A device for separating and enriching organomercury phenyl derivatives

Abstract

This invention belongs to the field of analytical detection and relates to a device for the separation and enrichment of organomercury phenyl derivatives, comprising: a liquid phase tube 7 and a gas phase tube 8; the gas phase tube 8 is fixed inside the liquid phase tube 7; the liquid phase tube 7 and the gas phase tube 8 are respectively provided with independent inlets and outlets; one end of the gas outlet 3 of the gas phase tube 8 is connected to an adsorption tube 9, and the end of the adsorption tube 9 away from the gas phase tube 8 is connected to a vacuum filtration pump 10. Utilizing the selective permeability of a membrane, a highly efficient device for separating and enriching organomercury phenyl derivatives is designed through a pervaporation method. This device can directly separate organomercury phenyl derivatives from liquid samples, improving separation efficiency, reducing gas consumption during the separation process, and simplifying the separation operation steps compared to traditional separation methods. Furthermore, the device of this invention is more compact, saving experimental space.

Description

Technical Field

[0001] This invention belongs to the field of analytical detection, and specifically relates to a device for the separation and enrichment of organomercury phenyl derivatives. Background Technology

[0002] The information disclosed in this background section is intended only to enhance understanding of the overall background of the invention and is not necessarily to be construed as an admission or in any way implying that such information constitutes prior art known to those skilled in the art.

[0003] The most common current method for detecting organic mercury is ethylation derivatization-purge-trap-gas chromatography-cold atomic fluorescence spectrometry (CAVFS), which is also the most widely used standard method for MeHg detection worldwide. The main advantage of this derivatization method is that the reaction is carried out in aqueous solution, allowing it to be combined with purge-trap pre-concentration systems and sensitive detectors like AFS or ICP-MS, thus achieving a low detection limit. However, ethylation cannot distinguish between inorganic mercury and EtHg, which limits its application in environments where EtHg and Hg²⁺ coexist. Furthermore, the ethylation derivatization reagent is sodium tetraethylborate, which is unstable in aqueous solution and needs to be freshly prepared and treated under a protective gas atmosphere. Additionally, the ethylation process is significantly affected by the sample matrix. Chloride ions and dissolved organic matter (DOM) greatly reduce the sensitivity and reproducibility of this method.

[0004] The phenylation process is unaffected by chloride ions and DOM matrix interference, allowing direct analysis of environmental water samples without extraction or distillation. However, compared to ethylation, the products of phenylation are less volatile, making complete separation and enrichment from solution difficult. Current methods utilize purge-and-trap for product separation, involving heating the aqueous phase and adding a high-concentration salt solution to leverage the salting-out effect and improve purge-and-trap efficiency. This process is time-consuming, complex, and difficult to automate. Summary of the Invention

[0005] To address the aforementioned issues, this invention utilizes the selective permeability of membranes and employs a pervaporation method to design a highly efficient device for separating and enriching organomercury phenyl derivatives. This device can directly separate organomercury phenyl derivatives from liquid samples, improving separation efficiency, reducing gas consumption, and simplifying separation procedures compared to traditional methods. Furthermore, the device is more compact, saving experimental space.

[0006] To achieve the above technical objectives, the present invention adopts the following technical solution:

[0007] In a first aspect, the present invention provides a separation and enrichment apparatus for organomercury phenyl derivatives, comprising: a liquid phase tube 7 and a gas phase tube 8; the gas phase tube 8 is fixed inside the liquid phase tube 7; the liquid phase tube 7 and the gas phase tube 8 are respectively provided with independent inlets and outlets; one end of the gas outlet 3 of the gas phase tube 8 is connected to an adsorption tube 9, and the end of the adsorption tube 9 away from the gas phase tube 8 is connected to a vacuum filtration pump 10.

[0008] A second aspect of the present invention provides a method for the separation and enrichment of organomercury phenyl derivatives, using the above-described apparatus for separation and enrichment, comprising:

[0009] The sample liquid is injected from the liquid phase tube 7, and the organomercury phenyl derivative permeates and vaporizes from the liquid phase tube 7 into the gas phase tube 8.

[0010] The organomercury phenyl derivative enters the adsorption tube 9 along with the carrier gas and is adsorbed on the Tenax packing material to obtain the product.

[0011] The beneficial effects of this invention are as follows:

[0012] (1) Compared with the traditional purge-collection separation method, the present invention improves separation efficiency, reduces gas consumption during the separation process, simplifies separation operation steps, shortens separation time, and achieves automated separation. Moreover, the device of the present invention is more compact and saves experimental space.

[0013] (2) The device of the present invention has a simple structure, is easy to operate, is highly practical, and is easy to promote. Attached Figure Description

[0014] The accompanying drawings, which form part of this invention, are used to provide a further understanding of the invention. The illustrative embodiments of the invention and their descriptions are used to explain the invention and do not constitute an improper limitation of the invention.

