Chromatographic baseline suppression device and method of manufacturing the same

Abstract

The present application provides a chromatographic baseline suppression device and a manufacturing method thereof, the chromatographic baseline suppression device comprises a container and two ion exchange membranes, the two ion exchange membranes divide the inside of the container into a first part, a second part and a third part, the second part has an inlet and an outlet; the chromatographic baseline suppression device further comprises two electrodes respectively in the first part and the second part, the electrodes comprise a matrix porous material layer and a polymer layer, the matrix porous material layer is conductive and is connected with the ion exchange membrane. The present application has the advantages of small noise and the like.

Description

TECHNICAL FIELD

[0001] The present application relates to ion chromatography, in particular to a chromatography baseline suppression device and a manufacturing method thereof. BACKGROUND

[0002] The ion chromatography self-regeneration suppression device generates H+ and OH+ ions by electrolyzing water, and replaces the ions in the eluent through an ion exchange membrane, so that the KOH or MSA eluent corresponding to the suppressor will be converted into water, thereby reducing the baseline background, and the signal of the sample passing through the suppressor will be improved. The conventional suppressor electrode has two electrode chambers, which actually include a platinum electrode and a polymer material. The current technical solution has the following problems:

[0003] 1. Low suppression efficiency. The potential field inside the current solution decreases from the inlet end of the mobile phase to the outlet end, that is, the inlet solution has high concentration and large current density, and the outlet solution has low concentration and small current density. The non-uniform electric field will limit the suppression efficiency to the membrane exchange capacity.

[0004] 2. Low current efficiency and difficult to control thermal noise. The flat sheet electrode and the membrane are directly present at a certain distance, which causes a certain potential difference in the electrolysis chamber, thereby causing the current efficiency to decrease, the heat generation to increase, the noise to increase, and the instrument sensitivity to decrease.

[0005] 3. Low reaction efficiency, limited contact area between platinum sheet and water.

[0006] 4. Difficult to control the bubbles generated by electrolyzing water, which causes large noise and decreases the instrument sensitivity

[0007] 5. Poor repeatability, electrode, resin or screen material filling process in the electrolysis chamber, which inevitably causes differences between each individual and cannot guarantee consistency. SUMMARY

[0008] To solve the above problems in the prior art, the present application provides a chromatography baseline suppression device.

[0009] The purpose of the present application is achieved by the following technical solutions:

[0010] The chromatography baseline suppression device comprises a container and two ion exchange membranes, the two ion exchange membranes divide the interior of the container into a first part, a second part and a third part, and the second part has an inlet and an outlet; the chromatography baseline suppression device further comprises:

[0011] Two electrodes are respectively located in the first part and the second part, the electrode comprises a matrix porous material layer and a polymer layer, the matrix porous material layer is conductive and connected to the ion exchange membrane.

[0012] Another objective of this invention is to provide a method for manufacturing a chromatographic baseline suppression device, which is achieved through the following technical solution:

[0013] A method for manufacturing a chromatographic baseline suppression device, the method comprising an electrode manufacturing stage, wherein the electrode manufacturing stage is as follows:

[0014] The porous matrix material was ultrasonically cleaned with organic reagents and pure water, and then dried.

[0015] A rotating matrix porous material is used to uniformly drip the synthesized polymer onto the surface of the matrix porous material; at the same time, the matrix porous material is tilted to adjust the modification thickness of the polymer material on the matrix porous material, so that the modification thickness gradually decreases from one side of the matrix porous material to the other end.

[0016] An ion exchange membrane is attached to the porous matrix material.

[0017] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0018] 1. High inhibition efficiency;

[0019] The design of gradually reducing the thickness of the surface-modified polymer layer greatly improves the uniformity of the overall potential field of the suppression device, resulting in a high current density at the inlet of the eluent and a low current density at the outlet, thereby improving suppression efficiency and reducing noise.

[0020] 2. Low noise and high sensitivity;

[0021] The matrix porous material layer has a hollow porous morphology, which increases the reaction contact area and generates uniform bubbles during water electrolysis, avoiding resistance changes and baseline fluctuations caused by bubbles and improving sensitivity.

[0022] The ion exchange membrane and electrode material are tightly bonded together through polymer modification, which reduces resistance and noise caused by heat generation.

