Water heavy metal element enrichment and sample preparation device for XRF (X-Ray Fluorescence) detection
By designing a sample preparation device for enriching heavy metal elements in water for XRF detection, a sample presser is used to compress particulate enrichment materials into sample cakes, which solves the equipment and power limitations of XRF detection equipment in trace analysis of liquid samples, and achieves rapid enrichment and detection.
Patent Information
- Application Number
- CN202422617901.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-29
- Publication Date
- 2026-01-23
- Estimated Expiration
- 2034-10-29
AI Technical Summary
Existing XRF detection equipment suffers from high scattering background and poor signal-to-noise ratio when performing trace analysis in liquid samples. It also requires additional equipment and power supply, which cannot meet the needs of rapid enrichment and detection on site.
A sample preparation device for enriching heavy metal elements in water for XRF detection was designed, including a sample carrier, a membrane ring, a circular limiting cap, and a sample presser. The sample presser compresses the particulate enrichment material into a sample cake to be tested, realizing in-situ enrichment of liquid samples and simplifying the sample preparation process.
It achieves efficient enrichment of heavy metal elements in liquid samples and simplifies the sample preparation process, improves detection sensitivity, meets the needs of rapid on-site enrichment and detection, simplifies equipment requirements, and avoids carrying additional instruments and power supplies.
Smart Images
Figure CN223827593U_ABST
Abstract
Description
Technical Field
[0001] This application relates to the field of XRF detection technology, and in particular to a water heavy metal enrichment sample preparation device for XRF detection. Background Technology
[0002] X-ray fluorescence spectrometry (XRF) is an environmentally friendly, non-destructive, multi-element simultaneous analysis method widely used for the analysis of major, minor, and trace elements in environmental samples. In recent years, portable XRF spectrometers have been widely used in trace element analysis of geological materials due to their small size, light weight, fast analysis speed, and non-destructive on-site detection capabilities. They can also perform qualitative and quantitative analysis based on the characteristic X-ray fluorescence energy, wavelength, and intensity emitted by heavy metals excited to high energy states. However, XRF technology is typically used to analyze solid environmental samples. When directly analyzing liquid samples, the high background scattering of X-rays, poor signal-to-noise ratio, and high uncertainty in the results limit its application, with detection limits generally above mg / L.
[0003] Therefore, in order for portable XRF devices to meet the requirements for detecting trace analytes in liquid samples at the μg / L level, a pre-enrichment method is generally used to enrich the target substance in the liquid sample with an enrichment material, so that the content of the target substance in the liquid sample in the enrichment material is increased to above the detection limit of the XRF device, thereby realizing the detection of the content of the target substance in the liquid sample.
[0004] However, current on-site testing processes require small solid-phase extraction devices to enrich the liquid under positive pressure, followed by vacuum pump-assisted negative pressure filtration to collect the enriched material. This necessitates carrying the necessary instruments and power supply. Furthermore, due to equipment limitations, the volume of enriched liquid is relatively small; large volumes of liquid require repeated operations, failing to meet the demands for rapid on-site enrichment and testing.
[0005] On the other hand, although existing enrichment devices do not have an external power supply, the operation method is complicated and still requires manual vacuum filtration pump. The enriched material is then vacuum filtered onto a filter membrane, the filter membrane is removed, and a sample is prepared using a sample box. The prepared sample is then sent to the XRF detection equipment for detection.
[0006] Therefore, there is an urgent need for a new water-based heavy metal enrichment and sample preparation device for XRF detection to meet the requirements of rapid on-site enrichment and detection. Utility Model Content
[0007] This application provides a water heavy metal element enrichment and sample preparation device for XRF detection, characterized in that it includes:
[0008] A sample carrier for collecting particulate enriched material is cylindrical and has a first open side and a second open side. The sample carrier includes a sample collection part and a sample cup part, which are arranged sequentially from the first open side to the second open side in the axial direction of the sample carrier and are interconnected with each other.
[0009] A membrane sleeve ring is fitted around the outer periphery of the sample cup to fix the filter screen used for filtering liquids.
[0010] The circular limiting cap is located on the second open side. The circular limiting cap is detachably connected to the sample collection part and is used to fix the membrane sleeve. The circular limiting cap itself has a liquid outlet corresponding to the position of the sample cup part in the axial direction.
[0011] The sample press includes a connected pressure head and a pressure rod. When the sample press is inserted into the sample carrier from the first open side, the pressure rod pushes the particle-enriched material to gather towards the sample cup. The particle-enriched material is pressed into a sample cake to be tested in the sample cup by the pressure head and the pressure rod.