[0015] Figure 1 This is a schematic diagram of the device structure according to Embodiment 1 of the present invention;

[0016] Figure 2 This is a partial schematic diagram of the device structure according to Embodiment 1 of the present invention;

[0017] Among them, 1. fixed back plate, 2. air inlet, 3. air outlet, 4. liquid phase outlet, 5. liquid phase inlet, 6. rubber sealing ring, 7. liquid phase pipe, and 8. gas phase pipe. Detailed Implementation

[0018] It should be noted that the following detailed descriptions are exemplary and intended to provide further illustration of the invention. Unless otherwise specified, all technical and scientific terms used in this invention have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains.

[0019] A device for separating and enriching organomercury phenyl derivatives includes: a liquid phase tube 7 and a gas phase tube 8; the gas phase tube 8 is fixed inside the liquid phase tube 7; the liquid phase tube 7 and the gas phase tube 8 are respectively provided with independent inlets and outlets; one end of the gas outlet 3 of the gas phase tube 8 is connected to an adsorption tube 9, and the end of the adsorption tube 9 away from the gas phase tube 8 is connected to a vacuum filtration pump 10.

[0020] In some embodiments, the gas phase pipe 8 is provided with an outlet 3 and an inlet 2 at both ends.

[0021] In some embodiments, the liquid phase tube 7 is provided with a liquid phase inlet 5 and a liquid phase outlet 4 at both ends.

[0022] In some embodiments, the adsorption tube is a quartz tube filled with Tenax packing material.

[0023] In some embodiments, the inner diameter of the adsorption tube is 0.38 mm and the Tenax packing material is 0.1 g. The tube diameter and packing amount can be adjusted according to specific test requirements.

[0024] In some embodiments, a rubber sealing ring 6 is provided inside the liquid phase tube 7, and the gas phase tube 8 passes through the rubber sealing ring 6.

[0025] In some embodiments, the liquid phase tube 7 is a Teflon FEP tube.

[0026] In some embodiments, the gas phase tube 8 is a PDMS membrane pipeline. In some embodiments, the inner diameter of the gas phase tube is approximately 0.2 mm, and the tube diameter can be adjusted according to specific test requirements.

[0027] In some embodiments, the liquid phase tube 7 and the adsorption tube 9 are fixed on the fixed back plate 1.

[0028] A method for separating and enriching organomercury phenyl derivatives, using the above-mentioned apparatus, includes:

[0029] The sample liquid is injected from the liquid phase tube 7, and the organomercury phenyl derivative permeates and vaporizes from the liquid phase tube 7 into the gas phase tube 8.

[0030] The organomercury phenyl derivative enters the adsorption tube 9 along with the carrier gas and is adsorbed on the Tenax packing material to obtain the product.

[0031] In some embodiments, the liquid phase flows in the opposite direction to the gas phase.

[0032] The present invention will be further described in detail below with reference to specific embodiments. It should be noted that the specific embodiments are explanations of the present invention and not limitations thereof.

[0033] Example 1

[0034] This embodiment includes three parts: a fixed back plate 1, a gas phase tube 8, and a liquid phase tube 7. The gas phase tube 8 is located inside the liquid phase tube 7. The two parts are relatively independent, sealed, and do not communicate with each other.

[0035] In the gas phase piping section, Figure 1 , Figure 2 2 is the air inlet, 3 is the air outlet, and 9 is connected after the air outlet to a quartz adsorption tube filled with Tenax packing material, which is used to adsorb organomercury phenyl derivatives separated from the solution.

[0036] In the liquid phase pipeline section Figure 1 , Figure 2 In the diagram, 5 is the liquid phase inlet and 4 is the liquid phase outlet, with the liquid phase flowing in the opposite direction to the gas phase. This counter-current flow ensures sufficient contact between the sample solution and the membrane, guaranteeing effective separation.

[0037] Figure 1 , Figure 2 The middle 6 is a rubber sealing ring, which ensures that the gas phase pipeline and the liquid phase pipeline are independently sealed, ensuring that the liquid phase cannot enter the gas phase pipeline.

[0038] Figure 1 , Figure 2 7 is the liquid phase tube, which uses Teflon FEP tubing.

[0039] Figure 1 , Figure 2 The middle 8 is the gas phase tube, which uses a PDMS membrane tube.

[0040] Figure 1 , Figure 2 The middle 10 is a vacuum filtration pump.

[0041] Apart from this, all other piping in the device uses Teflon FEP tubing with an outer diameter of 1 / 8 inch and an inner diameter of 1 / 16 inch.

