A solid phase extraction device for large volume detection of plasticizers in water-sports products

Abstract

The utility model relates to a kind of solid phase extraction device of bulky water sample, especially a kind of solid phase extraction device of bulky water product plasticizer detection, the device is mainly related to four parts: sample loading part, solid phase extraction part, eluent collection part, waste liquid treatment part, sample loading device part is composed of separating funnel, separating funnel frame, for controlling sample into solid phase extraction column;Solid phase extraction part is composed of silica gel sealing ring, glass solid phase extraction column, glass jar and its top cover and vacuum pump connection port;Eluent collection part is composed of test tube rack, with scale nitrogen blowing tube;Waste liquid collection part is composed of glass jar and its drain, glass jar anti-skid base.In the device, solid phase extraction of phthalate in water product soaking liquid is carried out, and the detection result meets the standard requirement, the device has lower background value compared with the solid phase extraction device currently sold on the market, and the detection result is more accurate, more convenient for actual operation.

Description

Technical Field

[0001] This utility model relates to a device for solid-phase extraction of phthalates, plasticizers, from water-related products. Specifically, it relates to a sample flow path free of plastic products, a 1.0L separatory funnel for holding the sample, a separatory funnel and a vacuum pump valve for unified control of the sample flow rate, a large-volume waste liquid collection device, a waste liquid discharge device, and an extract collection device. Background Technology

[0002] Phthalate esters, also known as phthalic acid esters, are a collective term for esters formed from phthalic acid. Excessive PAEs can interfere with the human endocrine system. Because of their ability to soften plastics, they are widely used as plasticizers in plastic products. Many plastic products in water-related applications come into full contact with drinking water, and the potential leaching of plasticizers is highly relevant to drinking water quality. The "Standards for Drinking Water Quality" (GB 5749-2022) sets the limit for dioctyl phthalate in water at 0.008 mg / L. The "Standards for Hygienic Safety Evaluation of Drinking Water Transmission and Distribution Equipment and Protective Materials" (Health Law Supervision Document

[2001] No. 161) requires that the amount of phthalate esters introduced into drinking water after immersion in a certain amount of drinking water transmission and distribution equipment and protective materials should not exceed 0.01 mg / L. The current standard "Standard Examination Methods for Drinking Water - Part 8: Organic Matter Indicators" (GBT5750.8-2023) specifies solid-phase extraction (SPE) as the detection method. This requires extraction of a 1.0L volume of soaking solution at a flow rate of 10–15 ml / min. Currently available SPE devices introduce large volumes of samples using plastic tubes to draw water from the sample bottle. The SPE column, flow control valve, and guide tube are mostly made of plastic, posing a potential risk of PAE (phthalic acid ester) precipitation, making them unsuitable for phthalate detection. Furthermore, their waste collection containers are typically only 1L in volume and lack a waste discharge port, necessitating frequent interruptions of the extraction process for waste discharge, causing operational inconvenience. If waste is not discharged promptly, excessive waste will be drawn into the vacuum pump.

[0003] Based on this, this utility model designs a solid phase extraction device for detecting plasticizers in large-volume water-related products, in order to solve the problem that PAEs may precipitate during solid phase extraction in the aforementioned commercially available solid phase extraction devices. Utility Model Content

[0004] To address the problems existing in the background technology, a solid-phase extraction device that is more suitable for PAE extraction is designed.