[0012] In some optional embodiments of this application, a through channel extending along the axial direction of the sample carrier is formed in the sample collection section, and a sample receiving cavity is formed in the sample cup section. The through channel communicates with the sample receiving cavity, and the diameter of the through channel is larger than the diameter of the sample receiving cavity.
[0013] In some optional embodiments of this application, the diameter of the through channel decreases from the first open side to the second open side.
[0014] In some optional embodiments of this application, the through channel includes a narrowed section with a tapered cross-section along the axial direction of the sample carrier.
[0015] In some optional embodiments of this application, the pressure head is detachably connected to the first open side of the sample carrier.
[0016] In some optional embodiments of this application, the pressure head is connected to the sample carrier, and the tail end of the pressure rod is located inside the sample cup portion and there is a gap between it and the end of the sample cup portion located on the second open side.
[0017] In some optional embodiments of this application, the sample carrier has a circular cap formed on the first open side, the circular cap is connected to the pressure head and the connection between the two is sealed by a sealing ring, and the circular cap is connected to the portion of the sample collection part near the first open side.
[0018] In some optional embodiments of this application, the annular cap is threadedly connected to the pressure head.
[0019] In some optional embodiments of this application, a first internal thread is formed on the inner circumference of the annular cap, and a first external thread matching the first internal thread is formed on the outer circumference of the pressure head.
[0020] In some optional embodiments of this application, the pressure head and the pressure rod are integrally formed, and the pressure head has a screwing portion that protrudes axially from the annular cap head of the sample carrier.
[0021] In some optional embodiments of this application, the pressure head includes a separately disposed round cover and a tightening member. The round cover and the pressure rod are integrally formed, and the pressure rod and the round cover are coaxially disposed. A first external thread is formed on the outer periphery of the round cover. The tightening member and the round cover and the pressure rod are mated on opposite sides, so that the round cover is threadedly connected to the annular cap and the pressure rod is pressed down towards the second open side by screwing the tightening member.
[0022] In some optional embodiments of this application, a cross groove is formed on the side of the round cover opposite to the pressure rod, and the tightening member has a handle and a cross protrusion provided on the handle, with the cross groove and the cross protrusion mating together.
[0023] In some optional embodiments of this application, the sample collection part is threadedly connected to the annular limiting cap.
[0024] In some optional embodiments of this application, the outer periphery of the sample collection part is formed with a second external thread, and the inner periphery of the annular limiting cap is formed with a second internal thread that matches the second external thread.
[0025] In some optional embodiments of this application, the second external thread is fully distributed on the outer periphery of the sample collection part along the axial direction of the sample carrier. When the annular limiting cover is threadedly connected to the sample collection part, the cover body of the annular limiting cover covers the entire outer periphery of the sample collection part.
[0026] In some optional embodiments of this application, the sample collection part includes an extension section and an end section near the second open side in the axial direction of the sample carrier. A second external thread is formed on the end section. When the annular limiting cap is threadedly connected to the sample collection part, the cover body of the annular limiting cap covers the outer periphery of the end section.
[0027] Beneficial effects:
[0028] This application provides a water-based heavy metal enrichment and sample preparation device for XRF detection. During the enrichment process of the test liquid, the device connects to the enrichment bottle for in-situ collection after enrichment. After enrichment, the enriched material is collected into the sample carrier through the enrichment and sample preparation device. The enriched water flows out from the filter screen fixed by the membrane ring into the circular limiting cap, and finally, the water is discharged through the outlet. A sample cake is then prepared by the mutual compression of the sample press and the sample carrier. This water-based heavy metal enrichment and sample preparation device for XRF detection integrates the enrichment of the target analyte in the test liquid, the collection of particulate enrichment material, and the preparation of the sample cake, simplifying the experimental procedure, shortening the experimental time, and effectively improving the sensitivity of the XRF detection method. It eliminates the need for additional supporting instruments, power supplies, and vacuum pumps, simplifying the equipment requirements for XRF detection in outdoor settings, meeting the needs for rapid on-site enrichment and detection, and simplifying the detection steps. Attached Figure Description
[0029] To more clearly illustrate the technical solutions in the embodiments of this application 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 only some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0030] Figure 1 This is an overall assembly structure diagram of the water heavy metal element enrichment and sample preparation device for XRF detection in Embodiment 1 of this application;
[0031] Figure 2 This is an exploded view of the water heavy metal enrichment and sample preparation device used for XRF detection in Embodiment 1 of this application.
