Extraction and filtration device for extracting target substances from solid samples

By using a modified extraction and filtration device in solid samples, multiple extraction and filtration are achieved, which solves the problems of low recovery rate and poor stability during the extraction process in the prior art, and improves the accuracy and working efficiency of sample analysis .

CN112843783BActive Publication Date: 2025-02-11TIANJIN ENVIRONMENT MONITORING CENT
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Patent Information

Application Number
CN202110084199.0
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2021-01-21
Publication Date
2025-02-11
Estimated Expiration
2041-01-21

AI Technical Summary

Technical Problem

The prior art is difficult to achieve multiple extractions during the extraction process of semi-volatile and non-volatile organic matter in solid samples, resulting in low recovery and poor stability, which affects the accuracy of sample analysis.

Method used

It provides an extraction and filtration device, which is used to perform ultrasonic extraction or oscillation extraction using an extraction bottle, and after completion, it is converted into an extract liquid filtration kit to achieve multiple extractions and filtration, and improve the accuracy of sample analysis.

Benefits of technology

Through multiple extractions and filtration, the accuracy of sample analysis is improved, sample loss is reduced, working efficiency is improved, and it is suitable for the extraction of organic matter with poor thermal stability or strong water-solubleness.

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Abstract

The present invention relates to an extraction and filtration device for extracting a target substance from a solid sample, wherein the main body is an extraction bottle. After the extraction is performed using the extraction bottle, the extraction bottle is converted into an extraction liquid filtration kit to facilitate filtering the extraction liquid. The extraction bottle comprises a bottle body (4) with an open top and a bottom, a first sealing screw cover (1), a second sealing screw cover (8) and a fastening clamp (9), wherein a screw cover fastening groove (14) is arranged on the outer surface of the second sealing screw cover (8); a bottle mouth fastening groove (5) is arranged on the outer surface of the lower end of the bottle body (4) near the position of the lower screw mouth (6) of the extraction bottle; the fastening clamp (9) is in a double arc shape, including a bottle mouth arc circle (91) and a screw cover arc circle (92). The present invention can conveniently realize multiple extractions by extraction methods such as ultrasonic extraction method and oscillation extraction method, thereby improving the accuracy of sample analysis.
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Description

Technical Field

[0001] The invention relates to the technical field of organic matter analysis, and relates to an extraction and filtering device and an extraction method for extracting a target object from a solid sample, and is particularly suitable for extracting semi-volatile and non-volatile organic matter. Background Art

[0002] With the continuous acceleration of the development of industry and agriculture in my country, the large-scale use of various chemical raw materials, chemical products and by-products, pesticides, veterinary drugs, herbicides, etc. has led to the continuous increase in the content of organic pollutants in environmental media such as water bodies, soils and sediments in my country. Environmental pollution problems seriously affect the sustainable development of the natural environment and pose a huge threat to human health. At present, semi-volatile organic compounds (SVOCs) and non-volatile organic compounds (NVOCs) in solid matrices such as soil and sediments are mainly extracted through pretreatment technology. After purification and concentration, they are analyzed using instruments such as gas chromatography (GC), gas chromatography / mass spectrometry (GC / MS or GC / MS / MS), liquid chromatography (HPLC) or liquid chromatography / mass spectrometry (HPLC / MS or HPLC / MS / MS), and sample extraction technology has a decisive influence on the accuracy of sample test results. Commonly used pretreatment techniques for solid matrix samples such as soil and sediment include Soxhlet Extraction (SE), Pressurized Liquid Extraction (PLE) / Accelerated Solvent Extraction (ASE), Ultrasonic Extraction (UE), Microwave Assisted Extraction (MAE), Oscillatory Extraction (OE) (including horizontal oscillation, flip oscillation, etc.). Each of the above methods has different advantages and disadvantages. For example, SE is a classic solid sample extraction method with high recovery rate but long time consumption; PLE and ASE have high automation and good recovery, but the instrument is expensive. SE, PLE and ASE are not suitable for the determination of compounds that are easily decomposed at high temperature and compounds with strong water solubility. UE and OE have the advantages of low instrument cost, small space occupation, easy use, short extraction time, simultaneous extraction of multiple samples, high work efficiency, and are particularly suitable for extracting components with poor thermal stability, strong water solubility and high polarity, and have received widespread attention and application. However, the two methods currently have a technical bottleneck that the extraction container is only suitable for one extraction of the sample, making it difficult to achieve the multiple extractions required for the full determination of the target in the sample. When determining the total content of the target in the sample, the recovery rate is low and the stability is poor. Summary of the invention

