A rapid enrichment device for stirred silicone rubber composite membranes

Abstract

This utility model relates to the field of environmental analysis and testing technology. Addressing the problems of low efficiency, complex operation, and unsuitability for on-site testing in existing membrane enrichment devices, it provides a rapid enrichment device using a stirred silicone rubber composite membrane. This enrichment device consists of a silicone rubber sheet, a separating mesh, a fixing head, and a connecting rod. The silicone rubber sheet and the separating mesh are clamped together by the fixing head to form a composite membrane. Connected to an electric drill via the connecting rod, it can rapidly adsorb organic matter in water samples through rotational stirring. After enrichment, it is placed in a thermal desorption container, and the desorbed gas is detected by ion mobility spectrometry via a carrier gas. By enhancing mass transfer through stirring and expanding the adsorption area of ​​the composite membrane, enrichment can be completed within 30 minutes. It is suitable for on-site and laboratory detection of organic matter in water and air samples, significantly improving efficiency and portability.

Description

Technical Field

[0001] This utility model relates to the field of environmental analysis and testing technology, and more specifically, to a rapid enrichment device for a stirred silicone rubber composite membrane. Background Technology

[0002] Extracting and analyzing organic matter from water samples is a key step in water quality monitoring and pollution control, and an important technical means to achieve sustainable use of water resources.

[0003] In the field of organic matter detection in aquatic environments, efficient extraction technology is a core prerequisite for accurate analysis. Currently, mainstream extraction technologies include liquid-liquid extraction, solid-phase extraction, solid-phase microextraction, and membrane enrichment extraction. Among them, membrane enrichment extraction technology, with its unique separation mechanism, shows significant advantages in the extraction of volatile and semi-volatile organic compounds.

[0004] Specifically, static membrane extraction technology achieves mass transfer by keeping the water sample and the extract phase in static contact on both sides of the membrane. It is simple to operate and has few interfering factors, making it particularly suitable for the extraction of volatile organic compounds. Dynamic membrane extraction technology, on the other hand, significantly improves the mass transfer efficiency of organic matter on both sides of the membrane by integrating dynamic enhancement methods such as peristaltic pump circulation and stirring. Therefore, it is more suitable for processing water samples with complex composition and strong matrix interference.

[0005] Existing patent document with application number 201010253173.6 discloses a β-cyclodextrin-based solid-phase microextraction coating and extraction head. This extraction head consists of quartz fiber and a solid-phase microextraction coating on its surface. The solid-phase microextraction coating includes β-cyclodextrin and polydimethylsiloxane bonded together. Utilizing its unique cavity structure (hydrophobic inside, hydrophilic outside), it increases the adsorption capacity for polar substances. Combined with the non-polar characteristics of polydimethylsiloxane, this expands the coating's selectivity range for the polarity of adsorbed substances. It involves bonding an extraction head containing β-cyclodextrin and silicone rubber to a metal wire to broaden the coating's selectivity range for the polarity of adsorbed substances. However, this method is inconvenient to operate and not suitable for the rapid extraction of organic matter from water / air samples. Utility Model Content

[0006] In response to the aforementioned technical problems, a rapid enrichment device for a stirred silicone rubber composite membrane is provided. The composite membrane is rotated by an electric drill, which can rapidly enrich and extract organic matter from water samples.

[0007] The technical means adopted in this utility model are as follows:

[0008] A rapid enrichment device for a stirred silicone rubber composite membrane includes a connecting rod, a fixing head, a separating mesh, and a silicone rubber sheet. The separating mesh is connected to the silicone rubber sheet and clamped inside the fixing head. The fixing head is connected to the connecting rod, and the connecting rod can be connected to the output end of an electric drill in its first working state.

[0009] Furthermore, in the second working state, the rapid enrichment device is placed inside the thermal desorption container, which includes an open cavity, a top cover, a heating element, an inlet pipe, and an outlet pipe. The cavity and the top cover are connected by threads. The inlet pipe and the outlet pipe are used to connect the carrier gas circuit of the ion migration tube in series. The heating element is used to heat and volatilize the organic matter enriched by the silicone rubber sheet in the first working state.