[0032] Figure 3 This is an exploded view from another perspective of the water heavy metal enrichment and sample preparation device used for XRF detection in Embodiment 1 of this application;
[0033] Figure 4 yes Figure 1 Schematic diagram of the cross-sectional structure along the AA direction;
[0034] Figure 5 This is an overall assembly structure diagram of the water heavy metal element enrichment and sample preparation device for XRF detection in Embodiment 2 of this application;
[0035] Figure 6 This is an exploded view from one perspective of the water heavy metal enrichment and sample preparation device used for XRF detection in Embodiment 2 of this application;
[0036] Figure 7This is an exploded view from another perspective of the water heavy metal enrichment and sample preparation device used for XRF detection in Embodiment 2 of this application;
[0037] Figure 8 yes Figure 5 A schematic diagram of the cross-sectional structure along the BB direction.
[0038] Explanation of reference numerals in the attached figures:
[0039] Sample carrier-1; First open side-a; Second open side-b; Sample collection section-11; Through channel-111; Narrowing section-1111; Second external thread-112; Extension section-113; End section-114; Sample cup section-12; Sample cavity-121; Circular cap-13; First internal thread-131; Sealing ring-14;
[0040] Membrane collar-2;
[0041] Circular limiting cap-3; Dispensing nozzle-31; Second internal thread-32;
[0042] Sample presser-4; pressure head-41; first external thread-411; tightening part-412; round cover-413; cross groove-4131; tightening part-414; handle-4141; cross protrusion-4142; pressure bar-42; spacing-c. Detailed Implementation
[0043] The technical solutions of this application will now be clearly and completely described with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of this application. Based on the embodiments of this application, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this application.
[0044] In the description of this application, it should be noted that the terms "center," "upper," "lower," "left," "right," "vertical," "horizontal," "inner," and "outer," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are used only for the convenience of describing this application and simplifying the description, and 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. Therefore, they should not be construed as limitations on this application. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and should not be construed as indicating or implying relative importance.
[0045] In the description of this application, it should be noted that, unless otherwise expressly specified and limited, the terms "installation," "connection," and "linking" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection between two components. Those skilled in the art can understand the specific meaning of the above terms in this application based on the specific circumstances.
[0046] Furthermore, the technical features involved in the different embodiments of this application described below can be combined with each other as long as they do not conflict with each other.
[0047]
Example 1
[0048] like Figures 1 to 4 As shown, this application provides a water heavy metal element enrichment and sample preparation device for XRF detection, comprising:
[0049] The sample carrier 1 is used to collect particulate enrichment material. It is cylindrical and has a first open side a and a second open side b. The sample carrier 1 includes a sample collection part 11 and a sample cup part 12. The sample collection part 11 and the sample cup part 12 are arranged sequentially from the first open side a to the second open side b in the axial direction of the sample carrier 1 and are interconnected with each other.
[0050] Membrane ring 2 is fitted around the outer periphery of sample cup 12 to fix the filter screen used for filtering liquid;
[0051] The circular limiting cover 3 is located on the second open side b. The circular limiting cover 3 is detachably connected to the sample collection part 11 and is used to fix the membrane sleeve 2. The circular limiting cover 3 itself has a liquid outlet 31 on its axial direction that corresponds to the position of the sample cup part 12.
[0052] The sample presser 4 includes a pressure head 41 and a pressure rod 42 connected together. When the sample presser 4 is inserted into the sample carrier 1 from the first open side a, the pressure rod 42 pushes the particle enriched material to gather towards the sample cup 12. The particle enriched material is pressed into a sample cake to be tested in the sample cup 12 by the pressure head 41 and the pressure rod 42.
[0053] This application provides a water-based heavy metal enrichment and sample preparation device for XRF detection. During the enrichment process of the test liquid, the device connects to the enrichment bottle for in-situ collection after enrichment. After enrichment, the enriched material is collected into the sample carrier 1 through the enrichment and sample preparation device. The enriched water flows out from the filter screen fixed by the membrane sleeve 2 into the circular limiting cap 3, and finally discharges through the outlet 31. The sample cake is then prepared by the mutual compression of the sample press 4 and the sample carrier 1. This water-based heavy metal enrichment and sample preparation device for XRF detection integrates the enrichment of the target analyte in the test liquid, the collection of particulate enrichment material, and the preparation of the sample cake, simplifying the experimental procedure, shortening the experimental time, and effectively improving the sensitivity of the XRF detection method. It eliminates the need for additional supporting instruments, power supplies, and vacuum filtration pumps, simplifying the equipment requirements for XRF detection in outdoor settings, meeting the needs for rapid on-site enrichment and detection, and simplifying the detection steps.