[0003] In order to solve the above problems, the present invention provides an extraction and filtration device that can conveniently implement multiple extractions by extraction methods such as ultrasonic extraction and oscillation extraction, and improve the accuracy of sample analysis. The technical solution is as follows:

[0004] An extraction and filtration device for extracting a target substance from a solid sample, wherein the main body is an extraction bottle. After the extraction is performed using the extraction bottle, the extraction bottle is converted into an extraction liquid filtration kit to facilitate filtering the extraction liquid, wherein:

[0005] The extraction bottle comprises a bottle body 4 with open upper and lower ends, a first sealing screw cover 1, a second sealing screw cover 8 and a fastening clip 9. The upper and lower ends of the bottle body 4 are both provided with threads. The upper end is called the upper screw opening 3 of the extraction bottle, which cooperates with the first sealing screw cover 1; the lower end is called the lower screw opening 6 of the extraction bottle, which cooperates with the second sealing screw cover 8;

[0006] A screw cover fastening groove 14 is provided on the outer surface of the second sealing screw cover 8; a bottle mouth fastening groove 5 is provided on the outer surface of the lower end of the bottle body 4 near the lower screw mouth 6 of the extraction bottle; the fastening clamp 9 is in a double arc shape, including a bottle mouth arc circle 91 and a screw cover arc circle 92, and the inner walls of the bottle mouth arc circle 91 and the screw cover arc circle 92 are both provided with raised small teeth, the small teeth on the inner wall of the bottle mouth arc circle 91 match the bottle mouth fastening groove 5, and the small teeth on the inner wall of the screw cover arc circle 92 match the screw cover fastening groove 14 on the outer surface of the second sealing screw cover 8.

[0007] The above-mentioned extraction bottle is converted into an extraction liquid filtration kit, comprising: a bottle body 4 with open upper and lower ends, a second sealing screw cover 8, threads are arranged on the upper and lower ends of the bottle body 4, the lower end is called the lower screw mouth 6 of the extraction bottle, which cooperates with the second sealing screw cover 8, and the upper end is called the upper screw mouth 3 of the extraction bottle. The extraction liquid filtration kit also includes filter paper 10, a filter screen plate 11, a funnel 12 and a perforated fastening screw cover 13 made according to the size of the upper screw mouth 3 of the extraction bottle, the small holes arranged on the filter screen plate 11 are used to pass the extraction liquid; the perforated fastening screw cover 13 has a hole in the middle; the perforated fastening screw cover 13 is used to fix the filter paper 10, the filter screen plate 11, and the funnel 12 on the upper screw mouth 3 of the extraction bottle.

[0008] Furthermore, the extraction bottle further comprises a hoop 93 , and the bottle mouth arc circle 91 and the screw cover arc circle 92 are fixedly connected by the hoop 93 .

[0009] Furthermore, the upper edge of the funnel 12 has a protruding outer edge, and the size of the protruding outer edge matches the inner diameter of the perforated fastening screw cover 13 .

[0010] Furthermore, the extract filtering kit also includes a sealing ring that matches the inner diameter of the perforated fastening screw cover 13 for sealing connection.

[0011] Furthermore, the filter paper is a quantitative filter paper that does not contain the target object.

[0012] Furthermore, the first sealing screw cover and the screw opening on the extraction bottle are sealed and connected via a sealing gasket.

[0013] Furthermore, the second sealing screw cover and the lower screw opening of the extraction bottle are sealed and connected via a sealing gasket.

[0014] Furthermore, the size of the hole in the middle of the perforated fastening screw cover 13 is determined according to the size of the front part of the funnel 12 .

[0015] The beneficial effects of the present invention are:

[0016] (1) The present invention provides an extraction bottle that can be used for separating organic matter in a solid matrix. The extraction bottle can be combined with an extraction method such as ultrasonic extraction or oscillation extraction to achieve the extraction of the target substance. Since no pressurization or heating is required during the extraction process, extraction can be achieved at room temperature or even low temperature. The extraction bottle is particularly suitable for the extraction of organic matter with poor thermal stability or strong water solubility.