[0010] Furthermore, the number of silicone rubber sheets is 1 to 20.

[0011] Furthermore, the thickness of the silicone rubber sheet is 0.1~1mm, and the length is 3~30cm.

[0012] Furthermore, the arrangement of the silicone rubber sheet and the isolation net is selected from: parallel arrangement at intervals, free arrangement without parallelism, spiral roll of 1 silicone rubber sheet and 1 isolation net, or spiral roll of n silicone rubber sheets and n-1 isolation nets, where n≥2.

[0013] Furthermore, the isolation net is made of stainless steel or polytetrafluoroethylene.

[0014] Furthermore, the mesh size of the isolation net is 0.1~1mm, and the thickness is 0.05~0.2mm.

[0015] Furthermore, the fixing head has a slot inside, the depth of which is adapted to the total thickness of each silicone rubber sheet and the isolation mesh, for clamping and fixing the composite film.

[0016] Furthermore, the fixing head and the connecting rod are connected by a snap-fit. The snap-fit ​​connection includes a boss on the fixing head and a groove on the connecting rod. The boss and the groove are interference-fitted, and the outer wall of the boss is provided with anti-slip texture.

[0017] Compared with the prior art, the present invention has the following advantages:

[0018] 1. The present invention uses an electric drill to drive the composite membrane to rotate, which causes the sample to form turbulence around the membrane, breaks the concentration boundary layer in static extraction, effectively increases the diffusion rate of organic matter into the membrane, and improves the enrichment efficiency.

[0019] 2.1~20 silicone rubber sheets are arranged alternately with the isolation mesh, which effectively expands the adsorption area compared to a single membrane. The isolation mesh is used to prevent the membranes from sticking together and ensure that each sheet effectively contacts the sample.

[0020] 3. The device is lightweight and compact, making it easy to carry to the field. It also features a switchable stirring / static mode to accommodate samples of different concentrations. It can enrich organic matter in water samples and also enrich gaseous samples by exposing them to air. Attached Figure Description

[0021] To more clearly illustrate the technical solutions in the embodiments of this utility model or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of this utility model. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0022] Figure 1 This is a schematic diagram of a silicone rubber composite membrane enrichment device.

[0023] Figure 2 This is a schematic diagram of a silicone rubber composite membrane enrichment device used for enrichment and extraction in a water sample.

[0024] Figure 3 This is a schematic diagram of the present invention placed in a thermal desorption heating container.

[0025] In the figure: 1. Silicone rubber sheet; 2. Isolation net; 3. Fixing head; 4. Connecting rod; 5. Water sample; 6. Silicone rubber composite membrane enrichment device; 7. Thermal desorption container; 8. Gas outlet pipe; 9. Gas inlet pipe. Detailed Implementation

[0026] It should be noted that, where there is no conflict, the embodiments and features in the embodiments of this utility model can be combined with each other. The present utility model will now be described in detail with reference to the accompanying drawings and embodiments.

[0027] To make the objectives, technical solutions, and advantages of the embodiments of this utility model clearer, the technical solutions of the embodiments of this utility model will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this utility model, and not all embodiments. The following description of at least one exemplary embodiment is merely illustrative and is in no way intended to limit this utility model or its application or use. Based on the embodiments of this utility model, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this utility model.

[0028] It should be noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the exemplary embodiments according to the present invention. As used herein, the singular form is intended to include the plural form as well, unless the context clearly indicates otherwise. Furthermore, it should be understood that when the terms "comprising" and / or "including" are used in this specification, they indicate the presence of features, steps, operations, devices, components, and / or combinations thereof.

[0029] Unless otherwise specifically stated, the relative arrangement, numerical expressions, and values ​​of the components and steps described in these embodiments do not limit the scope of this invention. It should also be understood that, for ease of description, the dimensions of the various parts shown in the drawings are not drawn to actual scale. Techniques, methods, and devices known to those skilled in the art may not be discussed in detail, but where appropriate, such techniques, methods, and devices should be considered part of the specification. In all examples shown and discussed herein, any specific values ​​should be interpreted as merely exemplary and not as limitations. Therefore, other examples of exemplary embodiments may have different values. It should be noted that similar reference numerals and letters in the following figures denote similar items; therefore, once an item is defined in one figure, it need not be further discussed in subsequent figures.