[0005] To achieve the above objectives, this utility model provides the following technical solution: a solid-phase extraction device for detecting plasticizers in large-volume water-related products, comprising a sample loading section, a solid-phase extraction section, an eluent collection section, a waste liquid treatment section, and a sample, characterized in that: Sample loading section: The sample loading section consists of a separatory funnel and a separatory funnel holder, used to control the sample to enter the solid phase extraction section; Solid phase extraction section: The solid phase extraction section consists of a silicone sealing ring, a glass cylinder top cover, a solid phase extraction column, a glass cylinder, and a vacuum pump connection port; Elution buffer collection section: The eluent collection section consists of a test tube rack and a graduated nitrogen blow-off tube; Waste liquid collection section: The waste liquid collection section consists of a glass tank, a drain outlet, and an anti-slip base for the glass tank; The separating funnel is mounted on the separating funnel stand. The solid-phase extraction column is positioned directly below the sample outlet of the separating funnel, with the funnel outlet slightly submerged. An extraction column hole is provided at the junction of the glass cylinder top cover and the solid-phase extraction column. A silicone sealing ring is placed inside the extraction column hole to facilitate the solid-phase extraction column's fixation and sealing. A glass cylinder is located under the glass cylinder top cover. A test tube rack is provided inside the glass cylinder for eluent collection. The test tube rack has holes for placing graduated nitrogen blow-off tubes, which are connected to the lower end of the solid-phase extraction column. The vacuum pump connection port is located on the upper end of the glass cylinder side wall, and the drain port is located on the lower end of the glass cylinder side wall. The anti-slip base of the glass cylinder is located at the bottom of the glass cylinder.

[0006] Preferably, the separating funnel has a volume of 1.0L; the length, width, and height of the separating funnel stand are 450mm, 200mm, and 400mm, respectively; the glass cylinder top cover is made of polytetrafluoroethylene, with a length, width, and thickness of 400mm, 180mm, and 5mm, respectively; the solid-phase extraction column is a 6mL glass column containing 200mg of highly cross-linked polymethyl methacrylate-styrene extraction phase, with a diameter of 15mm; the silicone sealing ring has a diameter of 15mm; and the vacuum... The pump connection port has a diameter of 4mm; the test tube rack is made of aluminum, with a length, width, and height of 300mm, 120mm, and 100mm respectively; the graduated nitrogen blow tube has a volume of 10mL with a minimum graduation of 0.1mL; the drain port has a diameter of 4mm; the anti-slip base of the glass cylinder is made of ordinary rubber, with a length, width, and thickness of 400mm, 180mm, and 5mm respectively; the glass cylinder has a length, width, height, and thickness of 360mm, 160mm, 200mm, and 5mm respectively.

[0007] Preferably, the sample and extract do not come into contact with plastic articles that may contain plasticizers.

[0008] Preferably, a vacuum pump valve is connected to the vacuum pump connection port, and the sample is placed in the separatory funnel, which is suitable for solid-phase extraction of large-volume samples. The sample flow rate is controlled by the separatory funnel and the vacuum pump valve, which is easy to implement.

[0009] Preferably, the glass cylinder is a large-volume glass waste liquid tank, which facilitates the collection of waste liquid after extraction of multiple samples. The drain port is equipped with a drain valve to facilitate centralized discharge of waste liquid without interrupting the experimental operation.

[0010] Preferably, a vacuum valve is installed at the top of the glass waste liquid tank, so that the vacuuming operation is not affected when there is less than 8L of accumulated liquid in the glass waste liquid tank.

[0011] Preferably, it has three extraction positions, which is beneficial to ensure that the extraction conditions of one blank sample and two parallel sample solutions required for testing one water-related product sample are consistent under the same vacuum degree, and the extraction rates are comparable.

[0012] Compared with the prior art, the beneficial effects of this utility model are as follows: The sample container of this utility model is a separatory funnel. After the sample flow rate is adjusted, it flows directly into the glass extraction column. The waste liquid is collected in the glass cylinder. After extraction, the eluent directly enters the glass nitrogen blow-off tube through the extraction column outlet. There are no plastic products in the entire sample flow path, eliminating potential background detection interference. The separatory funnel and adjustable vacuum pump are used to control the flow rate of the sample entering the extraction column and the flow rate of the sample passing through the column, so that the two are consistent and reach the standard required flow rate. The glass waste liquid collection cylinder effectively prevents the organic eluent from corroding the cylinder body. Its volume is 11.5L and can collect about 8.0L of waste liquid for one discharge, which fully meets the requirement of extracting three samples at the same vacuum level and discharging the waste liquid at one time. The use of a nitrogen blow-off tube with a minimum scale of 0.1mL is conducive to accurate quantification of the concentrated volume of the extract. Attached Figure Description

