to a sample loading state, and driving the water sample/internal standard substance mixed solution to be pressed into the quartz capillary tube 10 by the pressure of the gas source 1 for 4S;
s5, opening the second electromagnetic valve 16, flushing the conductive needle of the grounding end 14 by the buffer solution in the pressure driving tube of the air source 1 for 15S continuously, and aiming at cleaning the left port of the quartz capillary, the buffer solution storage chamber and the mixed solution of the sample and the internal standard substance remained in the previous step in the conductive needle to avoid influencing the measurement result;
s6, closing the second electromagnetic valve 16, setting the output of the pressure controller 2 of the gas source 1 to 0 psi, opening the first electromagnetic valve 3, releasing the pressure in the pipeline, and enabling the left port and the right port of the quartz capillary tube 10 to be balanced with the atmospheric pressure for 5S;
s7, inputting high-voltage direct current of 15 kv to the electrode according to the separation requirement, wherein when separating positive ions, the high-voltage end 15 is connected with a direct current negative electrode, and the grounding end 14 is connected with a direct current positive electrode; when separating anions, the high-voltage end 15 is connected with a direct-current positive electrode, and the grounding end 14 is connected with a direct-current negative electrode; simultaneously, automatically triggering the non-contact conductivity detector 11 to perform a data acquisition task in the electrophoretic separation process, wherein the detection duration is 480 s;
s8, closing the first electromagnetic valve 3, opening the second electromagnetic valve 16, and outputting 16 psi pressure by the air source 1 to drive the background buffer solution to flush the buffer solution storage chamber 13 and the conductive needle for 6S;
s9, closing the second electromagnetic valve 16, increasing the output pressure of the gas source 1 to 25 psi, driving the background buffer solution to rapidly flush the quartz capillary tube 10 for 60S; the method aims to use a background buffer solution to wash out a sample and an internal standard substance possibly remained in a quartz capillary tube so as to prepare for normal running of next electrophoresis;
s10, the output of the pressure controller 2 of the gas source 1 is set to 0, the first electromagnetic valve 3 is opened, the pressure in the pipeline is released, and the release lasts for 10S.
See the following flow chart for the above methods of use.
The parameters of the table can be input into an upper computer program written by LabVIEW, each step is controlled by the upper computer program by scanning the program execution content line by line, and the operation and data acquisition of each part of the control system are automatically controlled by a computer. In the table, "A" represents that the six-way valve 5 is in a sample loading state, "B" represents that the six-way valve 5 is in a sample feeding state, and "ON" represents that the six-way valve is in a power-on opening state; "-" indicates a power-off state.
Using the capillary electrophoresis apparatus of this example, the relative standard deviations in migration time, peak height and peak area of the capillary electrophoresis apparatus were less than 5.00% in about 1700 electrophoretic analyses according to the above-described method of use, demonstrating that the capillary electrophoresis apparatus can be operated continuously for a long period of time.
The capillary electrophoresis apparatus of this example was used to detect a water sample from the water area of the acacia lake at the university of Guilin electronics technology, and during the detection, Bis (2-hydroxyethylamino) Tris (hydroxymethyl) methane/3- (N-morpholino) propanesulfonic acid (Bis-Tris/MOPS) and 2 mM 18-crown-6 were used as the background buffer, and lithium perchlorate (LiClO4) was used as the internal standard substance. And the water samples in the water area are detected and compared by adopting an ion chromatography method in the same time period. Fig. 3 is a comparison graph of typical variation trends of anion concentration with detection time obtained by two detection methods, and fig. 4 is a comparison graph of variation trends of typical cation concentration with detection time obtained by using the capillary electrophoresis apparatus of the present embodiment in the same time period.
Claims (3)
1. A capillary electrophoresis apparatus for monitoring water environment on site comprises a sample introduction device, a quartz capillary tube with a coating on the inner wall and a detector, and is characterized in that the sample introduction device comprises a gas source, a first electromagnetic valve, a peristaltic pump, a filter head, a liquid storage bottle, a six-way valve, a second electromagnetic valve, a second buffer liquid storage bottle, a buffer liquid storage chamber and a three-way connector; the outlet of the air source is respectively connected with the inlet of a first electromagnetic valve and the inlet of a liquid storage bottle through a pressure controller, the outlet of the first electromagnetic valve is communicated with the atmosphere, the peristaltic pump is connected with a six-way valve through a filter head, the outlet of the liquid storage bottle is connected with the upper port of a three-way joint after passing through the six-way valve, the left port of the three-way joint is connected with a second electromagnetic valve through a buffer liquid storage chamber, the outlet of the second electromagnetic valve is connected with a waste liquid discharge pipe, the left end of a quartz capillary tube is inserted from the right port of the three-way joint, the insertion depth is determined by exceeding or equal to half of the distance between the left port and the right port of the three-way joint, the right port of the quartz capillary tube is connected with a second buffer liquid storage bottle, an electrode connected with a high-pressure end is arranged in the second buffer liquid storage bottle, the detector is a non-contact conductivity detector, and when the detector works, a complete electrophoresis loop is formed between the conductive needle head connected with the grounding end and the high-voltage end electrode.
2. The capillary electrophoresis apparatus for in-situ monitoring of water environment according to claim 1 wherein the quartz capillary left port is flush with the tee junction left port.
3. The capillary electrophoresis apparatus for water environment field monitoring according to claim 1 or 2, wherein the sample injection device further comprises a mixing coil, the peristaltic pump is a two-channel peristaltic pump, one channel of the two-channel peristaltic pump is provided with the filter head, the channel is a water sample channel, the other channel is an internal standard channel, the water sample channel and the internal standard channel are combined and then connected with an inlet of the mixing coil, and an outlet of the mixing coil is connected with the six-way valve.
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| CN202020263182.2U CN211603025U (en) | 2020-03-06 | 2020-03-06 | Capillary electrophoresis apparatus for water environment field monitoring |
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| CN202020263182.2U CN211603025U (en) | 2020-03-06 | 2020-03-06 | Capillary electrophoresis apparatus for water environment field monitoring |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111141810A (en) * | 2020-03-06 | 2020-05-12 | 桂林电子科技大学 | Capillary electrophoresis apparatus for water environment field monitoring and use method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111141810A (en) * | 2020-03-06 | 2020-05-12 | 桂林电子科技大学 | Capillary electrophoresis apparatus for water environment field monitoring and use method thereof |
| CN111141810B (en) * | 2020-03-06 | 2023-10-27 | 桂林电子科技大学 | Capillary electrophoresis apparatus for water environment on-site monitoring and use method thereof |
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