[0017] (2) A groove design is adopted for one end of the extraction bottle and the connected screw cap, and a toothed fastening clamp is used to fix the two. The protruding teeth of the toothed fastening clamp are evenly distributed on the inner side of the large arc circle and the bottle mouth arc circle. The teeth of the bottle mouth arc circle are large, and the teeth of the large arc circle are small. The corresponding grooves on one end of the extraction bottle are sparse, and the grooves on the outer side of the screw cap are dense. The large teeth on the inner side of the bottle mouth arc circle match the large grooves of the extraction bottle, and the small teeth on the inner side of the large arc circle match the small grooves on the outer side of the screw cap. This can effectively ensure the airtightness of the extraction bottle during the extraction process and prevent leakage of the extract and sample.

[0018] (3) The design of the large groove at one end of the extraction bottle and the small groove on the connected screw cap facilitates processing and operation.

[0019] (4) There are three evenly distributed and outwardly protruding semi-curved ring hoops between the large arc circle of the toothed fastening clamp and the arc circle of the bottle mouth, so that the large and small arc circles of the fastening clamp can be firmly connected. The stainless steel or plastic material ensures that the extraction bottle has a certain elasticity when fixed to the screw cap, and the operation is convenient.

[0020] (5) After a sample extraction is completed, the first sealing screw cap is replaced with filter paper, filter screen plate, funnel and filter kit with a perforated fastening screw cap, and then the extraction bottle is turned over to achieve the purpose of filtering the extract, with less loss and convenient operation.

[0021] (6) The filter screen is made of polytetrafluoroethylene or ceramic, with multiple circular holes evenly distributed on it, which can support the filter paper during filtration, allowing the filtrate to pass through the filter paper smoothly and preventing the target object from being adsorbed on the filter screen.

[0022] (7) The perforated screw cap can be used to fasten the funnel, filter screen plate and filter paper to the upper end of the extraction bottle through the protrusion of the edge of the funnel mouth, tightly connecting them together, thereby preventing leakage of the filtrate during the filtration process.

[0023] (8) If multiple extractions are required, only the filter kit needs to be replaced and the extraction solution refilled to perform secondary extractions. Since the sample is always in the same extraction bottle, the loss of sample transfer is prevented, the accuracy of the measurement is improved, and the operation is convenient.

[0024] (9) The extraction kit is small in size and simple in structure, and can realize the extraction of multiple samples at the same time, thereby improving work efficiency.

[0025] (10) The device has high accuracy, is easy to disassemble and clean, has low cost and high efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] Figure 1 This is an exploded view of the extraction bottle (the fastening clip is not shown in the figure);

[0027] Figure 2 Schematic diagram of the extraction bottle fastening clamp structure.

[0028] Figure 3 Schematic diagram of the extraction liquid filtration kit.

[0029] Among them, 1-the first sealing screw cap; 2-sealing gasket; 3-the upper screw mouth of the extraction bottle; 4-the bottle body; 5-the bottle mouth fastening groove; 6-the lower screw mouth of the extraction bottle; 7-sealing gasket; 8-the second sealing screw cap; 9-fastening clamp; 91-the bottle mouth arc ring; 92-the screw cap arc ring; 93-the hoop; 10-the filter paper; 11-the filter screen plate; 12-the funnel; 13-the fastening screw cap with holes; 14-the screw cap fastening groove. DETAILED DESCRIPTION

[0030] The technical solution of the present invention is further described below in conjunction with the accompanying drawings:

[0031] This embodiment provides an extraction and filtration device that can be used to extract organic matter from a solid matrix using methods such as ultrasonic extraction or vibration extraction. The main body of the device is an extraction bottle. After an extraction is performed using the extraction bottle, the extraction bottle is directly converted into an extraction liquid filtration kit to facilitate filtering of the extraction liquid.

[0032] Figure 1The figure is a schematic diagram of the structure of the extraction bottle. The extraction bottle mainly includes a bottle body 4, a first sealing screw cover 1 and a second sealing screw cover 8. The upper and lower ends of the bottle body 4 are open, and threads are arranged on the outside. The upper end is called the upper screw opening 3 of the extraction bottle, and the lower end is called the lower screw opening 6 of the extraction bottle. The first sealing screw cover 1 and the second sealing screw cover 8 are made of plastic material, and the sealing gasket 2 and the sealing gasket 7 are both lined with polytetrafluoroethylene. The bottle body 4 is made of glass or polytetrafluoroethylene. The upper screw opening 3 of the extraction bottle can be matched with the first sealing screw cover 1, and the lower screw opening 6 of the extraction bottle can be matched with the second sealing screw cover 8. The two sealing screw covers are sealed and connected to the two screw openings respectively through two sealing gaskets, and the polytetrafluoroethylene linings of the two sealing gaskets are both facing outwards. The outer surface of the second sealing screw cover 8 is also provided with a screw cover fastening groove 14.