[0030] In the description of this utility model, it should be understood that the orientation or positional relationship indicated by directional terms such as "front, back, up, down, left, right", "horizontal, vertical, horizontal" and "top, bottom" is usually based on the orientation or positional relationship shown in the accompanying drawings, and is only for the convenience of describing this utility model and simplifying the description. Unless otherwise stated, these directional terms do not indicate or imply that the device or element referred to must have a specific orientation or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation on the scope of protection of this utility model. The directional terms "inner" and "outer" refer to the inner and outer contours relative to the outline of each component itself.

[0031] For ease of description, spatial relative terms such as "above," "over," "on the upper surface of," "above," etc., are used herein to describe the spatial positional relationship of a device or feature as shown in the figures to other devices or features. It should be understood that spatial relative terms are intended to encompass different orientations in use or operation besides the orientation of the device as described in the figures. For example, if the device in the figures is inverted, a device described as "above" or "above" other devices or structures would subsequently be positioned as "below" or "under" other devices or structures. Thus, the exemplary term "above" can include both "above" and "below." The device may also be positioned in other different ways (rotated 90 degrees or in other orientations), and the spatial relative descriptions used herein will be interpreted accordingly.

[0032] Furthermore, it should be noted that the use of terms such as "first" and "second" to define components is merely for the purpose of distinguishing the corresponding components. Unless otherwise stated, the above terms have no special meaning and therefore cannot be construed as limiting the scope of protection of this utility model.

[0033] like Figure 1 , Figure 2 As shown in the figure, this utility model embodiment discloses a rapid enrichment device 6 for a stirred silicone rubber composite membrane, including a connecting rod 4, a fixing head 3, an isolation net 2 and a silicone rubber sheet 1. The isolation net is connected to the silicone rubber sheet and then clamped in the fixing head. The fixing head is connected to the connecting rod, and the connecting rod can be connected to the output end of an electric drill in the first working state.

[0034] Furthermore, such as Figure 3 As shown, in the second working state, the rapid enrichment device is placed inside the thermal desorption container. The thermal desorption container includes an open cavity, a top cover, a heating element, an inlet pipe 9, and an outlet pipe 8. The cavity and the top cover are connected by threads. The inlet pipe and the outlet pipe are used to connect the carrier gas circuit of the ion migration tube in series. The heating element is used to heat and volatilize the organic matter enriched by the silicone rubber sheet in the first working state.

[0035] Furthermore, the number of silicone rubber sheets is 1 to 20.

[0036] Furthermore, the thickness of the silicone rubber sheet is 0.1~1mm, and the length is 3~30cm.

[0037] In this embodiment, the silicone rubber sheet is made of methyl vinyl silicone rubber.

[0038] Furthermore, the arrangement of the silicone rubber sheet and the isolation net is selected from: parallel arrangement at intervals, free arrangement without parallelism, spiral roll of 1 silicone rubber sheet and 1 isolation net, or spiral roll of n silicone rubber sheets and n-1 isolation nets, where n≥2.

[0039] Furthermore, the isolation net is made of stainless steel or polytetrafluoroethylene.

[0040] Furthermore, the mesh size of the isolation net is 0.1~1mm, and the thickness is 0.05~0.2mm.

[0041] Furthermore, the fixing head has a slot inside, the depth of which is adapted to the total thickness of each silicone rubber sheet and the isolation mesh, for clamping and fixing the composite film.

[0042] Furthermore, the fixing head and the connecting rod are connected by a snap-fit. The snap-fit ​​connection includes a boss on the fixing head and a groove on the connecting rod. The boss and the groove are interference-fitted, and the outer wall of the boss is provided with anti-slip texture.