[0013] To more clearly illustrate the technical solutions of the embodiments of this utility model, the accompanying drawings used in the description of the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this utility model. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0014] Figure 1 This is a schematic diagram of a solid-phase extraction device for detecting plasticizers in large-volume water-related products according to this utility model. Figure 2 This is a schematic diagram of the experimental results of this utility model.

[0015] 1-Separating funnel, 2-Separating funnel stand, 3-Glass cylinder top cover, 4-Solid phase extraction column, 5-Silicone sealing ring, 6-Vacuum pump connection port, 7-Test tube rack, 8-Graded nitrogen blowpipe, 9-Drain port, 10-Glass cylinder anti-slip base, 11-Glass cylinder. Detailed Implementation

[0016] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those skilled in the art without creative effort are within the protection scope of the present utility model.

[0017] Please see Figure 1 As shown, this utility model provides a technical solution: a solid-phase extraction device for detecting plasticizers in large-volume water-related products, comprising a sample loading section, a solid-phase extraction section, an eluent collection section, a waste liquid treatment section, and a sample, characterized in that: Sample loading section: The sample loading section consists of a separatory funnel 1 and a separatory funnel holder 2, which are used to control the sample to enter the solid phase extraction section; Solid phase extraction section: The solid phase extraction section consists of a silicone sealing ring 5, a glass cylinder top cover 3, a solid phase extraction column 4, a glass cylinder 11, and a vacuum pump connection port 6. Elution buffer collection section: The eluent collection section consists of a test tube rack 7 and a graduated nitrogen blow-off tube 8; Waste liquid collection section: The waste liquid collection section consists of a glass tank 11, a drain outlet 9, and a non-slip base 10 for the glass tank; The separating funnel 1 is mounted on the separating funnel stand 2. The solid-phase extraction column 4 is positioned directly below the sample outlet of the separating funnel 1, with the funnel outlet slightly submerged. An extraction column hole is provided at the junction of the glass cylinder top cover 3 and the solid-phase extraction column 4. A silicone sealing ring 5 is placed inside the extraction column hole to facilitate the fixation and sealing of the solid-phase extraction column 4. The solid-phase extraction column 4 and the extraction column hole are located at the glass cylinder top cover 3. A glass cylinder 11 is provided below the glass cylinder top cover 3. A test tube rack 7 is provided inside the glass cylinder 11 for collecting the eluent. A graduated nitrogen blow-off tube 8 is placed in a hole on the test tube rack 7. The graduated nitrogen blow-off tube 8 is connected to the lower end of the solid-phase extraction column 4. The vacuum pump connection port 6 is located at the upper end of the side wall of the glass cylinder 11. The drain port 9 is located at the lower end of the side wall of the glass cylinder 11. The anti-slip base 10 of the glass cylinder is located at the bottom of the glass cylinder 11.

[0018] The separatory funnel has a volume of 1.0L; the length, width, and height of the separatory funnel stand are 450mm, 200mm, and 400mm respectively; the glass cylinder top cover is made of polytetrafluoroethylene, with a length, width, and thickness of 400mm, 180mm, and 5mm respectively; the solid-phase extraction column is a 6mL glass column with a built-in 200mg highly cross-linked polymethyl methacrylate-styrene extraction phase and a diameter of 15mm; the silicone sealing ring has a diameter of 15mm; the vacuum pump connection port has a diameter of 4mm; the test tube rack is made of aluminum, with a length, width, and height of 300mm, 120mm, and 100mm respectively; the graduated nitrogen blow-off tube has a volume of 10mL with a minimum graduation of 0.1mL; the drain port has a diameter of 4mm; the anti-slip base of the glass cylinder is made of ordinary rubber, with a length, width, and thickness of 400mm, 180mm, and 5mm respectively; the length, width, height, and thickness of the glass cylinder are 360mm, 160mm, 200mm, and 5mm respectively.