[0023] 3. Good repeatability;

[0024] The integrated synthesis process of electrode chamber materials greatly improves consistency, reduces human error in filling, and ensures good repeatability between each device and the instrument itself. Attached Figure Description

[0025] The disclosure of this invention will become more readily understood with reference to the accompanying drawings. It will be readily understood by those skilled in the art that these drawings are merely illustrative of the technical solutions of this invention and are not intended to limit the scope of protection of this invention. In the drawings:

[0026] Figure 1 This is a schematic diagram of the structure of a chromatographic baseline suppression device according to an embodiment of the present invention. Detailed Implementation

[0027] Figure 1 The following description illustrates optional embodiments of the invention to teach those skilled in the art how to implement and reproduce the invention. Some conventional aspects have been simplified or omitted to explain the technical solutions of the invention. Those skilled in the art should understand that variations or substitutions derived from these embodiments will be within the scope of the invention. Those skilled in the art should understand that the following features can be combined in various ways to form multiple variations of the invention. Therefore, the invention is not limited to the following optional embodiments, but is defined only by the claims and their equivalents.

[0028] Example 1:

[0029] Figure 1 A schematic diagram of the chromatographic baseline suppression device according to an embodiment of the present invention is provided, as follows: Figure 1 As shown, the chromatographic baseline suppression device includes:

[0030] The container and two ion exchange membranes divide the interior of the container into a first part, a second part, and a third part, the second part having an inlet and an outlet; these structures are all prior art in the art.

[0031] Two electrodes are located in the first part and the second part, respectively. Each electrode includes a porous matrix material layer and a polymer layer. The porous matrix material layer is conductive and connected to the ion exchange membrane.

[0032] To further improve sensitivity, the particle size distribution of the matrix porous material is 200nm-400nm, and the pore size distribution is 10nm-50nm.

[0033] To further improve sensitivity, the matrix porous material has a hollow porous morphology or a porous core-shell structure.

[0034] To further improve sensitivity, the porous matrix material is modified with a polymer to have ion-exchange functional groups, such as sulfonic acid groups or carboxyl groups.

[0035] To further improve the suppression efficiency, the thickness of the polymer layer gradually decreases from the inlet to the outlet.

[0036] The manufacturing method of the chromatographic baseline suppression device according to an embodiment of the present invention includes an electrode manufacturing stage, wherein the electrode manufacturing stage is as follows:

[0037] The porous matrix material was ultrasonically cleaned with organic reagents and pure water, and then dried.

[0038] A rotating matrix porous material is used to uniformly drip the synthesized polymer onto the surface of the matrix porous material; at the same time, the matrix porous material is tilted to adjust the modification thickness of the polymer material on the matrix porous material, so that the modification thickness gradually decreases from one side of the matrix porous material to the other end.

[0039] An ion exchange membrane is attached to the porous matrix material.

[0040] To improve the stability of the modification, the reaction temperature was further set at 30-40 degrees Celsius, the polymer outflow rate at 0.25-0.4 ml / min, and the height difference between the outlet and the matrix material at 5-10 cm during the titration process.

[0041] To further improve the suppression efficiency, the tilt angle is set at 45-60 degrees, and the thickness of the polymer layer formed on the porous matrix material is 5-10 mm on one side and 1-3 mm on the other side.

[0042] Example 2:

[0043] Application examples of the chromatographic baseline suppression device and its manufacturing method according to Embodiment 1 of the present invention.

[0044] In this application example, such as Figure 1 As shown, the matrix porous material is a porous carbon material with a particle size of 400 mm and a pore size of 50 nm. The matrix porous material is modified by sulfonation, and the modification thickness is a maximum of 8 mm near the eluent inlet and a minimum of 1 mm near the eluent outlet, with the thickness decreasing in a gradient. From the inlet to the outlet, the distance between the two ion exchange membranes first increases and then decreases.

[0045] The ion exchange membrane was a sulfonated cation exchange membrane, and the resin was a sulfonated cation exchange resin. The flow rate was set to 0.25 mL / min, the eluent concentration was 20 mM potassium hydroxide, the current was constant with a current efficiency of 95%, and the sample was separated by a chromatographic column. The sample was desalted in the baseline device of this protocol and finally analyzed by a conductivity detector. The sample baseline was 3 μS / cm, and multiple inorganic anion analysis results were obtained within 10 minutes. The remaining waste liquid was discharged into the waste liquid channel after passing through the regeneration liquid channel.