[0054] In some optional embodiments of this application, a through channel 111 extending along the axial direction of the sample carrier 1 is formed in the sample collection part 11, and a sample receiving cavity 121 is formed in the sample cup part 12. The through channel 111 is connected to the sample receiving cavity 121, and the diameter of the through channel 111 is larger than the diameter of the sample receiving cavity 121.
[0055] In some optional embodiments of this application, the diameter of the through channel 111 is larger than the diameter of the sample cavity 121. This can be because the diameter at all points in the through channel 111 is larger than the diameter of the sample cavity 121, or the average diameter of the through channel 111 is larger than the diameter of the sample cavity 121. This facilitates the collection of particle-enriched material into the sample cavity 121 through the through channel 111. The sample cup portion 12 is annular, similar in shape to a typical XRF detection sample cup.
[0056] In some optional embodiments of this application, the diameter of the through channel 111 decreases from the first open side a to the second open side b. In these embodiments, it is advantageous for the particulate-rich material to move rapidly along the wall of the through channel 111 and slide down into the sample chamber 121 during the collection of particulate-rich material, thereby improving collection efficiency.
[0057] In some optional embodiments of this application, the through channel 111 includes a narrowed channel section 1111 with a tapered cross section in the axial direction of the sample 1.
[0058] In some optional embodiments of this application, the pressure head 41 is detachably connected to the first open side a of the sample carrier 1. In these embodiments, when the pressure head 41 is connected to the first open side a of the sample carrier 1, pressure is applied to the particulate enrichment material located in the sample cup portion 12 of the sample carrier 1. After the pressure head 41 is detached from the sample carrier 1, it is convenient for the sample carrier 1 to collect the particulate enrichment material enriched with heavy metal elements from the enrichment bottle in the enrichment bottle.
[0059] In some optional embodiments of this application, the pressure head 41 is connected to the sample carrier 1, and the tail end of the pressure rod 42 is located inside the sample cup portion 12 and there is a gap c between it and the end of the sample cup portion 12 located on the second open side b. In these embodiments, the gap c is reserved for forming the sample cake to be tested, and the length of the gap c is approximately equal to the thickness of the sample cake to be tested.
[0060] In some optional embodiments of this application, the length of the sample cup portion 121 is greater than the length of the spacing c, which facilitates the compactor 4 to compress the particle-rich material in the sample cavity 121 for sample preparation.
[0061] In some optional embodiments of this application, the sample carrier 1 has an annular cap 13 formed on the first open side a. The annular cap 13 is connected to the pressure head 41, and the connection between the two is sealed by a sealing ring 14. The sealing ring 14 can prevent the enriched test liquid and particulate enrichment material from flowing out from the first open side a, so that the enriched test liquid flows out of the sample carrier 1 from the second open side b, and then flows out from the outlet 31 of the annular limiting cap 3. The particulate enrichment material is collected in the sample cavity 121 of the sample cup portion 12 near the second open side b.
[0062] In some optional embodiments of this application, the annular cap 13 is threadedly connected to the pressure head 41. The pressure head 41 can apply pressure to the particle enrichment material in the sample chamber 121 via the pressure rod 42 by screwing it onto the annular cap 13. The threaded connection allows for quick and easy assembly and disassembly between the annular cap 13 and the pressure head 41, which is beneficial for enrichment and tableting operations.
[0063] In some optional embodiments of this application, a first internal thread 131 is formed on the inner circumference of the annular cap 13, and a first external thread 411 matching the first internal thread 131 is formed on the outer circumference of the pressure head 41. In some examples, a sealing ring 14 is disposed inside the annular cap 13 and on the side of the first internal thread 131 facing the second open side b, so as to achieve a threaded sealing connection between the pressure head 41 and the annular cap 13.
[0064] In some optional embodiments of this application, the pressure head 41 and the pressure rod 42 are integrally formed, and the pressure head 41 has a tightening portion 412 that protrudes axially from the annular cap 13 of the sample carrier 1. In some examples, the inspector holds the tightening portion 412 and rotates the sample press 4, so that the first external thread 411 of the pressure head 41 engages with the internal thread in the annular cap 13, completing the threaded connection between the sample press 4 and the annular cap 13 of the sample carrier 1, and realizing the connection between the pressure head 41 and the first open side a of the sample carrier 1.
[0065] In some optional embodiments of this application, the sample collection part 11 is threadedly connected to the annular limiting cap 3. In these embodiments, the threaded connection between the sample collection part 11 and the annular limiting cap 3 facilitates quick and convenient fixation of the membrane sleeve 2 to the outside of the sample cup part 12.