[0033] The structure of the fastening clip 9 is as follows Figure 2 As shown. The material of the fastening clamp 9 is plastic with certain toughness and fastening ability (stainless steel or aluminum materials, etc. can also be used). The fastening clamp 9 is in a double arc shape, including a bottle mouth arc circle 91 and a screw cover arc circle 92. The diameter of the bottle mouth arc circle 91 is smaller than the diameter of the screw cover arc circle 92, and the two are fixedly connected by a hoop 93. The inner walls of the bottle mouth arc circle 91 and the screw cover arc circle 92 are both provided with uniformly raised small teeth, and the raised small teeth of the two circles are matched with the bottle mouth fastening groove 5 and the screw cover fastening groove on the outer surface of the second sealing screw cover 8 respectively. The bottle mouth arc circle 91 and the screw cover arc circle 92 are respectively clamped on the tightly connected bottle mouth fastening groove 5 and the screw cover fastening groove of the second sealing screw cover 8 by using the raised small teeth on the inner wall. The groove size of the bottle mouth fastening groove is larger than the groove size of the screw cover fastening groove.

[0034] After the sample extraction is completed, when the target object needs to be filtered and extracted, the extraction bottle is modified to facilitate better filtering and extraction. The modified extraction bottle is called an extraction liquid filtration kit. The modification method is as follows:

[0035] According to the size of the screw mouth 3 on the extraction bottle, filter paper 10, filter screen plate 11, funnel 12 and perforated fastening screw cover 13 are manufactured. The filter paper 10 is a quantitative filter paper that does not contain the target substance. The filter screen plate 11 is made of polytetrafluoroethylene or ceramic material, and has small holes therein for the extraction liquid to pass through. The funnel 12 is made of glass or polytetrafluoroethylene material, and the upper edge has a circle of protruding outer edge, and the size of the protruding outer edge matches the inner diameter of the perforated fastening screw cover 13. The perforated fastening screw cover 13 has a hole in the middle, and the size of the hole is determined according to the size of the funnel 12. The perforated fastening screw cover 13 can fix the filter paper 10, filter screen plate 11 and funnel 12 on the screw mouth 3 on the extraction bottle.

[0036] When used as an extract filtration kit, remove the first sealing screw cap 1 and the sealing gasket 2, place the filter paper 10, the filter screen plate 11, and the funnel 12 on the screw mouth 3 of the extraction bottle in sequence, and fix the filter paper 10, the filter screen plate 11, and the funnel 12 on the screw mouth 3 of the extraction bottle with a perforated fastening screw cap 13. In this embodiment, since the funnel 12 is made of glass or polytetrafluoroethylene, the size of the protruding outer edge of the upper edge matches the inner diameter of the perforated fastening screw cap 13, thereby playing a sealing role. It is also possible not to make the protruding outer edge of the upper edge, but to make a sealing ring that matches the inner diameter of the perforated fastening screw cap 13, and use the sealing ring for sealing connection.

[0037] The working principle of the present invention is as follows:

[0038] When extracting the sample, the second sealing screw cover 8 and the sealing gasket 7 are respectively fastened to the lower screw mouth 6 of the bottle body 4, and the second sealing screw cover 8 and the bottle mouth fastening groove 5 are respectively tightened and fixed with a fastening clamp 9, the weighed solid sample and the extract are placed in the extraction bottle, the upper first sealing screw cover 1 and the sealing gasket 2 are fastened to the upper screw mouth 3 of the bottle body 4, and the bottle is placed in an ultrasonic extractor or fixed on an oscillator for extraction.

[0039] After the extraction is completed, the first sealing screw cap 1 and the sealing gasket 2 are replaced with the quantitative filter paper 10 and the filter screen plate 11, the filter paper 10 is placed on the upper screw mouth 3 of the bottle body 4, and the filter screen plate 11 and the funnel 12 are placed on it in sequence, and fixed to the upper screw mouth 3 of the extraction bottle with a perforated fastening screw cap 13, the extraction liquid filtration kit is reversed, and the extraction liquid collection container is placed under the outlet of the funnel 12, and the fixing clip 9 and the second sealing screw cap 8 and the sealing gasket 7 are removed to maintain the pressure balance during filtration, and the filtration is performed.