[0043] During the enrichment stage, the silicone rubber sheet and the isolation net are stacked in a preset manner, placed into the fixed head slot, and the bolts are tightened to fix them; the fixed head is connected to the connecting rod with a snap-fit, and the connecting rod is installed on the electric drill.

[0044] The silicone rubber membrane is immersed in the water sample. The electric drill is started, which drives the membrane enrichment device to rotate and stir in the water sample, quickly adsorbing and enriching organic matter. Under specific working conditions, the silicone rubber composite membrane enrichment device rotates and stirs in the water sample at a speed of 100~3000 rpm, in a clockwise or counterclockwise manner.

[0045] Alternatively, a silicone rubber composite membrane enrichment device can be used to enrich organic matter in a water sample by allowing it to stand for 0.1 to 48 hours.

[0046] At this point, the organic matter is adsorbed by the silicone rubber.

[0047] Remove the silicone rubber composite membrane enricher, loosen the connecting rod, and place the membrane enricher into the thermal desorption container to begin thermal desorption. The inlet and outlet pipes are connected in series with the carrier gas of the ion migration tube. The organic gas from thermal desorption enters the ion migration tube for analysis and detection.

[0048] Specifically, the fixing head and connecting rod are disassembled, and the composite membrane is placed into the thermal desorption container cavity; or the entire membrane is placed in the thermal desorption container cavity, the top cover is tightened, the inlet pipe is connected to the carrier gas source, and the outlet pipe is connected to the ion mobility spectrometer; the heating temperature is set, the temperature control sensor maintains the temperature stability, and the desorbed organic matter enters the detection equipment for analysis along with the carrier gas.

[0049] This novel silicone rubber composite membrane enricher can enrich and extract organic samples from water samples, as well as from air and mixed gases.

[0050] Prepare 250 ml of a 1 ppm tetrachloroethylene solution using purified water as the test sample;

[0051] Method for enriching and extracting organic matter from water samples: The rapid enrichment device of silicone rubber composite membrane was pretreated in an oven at 100°C for 1 hour, then immersed in 250 ml of 1 ppm tetrachloroethylene aqueous solution and left at room temperature for 30 minutes. The rapid enrichment device of silicone rubber composite membrane was then removed and placed in a thermal desorption heating container to start heating and maintain at 100±20°C. At the same time, it was connected to the carrier gas of ion mobility spectrometry for analysis, and the corresponding analytical spectra and results were obtained.

[0052] The analytical conditions for ion mobility spectrometry (IMS) were as follows: positive ion mode was used during IMS operation; the ion migration tube temperature was 150℃; the inner diameter of the migration zone of the ion migration tube was 20 mm and the length was 7 cm; the inter-ring voltage was 330 V; the TP-type ion gate voltage was 340 V; the gate opening time was 50 μs; the duration of each analytical cycle was 10 ms; the average number of spectra was 10; the drift gas flow rate was 0.5 L / min; and the carrier gas flow rate was 0.2 L / min. The drift gas entered from the Faraday disk end of the migration tube, and the carrier gas entered from the reaction zone. In the reaction zone, the drift gas and the carrier gas flowed in the same direction. The outlet was located in the reaction zone near the radio frequency lamp.

[0053] Example 1

[0054] In this embodiment, there is one silicone rubber sheet, with a thickness of 1 mm and a length of 3 cm; the silicone rubber sheet and the isolation net are arranged in a spiral roll, with one silicone rubber sheet and one isolation net forming 6 turns.

[0055] Following the method of enriching and extracting organic matter from water samples, the silicone rubber composite membrane was enriched in the water sample by rotating and stirring at 100 rpm for 6 minutes in a clockwise direction.

[0056] Then, the silicone rubber composite membrane was used to enrich organic matter in the water sample and allowed to stand for 0.1 hours.

[0057] Repeat the above steps of rotary stirring and static enrichment 10 times;

[0058] The above-mentioned silicone rubber composite film was enriched and extracted, and then subjected to thermal desorption and ion mobility spectrometry analysis. The results showed that the characteristic peak mobility constant of tetrachloroethylene was 1.83±0.03 and the maximum peak height was 0.8V.