[0042] When using, open Figure 1 , Figure 2 The 10 vacuum filtration pump in the device draws gas from... Figure 1 , Figure 2 Middle 2 Figure 1 , Figure 2 The sample liquid moves in three directions from the center. Figure 1 , Figure 2 Middle 5 Figure 1 , Figure 2 In the middle 4th step, during sample passage, the selective permeability of the membrane allows the organomercury phenyl derivative to be pervaporated from the liquid phase and introduced into the gas phase pipeline, thus completing the separation of the target organic compound. The organomercury phenyl derivative enters with the carrier gas. Figure 1 , Figure 2In the 9 adsorption tubes, the material is adsorbed onto the Tenax packing material to achieve enrichment.

[0043] Example 2

[0044] A device for separating and enriching organomercury phenyl derivatives includes: a liquid phase tube 7 and a gas phase tube 8; the gas phase tube 8 is fixed inside the liquid phase tube 7; the liquid phase tube 7 and the gas phase tube 8 are respectively provided with independent inlets and outlets; one end of the gas outlet 3 of the gas phase tube 8 is connected to an adsorption tube 9, and the end of the adsorption tube 9 away from the gas phase tube 8 is connected to a vacuum filtration pump 10.

[0045] Example 3

[0046] A device for separating and enriching organomercury phenyl derivatives includes: a liquid phase tube 7 and a gas phase tube 8; the gas phase tube 8 is fixed inside the liquid phase tube 7; the liquid phase tube 7 and the gas phase tube 8 are respectively provided with independent inlets and outlets; one end of the gas outlet 3 of the gas phase tube 8 is connected to an adsorption tube 9, and the end of the adsorption tube 9 away from the gas phase tube 8 is connected to a vacuum filtration pump 10.

[0047] In some embodiments, the gas phase pipe 8 is provided with an outlet 3 and an inlet 2 at both ends.

[0048] Example 4

[0049] A device for separating and enriching organomercury phenyl derivatives includes: a liquid phase tube 7 and a gas phase tube 8; the gas phase tube 8 is fixed inside the liquid phase tube 7; the liquid phase tube 7 and the gas phase tube 8 are respectively provided with independent inlets and outlets; one end of the gas outlet 3 of the gas phase tube 8 is connected to an adsorption tube 9, and the end of the adsorption tube 9 away from the gas phase tube 8 is connected to a vacuum filtration pump 10.

[0050] The liquid phase tube 7 is provided with a liquid phase inlet 5 and a liquid phase outlet 4 at both ends.

[0051] Example 5

[0052] A device for separating and enriching organomercury phenyl derivatives includes: a liquid phase tube 7 and a gas phase tube 8; the gas phase tube 8 is fixed inside the liquid phase tube 7; the liquid phase tube 7 and the gas phase tube 8 are respectively provided with independent inlets and outlets; one end of the gas outlet 3 of the gas phase tube 8 is connected to an adsorption tube 9, and the end of the adsorption tube 9 away from the gas phase tube 8 is connected to a vacuum filtration pump 10.

[0053] The adsorption tube is a quartz tube filled with Tenax packing material.

[0054] Example 6

[0055] A device for separating and enriching organomercury phenyl derivatives includes: a liquid phase tube 7 and a gas phase tube 8; the gas phase tube 8 is fixed inside the liquid phase tube 7; the liquid phase tube 7 and the gas phase tube 8 are respectively provided with independent inlets and outlets; one end of the gas outlet 3 of the gas phase tube 8 is connected to an adsorption tube 9, and the end of the adsorption tube 9 away from the gas phase tube 8 is connected to a vacuum filtration pump 10.

[0056] The liquid phase tube 7 is provided with a rubber sealing ring 6 inside, and the gas phase tube 8 passes through the rubber sealing ring 6.

[0057] Example 7

[0058] A device for separating and enriching organomercury phenyl derivatives includes: a liquid phase tube 7 and a gas phase tube 8; the gas phase tube 8 is fixed inside the liquid phase tube 7; the liquid phase tube 7 and the gas phase tube 8 are respectively provided with independent inlets and outlets; one end of the gas outlet 3 of the gas phase tube 8 is connected to an adsorption tube 9, and the end of the adsorption tube 9 away from the gas phase tube 8 is connected to a vacuum filtration pump 10.

[0059] The liquid phase tube 7 is a Teflon FEP tube.

[0060] Example 8

[0061] A device for separating and enriching organomercury phenyl derivatives includes: a liquid phase tube 7 and a gas phase tube 8; the gas phase tube 8 is fixed inside the liquid phase tube 7; the liquid phase tube 7 and the gas phase tube 8 are respectively provided with independent inlets and outlets; one end of the gas outlet 3 of the gas phase tube 8 is connected to an adsorption tube 9, and the end of the adsorption tube 9 away from the gas phase tube 8 is connected to a vacuum filtration pump 10.

[0062] The gas phase tube 8 is a PDMS membrane pipeline.