[0040] After the filtration is completed, if the solid sample needs to be repeatedly extracted, the second sealing screw cover 8 and the sealing gasket 7 are respectively fastened to the lower screw mouth 6 of the bottle body 4, and the second sealing screw cover 8 and the bottle mouth fastening groove 5 are tightened and fixed with the fastening clamp 9, the extraction bottle is reversed, the filter paper 10, the filter screen plate 11, the funnel 12 and the perforated fastening screw cover 13 are removed, and the extraction liquid is added, and the filter paper 10, the filter screen plate 11, the funnel 12, and the perforated fastening screw cover 13 are replaced with the first sealing screw cover 1 and the sealing gasket 2, and the secondary extraction and filtration are performed. Combine the extracts.

[0041] Repeat the above steps for multiple extractions.

[0042] For the devices described in the various embodiments of the present invention, any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. An extraction and filtration device for extracting a target substance from a solid sample, wherein the main body is an extraction bottle. After the extraction is performed using the extraction bottle, the extraction bottle is converted into an extraction liquid filtration kit to facilitate filtering the extraction liquid, wherein: The extraction bottle comprises a bottle body (4) with open top and bottom, a first sealing screw cover (1), a second sealing screw cover (8) and a fastening clamp (9). The top and bottom of the bottle body (4) are both provided with threads. The top is called the extraction bottle upper screw opening (3), which is matched with the first sealing screw cover (1); the bottom is called the extraction bottle lower screw opening (6), which is matched with the second sealing screw cover (8); A screw cap fastening groove (14) is arranged on the outer surface of the second sealing screw cap (8); a bottle mouth fastening groove (5) is arranged on the outer surface of the lower end of the bottle body (4) near the lower screw mouth (6) of the extraction bottle; the fastening clamp (9) is in a double arc shape, including a bottle mouth arc circle (91) and a screw cap arc circle (92); the inner walls of the bottle mouth arc circle (91) and the screw cap arc circle (92) are both provided with protruding small teeth, the small teeth on the inner wall of the bottle mouth arc circle (91) match the bottle mouth fastening groove (5), and the small teeth on the inner wall of the screw cap arc circle (92) match the screw cap fastening groove (14) on the outer surface of the second sealing screw cap (8); The above-mentioned extraction bottle is converted into an extraction liquid filtering kit, comprising: a bottle body (4) with open upper and lower ends, a second sealing screw cover (8), threads are arranged on the upper and lower ends of the bottle body (4), the lower end is called the extraction bottle lower screw mouth (6), which cooperates with the second sealing screw cover (8), and the upper end is called the extraction bottle upper screw mouth (3). In addition, the extraction liquid filtering kit also includes filter paper (10) made according to the size of the extraction bottle upper screw mouth (3), a filter screen plate (11), a funnel (12) and a perforated fastening screw cover (13), the small holes arranged on the filter screen plate (11) are used to pass the extraction liquid; the perforated fastening screw cover (13) has a hole in the middle; the perforated fastening screw cover (13) is used to fix the filter paper (10), the filter screen plate (11) and the funnel (12) on the extraction bottle upper screw mouth (3).

2. The extraction and filtration device according to claim 1, characterized in that The extraction bottle further comprises a hoop (93), and the bottle mouth circular arc circle (91) and the screw cover circular arc circle (92) are fixedly connected by the hoop (93).

3. The extraction and filtration device according to claim 1, characterized in that The upper edge of the funnel (12) has a protruding outer edge, and the size of the protruding outer edge matches the inner diameter of the perforated fastening screw cover (13).

4. The extraction and filtration device according to claim 1, characterized in that The extract filtering kit also includes a sealing ring matching the inner diameter of the fastening screw cover with holes for sealing connection.

5. The extraction and filtration device according to claim 1, characterized in that The filter paper is a quantitative filter paper that does not contain a target object.

6. The extraction and filtration device according to claim 1, characterized in that The first sealing screw cover and the screw opening on the extraction bottle are sealed and connected via a sealing gasket.

7. The extraction and filtration device according to claim 1, characterized in that The second sealing screw cover and the lower screw opening of the extraction bottle are sealed and connected via a sealing gasket.

8. The extraction and filtration device according to claim 1, characterized in that The size of the hole in the middle of the perforated fastening screw cover is determined according to the size of the front part of the funnel.

Citation Information

Patent Citations

  • Extraction and filtration method for extracting target object in solid sample

    CN112843782A

  • Extraction and filtration device for extracting target object in solid sample

    CN214808572U