[0059] Example 2

[0060] In this embodiment, the number of silicone rubber sheets is 20, with a thickness of 0.1 mm and a length of 30 cm;

[0061] The silicone rubber sheets and the isolation mesh are arranged in a parallel, spaced-out pattern.

[0062] Following the method of enriching and extracting organic matter from water samples, the silicone rubber composite membrane was enriched in the water sample by rotating and stirring at a speed of 3000 rpm for 30 minutes in a clockwise / counterclockwise rotation mode.

[0063] The above-mentioned silicone rubber composite film was enriched and extracted, and then subjected to thermal desorption and ion mobility spectrometry analysis. The results showed that the characteristic peak mobility constant of tetrachloroethylene was 1.83±0.03 and the maximum peak height was 5.8V.

[0064] Example 3

[0065] In this embodiment, the number of silicone rubber sheets is 20, with a thickness of 0.1 mm and a length of 30 cm;

[0066] The silicone rubber sheet and the isolation mesh are arranged in a non-parallel, free arrangement.

[0067] Following the method of enriching and extracting organic matter from air, the rapid enricher of the aforementioned silicone rubber composite membrane was placed in air containing 1 ppm tetrachloroethylene and allowed to stand for 48 hours to enrich organic matter at an air humidity of 20%RH. After heating and thermal desorption and ion mobility spectrometry analysis, the migration constant of the characteristic peak of tetrachloroethylene was found to be 1.83±0.03, and the maximum peak height was 6.2V.

[0068] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of this utility model, and are not intended to limit it. Although the utility model has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of this utility model.

Claims

1. A rapid concentrator for a stirred silicone rubber composite membrane, characterized by, It includes a connecting rod, a fixing head, an isolation net, and a silicone rubber sheet. The isolation net is connected to the silicone rubber sheet and then clamped inside the fixing head. The fixing head is connected to the connecting rod, and the connecting rod can be connected to the output end of the electric drill in the first working state.

2. The rapid concentrator of a stirred silicone rubber composite membrane according to claim 1, characterized in that, In the second working state, the rapid enrichment device is placed inside the thermal desorption container, which includes an open cavity, a top cover, a heating element, an inlet pipe, and an outlet pipe. The cavity and the top cover are connected by threads. The inlet pipe and the outlet pipe are used to connect the carrier gas circuit of the ion migration tube in series. The heating element is used to heat and volatilize the organic matter enriched by the silicone rubber sheet in the first working state.

3. The rapid concentrator of a stirred silicone rubber composite membrane according to claim 1, characterized in that, The number of silicone rubber sheets is 1 to 20.

4. The rapid concentrator of a stirred silicone rubber composite membrane according to claim 1, characterized in that, The thickness of the silicone rubber sheet is 0.1~1mm and the length is 3~30cm.

5. The rapid concentrator of a stirred silicone rubber composite membrane according to claim 1, characterized in that, The arrangement of the silicone rubber sheet and the isolation net is selected from: parallel arrangement at intervals, free arrangement without parallelism, spiral roll of 1 silicone rubber sheet and 1 isolation net, or spiral roll of n silicone rubber sheets and n-1 isolation nets, where n≥2.

6. The rapid concentrator of a stirred silicone rubber composite membrane according to claim 1, characterized in that, The isolation net is made of stainless steel or polytetrafluoroethylene.

7. The rapid concentrator of a stirred silicone rubber composite membrane according to claim 1, characterized in that, The mesh size of the isolation net is 0.1~1mm, and the thickness is 0.05~0.2mm.

8. The rapid concentrator of a stirred silicone rubber composite membrane according to claim 1, characterized in that, The fixing head has a slot inside, the depth of which is adapted to the total thickness of each silicone rubber sheet and the isolation mesh, for clamping and fixing the composite film.

9. The rapid concentrator of a stirred silicone rubber composite membrane according to claim 1, characterized in that, The fixing head and the connecting rod are connected by a snap fastener. The snap fastener connection includes a boss on the fixing head and a groove on the connecting rod. The boss and the groove are interference-fitted, and the outer wall of the boss is provided with anti-slip texture.

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