[0063] Example 9

[0064] A device for separating and enriching organomercury phenyl derivatives includes: a liquid phase tube 7 and a gas phase tube 8; the gas phase tube 8 is fixed inside the liquid phase tube 7; the liquid phase tube 7 and the gas phase tube 8 are respectively provided with independent inlets and outlets; one end of the gas outlet 3 of the gas phase tube 8 is connected to an adsorption tube 9, and the end of the adsorption tube 9 away from the gas phase tube 8 is connected to a vacuum filtration pump 10.

[0065] The liquid phase tube 7 and the adsorption tube 9 are fixed on the fixed back plate 1.

[0066] Example 10

[0067] A device for separating and enriching organomercury phenyl derivatives includes: a liquid phase tube 7 and a gas phase tube 8; the gas phase tube 8 is fixed inside the liquid phase tube 7; the liquid phase tube 7 and the gas phase tube 8 are respectively provided with independent inlets and outlets; one end of the gas outlet 3 of the gas phase tube 8 is connected to an adsorption tube 9, and the end of the adsorption tube 9 away from the gas phase tube 8 is connected to a vacuum filtration pump 10.

[0068] A method for separating and enriching organomercury phenyl derivatives, using the above-mentioned apparatus, includes:

[0069] The sample liquid is injected from the liquid phase tube 7, and the organomercury phenyl derivative permeates and vaporizes from the liquid phase tube 7 into the gas phase tube 8.

[0070] The organomercury phenyl derivative enters the adsorption tube 9 along with the carrier gas and is adsorbed on the Tenax packing material to obtain the product.

[0071] In this case, the liquid phase flows in the opposite direction to the gas phase.

[0072] While the specific embodiments of the present invention have been described above, they are not intended to limit the scope of protection of the present invention. Those skilled in the art should understand that various modifications or variations that can be made by those skilled in the art without creative effort based on the technical solutions of the present invention are still within the scope of protection of the present invention.

Claims

1. A device for separating and enriching organomercury phenyl derivatives, characterized in that, include: Liquid phase tube (7), gas phase tube (8); gas phase tube (8) is fixed inside the liquid phase tube (7); the liquid phase tube (7) and gas phase tube (8) are respectively provided with independent inlets and outlets; one end of the gas outlet (3) of the gas phase tube (8) is connected to the adsorption tube (9), and the end of the adsorption tube (9) away from the gas phase tube (8) is connected to the vacuum filtration pump (10); The liquid phase pipe (7) is provided with a rubber sealing ring (6), and the gas phase pipe (8) passes through the rubber sealing ring (6); the gas phase pipe (8) is located inside the liquid phase pipe (7), and the two parts are relatively independent, sealed and not interconnected; The liquid phase flows in the opposite direction to the gas phase; The method for separation and enrichment using the aforementioned apparatus includes: The sample liquid is injected from the liquid phase tube (7), and the organomercury phenyl derivative permeates and vaporizes from the liquid phase tube (7) into the gas phase tube (8). The organomercury phenyl derivative enters the adsorption tube (9) along with the carrier gas and is adsorbed on the Tenax packing material to obtain the product. The gas phase tube (8) is a PDMS membrane tube; The organomercury phenyl derivatives are poorly volatile and difficult to separate from solution.

2. The apparatus for separating and enriching organomercury phenyl derivatives as described in claim 1, characterized in that, The gas phase pipe (8) is provided with an outlet (3) and an inlet (2) at both ends.

3. The apparatus for separating and enriching organomercury phenyl derivatives as described in claim 1, characterized in that, The liquid phase tube (7) is provided with a liquid phase inlet (5) and a liquid phase outlet (4) at both ends.

4. The apparatus for separating and enriching organomercury phenyl derivatives as described in claim 1, characterized in that, The adsorption tube (9) is a quartz tube filled with Tenax packing material.

5. The apparatus for separating and enriching organomercury phenyl derivatives as described in claim 1, characterized in that, The liquid phase pipe (7) is a Teflon FEP pipe.

6. The apparatus for separating and enriching organomercury phenyl derivatives as described in claim 1, characterized in that, The liquid phase tube (7) and adsorption tube (9) are fixed on the fixed back plate (1).

7. A method for the separation and enrichment of organomercury phenyl derivatives, characterized in that, Separation and enrichment using the apparatus according to any one of claims 1-6, comprising: The sample liquid is injected from the liquid phase tube (7), and the organomercury phenyl derivative permeates and vaporizes from the liquid phase tube (7) into the gas phase tube (8). The organomercury phenyl derivative enters the adsorption tube (9) along with the carrier gas and is adsorbed on the Tenax packing material to obtain the product.

8. The method as described in claim 7, characterized in that, The liquid phase flows in the opposite direction to the gas phase.

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