[0066] In some optional embodiments of this application, the outer periphery of the sample collection part 11 is formed with a second external thread 112, and the inner periphery of the annular limiting cover 3 is formed with a second internal thread 32 that matches the second external thread 112.
[0067] In some optional embodiments of this application, the second external thread 112 is fully distributed on the outer periphery of the sample collection part 11 in the axial direction of the sample carrier 1. When the annular limiting cover 3 is threadedly connected to the sample collection part 11, the cover body of the annular limiting cover 3 covers the entire outer periphery of the sample collection part 11.
[0068]
Example 2
[0069] like Figure 2 As shown, this application provides a water heavy metal element enrichment and sample preparation device for XRF detection, comprising:
[0070] The sample carrier 1 is used to collect particulate enrichment material. It is cylindrical and has a first open side a and a second open side b. The sample carrier 1 includes a sample collection part 11 and a sample cup part 12. The sample collection part 11 and the sample cup part 12 are arranged sequentially from the first open side a to the second open side b in the axial direction of the sample carrier 1 and are interconnected with each other.
[0071] Membrane ring 2 is fitted around the outer periphery of sample cup 12 to fix the filter screen used for filtering liquid;
[0072] The circular limiting cover 3 is located on the second open side b. The circular limiting cover 3 is detachably connected to the sample collection part 11 and is used to fix the membrane sleeve 2. The circular limiting cover 3 itself has a liquid outlet 31 on its axial direction that corresponds to the position of the sample cup part 12.
[0073] The sample presser 4 includes a pressure head 41 and a pressure rod 42 connected together. When the sample presser 4 is inserted into the sample carrier 1 from the first open side a, the pressure rod 42 pushes the particle enriched material to gather towards the sample cup 12. The particle enriched material is pressed into a sample cake to be tested in the sample cup 12 by the pressure head 41 and the pressure rod 42.
[0074] The diameter of the through channel 111 is larger than the diameter of the sample cavity 121. This can be because the diameter of all points in the through channel 111 is larger than the diameter of the sample cavity 121, or the average diameter of the through channel 111 is larger than the diameter of the sample cavity 121. This facilitates the collection of particle-enriched material into the sample cavity 121 through the through channel 111. The sample cup portion 12 is annular, similar in shape to a typical XRF detection sample cup.
[0075] The diameter of the through channel 111 decreases from the first open side a to the second open side b. In these embodiments, it is advantageous for the particulate-rich material to move rapidly along the wall of the through channel 111 and slide down into the sample chamber 121 during the collection of particulate-rich material, thereby improving collection efficiency.
[0076] The through passage 111 includes a narrow section 1111 with a cone-shaped cross section in the axial direction of the sample 1.
[0077] In some optional embodiments of this application, the pressure head 41 is detachably connected to the first open side a of the sample carrier 1. In these embodiments, when the pressure head 41 is connected to the first open side a of the sample carrier 1, pressure is applied to the particulate enrichment material located in the sample cup portion 12 of the sample carrier 1. After the pressure head 41 is detached from the sample carrier 1, it is convenient for the sample carrier 1 to collect the particulate enrichment material enriched with heavy metal elements from the enrichment bottle in the enrichment bottle.
[0078] In some optional embodiments of this application, the pressure head 41 is connected to the sample carrier 1, and the tail end of the pressure rod 42 is located inside the sample cup portion 12 and there is a gap c between it and the end of the sample cup portion 12 located on the second open side b. In these embodiments, the gap c is reserved for forming the sample cake to be tested, and the length of the gap c is approximately equal to the thickness of the sample cake to be tested.
[0079] In some optional embodiments of this application, the length of the sample cup portion 121 is greater than the length of the spacing c, which facilitates the compactor 4 to compress the particle-rich material in the sample cavity 121 for sample preparation.
[0080] The sample carrier 1 has a circular cap 13 formed on the first open side a. The circular cap 13 is connected to the pressure head 41, and the connection between the two is sealed by a sealing ring 14. The sealing ring 14 prevents the enriched test liquid and particulate enrichment material from flowing out from the first open side a, allowing the enriched test liquid to flow out of the sample carrier 1 from the second open side b, and then out from the outlet 31 of the circular limiting cap 3. The particulate enrichment material is collected in the sample cavity 121 of the sample cup portion 12 near the second open side b.