[0046] The manufacturing method of the chromatographic baseline suppression device according to an embodiment of the present invention includes an electrode manufacturing stage, wherein the electrode manufacturing stage is as follows:

[0047] The porous matrix material was ultrasonically cleaned with organic reagents and pure water, and then dried.

[0048] A rotating porous matrix material is used to uniformly drip the synthesized polymer onto its surface. The reaction temperature is 30 degrees Celsius, the polymer outflow rate is 0.25 ml / min, and the height difference between the outlet and the matrix material is 5 cm. Simultaneously, the porous matrix material is tilted at an angle of 45 degrees to adjust the modification thickness of the polymer material on the porous matrix material. This results in a modification thickness that gradually decreases from one side of the porous matrix material to the other, forming a polymer layer with a thickness of 5 mm on one side and 1 mm on the other.

[0049] An ion exchange membrane is attached to the porous matrix material.

[0050] Example 3:

[0051] An application example of the chromatographic baseline suppression device according to Embodiment 1 of the present invention differs from that in Embodiment 2 in that:

[0052] In the manufacturing method, the titration temperature is 40 degrees, the polymer outflow rate is 0.4 ml / min, the height difference between the outlet and the matrix material is 10 cm, the tilt angle is 60 degrees, and the thickness of the polymer layer formed is 10 mm on one side and 3 mm on the other side.

[0053] Example 4:

[0054] An application example of the chromatographic baseline suppression device according to Embodiment 1 of the present invention differs from that in Embodiment 2 in that:

[0055] In the manufacturing method, the titration temperature is 36 degrees, the polymer outflow rate is 0.32 ml / min, the height difference between the outlet and the matrix material is 7 cm, the tilt angle is 51 degrees, and the thickness of the polymer layer formed is 8 mm on one side and 2 mm on the other side.

Claims

1. A chromatographic baseline suppression device, comprising a container and two ion exchange membranes, the two ion exchange membranes dividing the interior of the container into a first part, a second part, and a third part, the second part having an inlet and an outlet; characterized in that, The chromatographic baseline suppression device further includes: Two electrodes are located in the first part and the second part respectively. Each electrode includes a porous matrix material layer and a polymer layer. The porous matrix material layer is conductive and connected to the ion exchange membrane. A polymer is modified on a porous matrix material, and the polymer is modified with ion-exchange functional groups; the thickness of the polymer layer gradually decreases from the inlet to the outlet.

2. The chromatographic baseline suppression device according to claim 1, characterized in that, The particle size distribution of the matrix porous material is 200nm-400nm, and the pore size distribution is 10nm-50nm.

3. The chromatographic baseline suppression device according to claim 2, characterized in that, The matrix porous material has a hollow porous morphology or a porous core-shell structure.

4. The chromatographic baseline suppression device according to claim 1, characterized in that, The functional group is a sulfonic acid group or a carboxyl group.

5. The chromatographic baseline suppression device according to claim 1, characterized in that, From the inlet to the outlet, the distance between the two ion exchange membranes first increases and then decreases.

6. A method for manufacturing a chromatographic baseline suppression device, the method comprising an electrode manufacturing stage, characterized in that, The manufacturing stages of the electrode are as follows: The porous matrix material was ultrasonically cleaned with organic reagents and pure water, and then dried. A rotating matrix porous material is used to uniformly drip the synthesized polymer onto the surface of the matrix porous material; at the same time, the matrix porous material is tilted to adjust the modification thickness of the polymer material on the matrix porous material, so that the modification thickness gradually decreases from one side of the matrix porous material to the other end. An ion exchange membrane is attached to the porous matrix material.

7. The method for manufacturing the chromatographic baseline suppression device according to claim 6, characterized in that, During the titration process, the reaction temperature is 30-40℃, the polymer outflow rate is 0.25-0.4 ml / min, and the height difference between the outlet and the matrix material is 5-10 cm.

8. The method for manufacturing the chromatographic baseline suppression device according to claim 6, characterized in that, The tilt angle is 45-60 degrees, and the thickness of the polymer layer formed on the porous matrix material is 5-10 mm on one side and 1-3 mm on the other side.

Images