[0019] The sample and extract did not come into contact with potentially plasticized plastic products.

[0020] The vacuum pump is connected to a vacuum pump valve. The sample is placed in the separatory funnel, and the sample flow rate is controlled by the separatory funnel and the vacuum pump valve.

[0021] The glass tank is a large-volume glass waste liquid tank, which facilitates the collection of waste liquid after extraction of multiple samples. A drain valve is installed on the drain outlet to facilitate the centralized discharge of waste liquid.

[0022] A vacuum valve is installed at the top of the glass waste liquid tank. The vacuuming operation is not affected when there is less than 8L of accumulated liquid in the glass waste liquid tank.

[0023] It has three extraction positions, which is beneficial to ensure that the extraction conditions of one blank sample and two parallel sample solutions required for testing one water-related product sample are consistent under the same vacuum degree.

[0024] A specific application of this embodiment is as follows: The method of using this utility model is as follows: First, close the separatory funnel valve, accurately measure 1.0L of sample and place it in the separatory funnel 1, then place the glass cylinder 11 below the separatory funnel 1, then put the solid phase extraction column 4 with the silicone sealing ring 5 and fix it on the top cover 3 of the glass cylinder, then close the top cover 3 of the glass cylinder, then adjust the position of the solid phase extraction column 4 so that the outlet of the separatory funnel 1 is located inside the solid phase extraction column 4, then close the drain valve, connect the vacuum pump, and finally start the vacuum pump, adjust the flow rate of the separatory funnel valve and the vacuum valve so that the liquid flowing out of the solid phase extraction column 4 is 5 drops / s, about 15mL / min. After the extraction is completed, remove the separatory funnel holder 2, continue to evacuate the vacuum for 1-2 minutes to dehydrate the solid phase extraction column, close the vacuum valve, open the drain valve to discharge the waste liquid. Apart from this, the remaining steps are operated according to GB / T5750. Compared with the currently commercially available solid phase extraction devices, this device has a lower background value, more accurate detection results, and is more convenient for actual operation.

[0025] Please see Figure 2 As shown, Figure 2 In the second embodiment of the novel invention, experiments were conducted. The lowest detectable concentration using this device in blank detection reached 0.15 ug / L, far below the standard limit of 0.41 ug / L, with a relative standard deviation (RSD) of 4.5%. In the blank spiked test, the recovery rate was 102% with an RSD of 3.0% at a spiked amount of 0.40 ug / L, and 105% with an RSD of 1.8% at a spiked amount of 2.0 ug / L, both meeting the standard requirements. This indicates that this device is suitable for solid-phase extraction of phthalates (plasticizers) from the soaking solution of water-contaminated products.

[0026] In the description of this specification, references to terms such as "an embodiment," "example," "specific example," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the present invention. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples.

[0027] The preferred embodiments of this utility model disclosed above are merely illustrative of the present utility model. These preferred embodiments do not exhaustively describe all details, nor do they limit the utility model to the specific implementations described. Clearly, many modifications and variations can be made based on the content of this specification. This specification selects and specifically describes these embodiments to better explain the principles and practical applications of this utility model, thereby enabling those skilled in the art to better understand and utilize it. This utility model is limited only by the claims and their full scope and equivalents.