[0081] The annular cap 13 is threadedly connected to the pressure head 41. The pressure head 41 can apply pressure to the particle enrichment material in the sample chamber 121 via the pressure rod 42 by screwing it onto the annular cap 13. The threaded connection allows for quick and easy assembly and disassembly between the annular cap 13 and the pressure head 41, which is beneficial for enrichment and tableting operations.
[0082] The inner circumference of the annular cap 13 is formed with a first internal thread 131, and the outer circumference of the pressure head 41 is formed with a first external thread 411 that matches the first internal thread 131. In some examples, the sealing ring 14 is disposed inside the annular cap 13 and on the side of the first internal thread 131 facing the second open side b, so as to achieve a threaded sealing connection between the pressure head 41 and the annular cap 13.
[0083] Unlike Embodiment 1, the pressure head 41 includes a separately disposed circular cap 413 and a tightening member 414. The circular cap 413 is integrally formed with the pressure rod 42, and the pressure rod 42 is coaxially disposed with the circular cap 413. A first external thread 411 is formed on the outer periphery of the circular cap 413. The tightening member 414 and the circular cap 413 are mated on the opposite side of the pressure rod 42, so that by screwing the tightening member 414, the circular cap 413 is threadedly connected to the annular cap 13 and the pressure rod 42 is pressed down towards the second open side b. A cross groove 4131 is formed on the opposite side of the circular cap 413 and the pressure rod 42. The tightening member 414 has a handle portion 4141 and a cross protrusion 4142 disposed on the handle portion 4141. The cross groove 4131 and the cross protrusion 4142 are mated. To form the sample cake to be tested, the granular enriched material in the sample cavity 121 needs to be compressed. Holding the round cap 413, insert the pressure rod 42 into the through channel 111, and then hold the handle 4141 of the screw-on member 414. Align the cross head 4142 with the cross groove 4131 on the round cap 413 and insert it into the cross groove 4131 to complete the male-female fit. Rotating the handle 4141 causes the round cap 413 and the pressure rod 42 to rotate together. The first external thread 411 on the outer circumference of the round cap 413 and the first internal thread 131 formed on the inner circumference of the annular cap 13 engage to complete the threaded connection.
[0084] In some optional embodiments of this application, the sample collection part 11 is threadedly connected to the annular limiting cap 3. In these embodiments, the threaded connection between the sample collection part 11 and the annular limiting cap 3 facilitates quick and convenient fixation of the membrane sleeve 2 to the outside of the sample cup part 12.
[0085] Unlike Embodiment 1, in the axial direction of the sample carrier 1, the sample collection part 11 includes an extension section 113 and an end section 114 near the second open side b. The second external thread 112 is formed on the end section 114. When the annular limiting cover 3 is threadedly connected to the sample collection part 11, the cover body of the annular limiting cover 3 covers the outer periphery of the end section 114.
[0086] The second aspect of this application provides a method for enriching and preparing heavy metal elements in water for XRF detection, using the XRF detection heavy metal element enrichment and preparation device of this application, including:
[0087] S10: Enrichment step, the first volume of particulate enrichment material is put into an open enrichment bottle containing the liquid to be tested to form a solid-liquid enrichment system. The solid-liquid enrichment system is shaken to enrich the target analyte in the liquid to be tested with particulate enrichment material. The first volume is the same as the volume of the sample chamber 121.
[0088] S20: Discharge the enriched test liquid, install the collection part of the water heavy metal element enrichment sample preparation device for XRF detection onto the mouth of the enrichment bottle. The collection part includes a sample carrier 1, a membrane sleeve ring 2 and a circular limiting cap 3. The first open side a of the sample carrier 1 corresponds to the position of the bottle mouth and is sealed. The filter screen is sealed on the opening of the sample cup 12 near the second open side b, and the edge of the filter screen is constrained by the membrane sleeve ring 2. The circular limiting cap 3 fixes the membrane sleeve ring 2. The enriched test liquid in the solid-liquid enrichment system is discharged from the enrichment bottle from the filter screen and the outlet 31 in sequence, and the particulate enrichment material is collected in the sample chamber 121 of the sample cup 12.
[0089] S30: Form the sample cake to be tested. Remove the collection part from the enrichment bottle. Insert the pressure rod 42 of the sample presser 4 into the through channel 111 from the first open side a. The tail end of the pressure rod 42 enters the sample chamber 121 through the through channel 111. The particulate enrichment material in the sample chamber 121 is squeezed by the pressure head 41 through the pressure rod 42 to form the sample cake to be tested.
[0090] In some optional embodiments of the second aspect of this application, the particulate enrichment material is particulate resin powder.
[0091] In some optional embodiments of the second aspect of this application, the first open side a of the sample carrier 1 corresponds to and is sealed to the bottle opening position, specifically by selecting a bottle opening with a first external thread 411 and a bottle opening size that matches the size of the annular cap 13. The bottle opening of the enrichment bottle can be threadedly connected to the annular cap 13, facilitating the drainage operation after enrichment.
[0092] The filter screen pore size is smaller than the particle size of the particulate enrichment material, and the membrane sleeve ring 2 fixes the filter screen to form a flat surface.
[0093] In some optional embodiments of the second aspect of this application, it further includes:
[0094] S40: Dry the sample cake to be tested. Disassemble the circular limiting cover 3 from the sample collection part 11 to expose the sample cake to be tested in the sample cavity 121. Use absorbent material to remove excess moisture from the sample cake to obtain a dry sample cake to be tested.
[0095] In some optional embodiments of the second aspect of this application, the absorbent material includes dried filter paper.
[0096] In some optional embodiments of the second aspect of this application, in step S20, the enrichment bottle is made of a compressible material, and in the step of discharging the enriched test liquid:
[0097] Squeeze the enrichment bottle so that the enriched test liquid in the enrichment bottle is squeezed out to the bottle mouth and discharged from the enrichment bottle through the filter screen.
[0098] In some optional embodiments of the second aspect of this application, the enrichment bottle is a plastic bottle. For example, it is a polyethylene (PE) plastic bottle, a polyethylene aliphatic polymer (PP) plastic bottle, a polyethylene terephthalate (PET) plastic bottle, or a polycarbonate (PC) plastic bottle.
[0099] The use of a squeezing operation combined with a filter eliminates the need to carry a vacuum pump or vacuum adsorption device, making it suitable for rapid on-site testing.
[0100] The second aspect of this application provides a method for enriching heavy metal elements in water for XRF detection. This method utilizes a granular enrichment material in a liquid sample via a shaking process, effectively improving the adsorption efficiency of the target analyte in the liquid. Furthermore, a volumetric flask with a volume proportionate to the volume of the liquid to be tested can be selected based on actual detection needs. The volume of granular enrichment material is selected according to the volume of the liquid to be tested. The enriched liquid is discharged by using a filter to intercept and collect the granular enrichment material. This process can be performed manually without the need for additional equipment. This method eliminates the limitation of traditional solid-phase extraction methods on the volume of the liquid to be tested, avoiding the need to carry solid-phase extraction devices or centrifuges for outdoor operations, and requires no power supply. Traditionally, the volume of the sample chamber 121 within the sample cup 12 is equal to the volume of the granular enrichment material used for XRF detection. Furthermore, the first open side a of the sample carrier 1 is set to correspond to the size of the bottle mouth of the enrichment bottle, which facilitates the operation when discharging the enriched test liquid and simplifies the sample preparation process and the equipment required for sample preparation.
[0101] This method eliminates the limitations of traditional solid-phase extraction (SPE) methods on the volume of the liquid to be tested, avoiding the need to carry SPE devices or centrifuges for field outdoor operations, and requires no power supply. The S10 step can process liquids ranging from tens of milliliters to several liters, achieving enrichment in approximately 10 minutes. The quality of the particulate enrichment material used is determined by the volume of the liquid to be tested; further determining the sample cup volume allows for the preparation of XRF detection heavy metal enrichment sample preparation devices of various specifications for water.
[0102] In steps S30 and S40, the steps of molding the particle-enriched material into an XRF test sample cake by pressing and drying the XRF test sample cake greatly avoid the influence of residual liquid on the measurement, while improving the stability of instrument detection and the method detection limit.
[0103] During the liquid discharge process in step S20, the use of a filter and the enrichment method of vibration greatly reduces the high pressure caused by particle powder accumulation, allowing for manual operation. Simultaneously, the collection step can be completed in approximately 1 minute (for a 100 mL water sample).
[0104] The above description is merely a specific embodiment of this application, but the scope of protection of this application is not limited thereto. Any variations or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in this application should be included within the scope of protection of this application. Therefore, the scope of protection of this application should be determined by the scope of the claims.