Claims

1. A solid-phase extraction device for detecting plasticizers in large-volume water-related products, comprising a sample loading section, a solid-phase extraction section, an eluent collection section, a waste liquid treatment section, and a sample, characterized in that: Sample loading section: The sample loading section consists of a separatory funnel (1) and a separatory funnel holder (2), which are used to control the sample to enter the solid phase extraction section; Solid phase extraction section: The solid phase extraction section consists of a silicone sealing ring (5), a glass cylinder top cover (3), a solid phase extraction column (4), a glass cylinder (11), and a vacuum pump connection port (6); Elution fluid collection section: The elution fluid collection section consists of a test tube rack (7) and a graduated nitrogen blow-off tube (8); Waste liquid collection section: The waste liquid collection section consists of a glass cylinder (11), a drain port (9), and a glass cylinder anti-slip base (10); The separating funnel (1) is mounted on the separating funnel stand (2). The solid phase extraction column (4) is positioned directly below the sample outlet of the separating funnel (1) and the funnel outlet is slightly submerged. The glass cylinder top cover (3) has an extraction column hole at the junction with the solid phase extraction column (4). The silicone sealing ring (5) is placed inside the extraction column hole to facilitate the solid phase extraction column (4) to be fixed and sealed. A glass cylinder (11) is provided under the glass cylinder top cover (3). A test tube rack (7) is provided inside the glass cylinder (11) when collecting the eluent. A graduated nitrogen blow-off tube (8) is placed in the test tube rack (7). The graduated nitrogen blow-off tube (8) is connected to the lower end of the solid phase extraction column (4). The vacuum pump connection port (6) is located on the upper end of the side wall of the glass cylinder (11). The drain port (9) is located on the lower end of the side wall of the glass cylinder (11). The anti-slip base (10) of the glass cylinder is located at the bottom of the glass cylinder (11).

2. The solid-phase extraction device for detecting plasticizers in large-volume water-related products according to claim 1, characterized in that: The separating funnel (1) has a volume of 1.0L; the length, width, and height of the separating funnel stand (2) are 450mm, 200mm, and 400mm, respectively; the glass cylinder top cover (3) is made of polytetrafluoroethylene, with a length, width, and thickness of 400mm, 180mm, and 5mm, respectively; the solid phase extraction column (4) is a 6mL glass column containing 200mg of highly cross-linked polymethyl methacrylate-styrene extraction phase, with a diameter of 15mm; the silicone sealing ring (5) has a diameter of 15mm; the vacuum pump is connected to... The Φ of the opening is 4mm; the test tube rack (7) is made of aluminum, with a length, width and height of 300mm, 120mm and 100mm respectively; the volume of the graduated nitrogen blow tube (8) is 10mL and the minimum graduation is 0.1mL; the Φ of the drain port (9) is 4mm; the anti-slip base (10) of the glass cylinder is made of ordinary rubber, with a length, width and thickness of 400mm, 180mm and 5mm respectively; the length, width, height and thickness of the glass cylinder (11) are 360mm, 160mm, 200mm and 5mm respectively.

3. The solid phase extraction device for detecting plasticizer in a large volume water contact product according to claim 1, characterized in that: The sample and extract were not in contact with any potentially plasticized plastic products.

4. The solid-phase extraction device for detecting plasticizers in large-volume water-related products according to claim 2, characterized in that: A vacuum pump valve is connected to the vacuum pump connection port (6). The sample is placed in the separatory funnel (1). The sample flow rate is controlled by the separatory funnel (1) and the vacuum pump valve.

5. The solid phase extraction device for detecting plasticizer in a large volume water contact product according to claim 2, characterized in that: The glass cylinder (11) is a large-volume glass waste liquid tank, which facilitates the collection of waste liquid after extraction of multiple samples. The drain port (9) is equipped with a drain valve to facilitate the centralized discharge of waste liquid.

6. The solid-phase extraction device for detecting plasticizers in large-volume water-related products according to claim 5, characterized in that: A vacuum valve is installed at the top of the glass waste liquid tank, and the vacuuming operation is not affected when there is less than 8L of accumulated liquid in the glass waste liquid tank.

7. The solid-phase extraction device for detecting plasticizers in large-volume water-related products according to claim 1, characterized in that: It has three extraction positions, which is beneficial to ensure that the extraction conditions of one blank sample and two parallel sample solutions required for testing one water-related product sample are consistent under the same vacuum degree.

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