Claims
1. A sample preparation device for enriching heavy metal elements in water for XRF detection, characterized in that, include: A sample carrier for collecting particulate enriched material is cylindrical and has a first open side and a second open side. The sample carrier includes a sample collection part and a sample cup part, which are arranged sequentially from the first open side to the second open side in the axial direction of the sample carrier and are interconnected with each other. A membrane sleeve ring is fitted around the outer periphery of the sample cup to fix the filter screen used for filtering the liquid. A circular limiting cap is located on the second open side. The circular limiting cap is detachably connected to the sample collection part and is used to fix the membrane sleeve. The circular limiting cap itself has a liquid outlet corresponding to the position of the sample cup part in its axial direction. The sample press includes a connected pressure head and a pressure rod. When the sample press is inserted into the sample carrier from the first open side, the pressure rod pushes the particle-enriched material to gather towards the sample cup portion. The particle-enriched material is pressed into a sample cake to be tested in the sample cup portion by the pressure head and the pressure rod.
2. The water heavy metal element enrichment and sample preparation device for XRF detection according to claim 1, characterized in that, A through channel extending along the axial direction of the sample carrier is formed in the sample collection section, and a sample receiving cavity is formed in the sample cup section. The through channel is connected to the sample receiving cavity, and the diameter of the through channel is larger than the diameter of the sample receiving cavity.
3. The water heavy metal element enrichment and sample preparation device for XRF detection according to claim 2, characterized in that, The diameter of the through channel decreases from the first open side to the second open side.
4. The water heavy metal element enrichment and sample preparation device for XRF detection according to claim 2, characterized in that, The through channel includes a narrow section with a cone-shaped cross-section along the axial direction of the sample.
5. The water heavy metal element enrichment and sample preparation device for XRF detection according to claim 1, characterized in that, The pressure head is detachably connected to the first open side of the sample carrier.
6. The water heavy metal element enrichment and sample preparation device for XRF detection according to claim 5, characterized in that, The pressure head is connected to the sample carrier, and the tail end of the pressure rod is located inside the sample cup and there is a gap between it and the end of the sample cup located on the second open side.
7. The water heavy metal element enrichment and sample preparation device for XRF detection according to claim 5, characterized in that, The sample carrier has a circular cap formed on the first open side. The circular cap is connected to the pressure head, and the connection between the two is sealed by a sealing ring. The circular cap is connected to the portion of the sample collection part near the first open side.
8. The water heavy metal element enrichment and sample preparation device for XRF detection according to claim 7, characterized in that, The circular cap is threadedly connected to the pressure head.
9. The water heavy metal element enrichment and sample preparation device for XRF detection according to claim 8, characterized in that, The inner circumference of the ring cap is formed with a first internal thread, and the outer circumference of the pressure head is formed with a first external thread that matches the first internal thread.
10. The water heavy metal element enrichment and sample preparation device for XRF detection according to claim 9, characterized in that, The pressure head is integrally formed with the pressure rod, and the pressure head has a screwing part that protrudes from the annular cap head in the axial direction of the sample carrier.
11. The water heavy metal element enrichment and sample preparation device for XRF detection according to claim 9, characterized in that, The pressure head includes a separately disposed circular cap and a tightening component. The circular cap is integrally formed with the pressure rod, and the pressure rod is coaxially disposed with the circular cap. The outer circumference of the circular cap is formed with the first external thread. The tightening component and the circular cap and the pressure rod are mated on opposite sides to each other, so that by screwing the tightening component, the circular cap is threadedly connected to the annular cap and the pressure rod is pressed down toward the second open side.
12. The water heavy metal element enrichment and sample preparation device for XRF detection according to claim 11, characterized in that, A cross groove is formed on the side of the round cover opposite to the pressure rod. The tightening member has a handle and a cross protrusion provided on the handle. The cross groove and the cross protrusion are mated together.
13. The water heavy metal element enrichment and sample preparation device for XRF detection according to claim 1, characterized in that, The sample collection part is threadedly connected to the circular limiting cover.
14. The water heavy metal element enrichment and sample preparation device for XRF detection according to claim 13, characterized in that, The outer periphery of the sample collection part is formed with a second external thread, and the inner periphery of the annular limiting cap is formed with a second internal thread that matches the second external thread.
15. The water heavy metal element enrichment and sample preparation device for XRF detection according to claim 14, characterized in that, Along the axial direction of the sample carrier, the second external thread is fully distributed on the outer periphery of the sample collection part. When the annular limiting cover is threadedly connected to the sample collection part, the cover body of the annular limiting cover covers the entire outer periphery of the sample collection part.
16. The water heavy metal element enrichment and sample preparation device for XRF detection according to claim 15, characterized in that, In the axial direction of the sample carrier, the sample collection part includes an extension section and an end section near the second open side, the second external thread is formed on the end section, and when the annular limiting cap is threadedly connected to the sample collection part, the cover body of the annular limiting cap covers the outer periphery of the end section.