Device and method for separating siliceous organism shells in sediments

Through the sediment pretreatment and sedimentation graded separation device, the problem of separating various siliceous biological shells in the sediment was solved, and efficient and non-destructive sample separation and analysis were achieved, providing a convenient solution for marine scientific research.

CN120668703APending Publication Date: 2025-09-19OCEAN UNIV OF CHINA
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Patent Information

Application Number
CN202510718092.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-05-30
Publication Date
2025-09-19

AI Technical Summary

Technical Problem

Existing technologies make it difficult to efficiently separate various siliceous biological shells in sediments, especially siliceous dinoflagellates and radiolarians, and the separation process is complicated, which may lead to sample loss and property changes.

Method used

Carbonate rock and organic matter are removed by pretreatment, and a siliceous bioshell separation device in sediments with components such as a sedimentation measuring cylinder and a glass slide is used to control the sedimentation time and graded separation to achieve the separation of various siliceous bioshells.

Benefits of technology

The method achieves efficient, rapid and non-destructive separation of various siliceous biological shells. The samples can be directly used for microscopic observation and subsequent analysis, and is suitable for laboratory and field research.

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Abstract

The invention belongs to the technical field of siliceous organism separation, and discloses a device and a method for separating siliceous organism shells in sediments. The method comprises the following steps: carrying out carbonate rock and organic matter removal treatment on the sediment to obtain a to-be-separated sample of the siliceous biological shell in the sediment; loading the to-be-separated sample of the siliceous biological shell in the sediment into a device for separating the siliceous biological shell in the sediment, controlling the sediment settling time by adjusting the volume of a measuring cylinder, and carrying out sediment settling operation for multiple times; performing grading separation after operation to obtain a plurality of different particle sediments and siliceous biological shells; and carrying out scanning electron microscope analysis on the separated siliceous biological shell, and detecting the damage degree of the siliceous biological shell. According to the scheme, the loss of the sample and the damage to the siliceous shell in the operation process can be reduced, the physical and chemical properties of the siliceous biological shell cannot be changed, and the treated sample can be directly used for microscopic observation or electron microscope sample preparation and subsequent research.
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Description

Technical Field

[0001] The present invention belongs to the technical field of siliceous biological separation, and in particular relates to a device and method for separating siliceous biological shells in sediments. Background Art

[0002] Siliceous bioshells in sediments are the siliceous skeletons of marine phytoplankton (such as diatoms and diatomaceous dinoflagellates) and marine animals (such as radiolarians and siliceous sponges) that remain in the sediments after death, sedimentation, and decomposition. Their primary component is hydrated silicon dioxide (SiO2·nH2O). The composition, type, diversity, and abundance of siliceous bioshells in sediments are crucial for studying and understanding the evolution of the marine environment.

[0003] The content of siliceous bioshells in offshore sediments is approximately 1-3%, while the content in deep-sea sediments ranges more widely, from approximately 1-90%. Other major components in sediments include carbonate rocks, silicate rocks, and organic matter. Rapidly and effectively separating siliceous bioshells from complex marine sediments can improve the efficiency of research on the composition of siliceous bioshells in sediments. Existing technologies for separating siliceous bioshells from sediments primarily rely on chemical treatment, physical screening, or heavy liquid flotation, exploiting the size and density differences between siliceous bioshells and other components. This process is complex and can result in sample loss during operation, affecting subsequent measurement results. Furthermore, current technologies primarily focus on separating diatom shells or sponge spicules from sediments, but not on separating siliceous bioshells such as dinoflagellates and radiolarians, which are often more abundant in marine sediments than diatoms. Therefore, it is necessary to establish a device and method for separating multiple siliceous biological shells in sediments, so as to efficiently separate multiple siliceous biological shells in sediments during research work and use them for related scientific research and practice. Summary of the Invention

[0004] To overcome the problems existing in the related art, the disclosed embodiments of the present invention provide a device and method for separating siliceous bioshells in sediments.

[0005] The technical solution is as follows: A method for separating siliceous bioshells from sediments, comprising:

[0006] S1, removing carbonate rocks and organic matter from the sediment to obtain a sample of siliceous biological shells to be separated from the sediment;

[0007] S2, placing the sample of siliceous bioshells to be separated from the sediment into a siliceous bioshell separation device in sediment, adjusting the volume of the graduated cylinder, controlling the sediment settling time, and performing sediment settling operations multiple times; after the operations, a plurality of different particle sediments and siliceous bioshells are obtained by fractionation and separation;

[0008] S3, performing scanning electron microscopy analysis on the separated siliceous bioshell to detect the degree of damage to the siliceous bioshell.

[0009] In step S1, the carbonate and organic matter removal treatment of the sediment includes:

[0010] First, the sediment was weighed and placed in a plastic centrifuge tube. The sediment was treated with hydrochloric acid to remove the carbonate rocks in the sediment.

[0011] Then, sodium alkylbenzene sulfonate and hydrogen peroxide were added to disperse the particles in the sediment and remove the organic matter in the sediment. After standing at room temperature, the mixture was shaken with an ultrasonic shaker. The test tube was placed in a centrifuge and the supernatant was removed.

[0012] Finally, deionized water was added to the centrifuge tube, and after being thoroughly mixed with the sediment, the centrifugation was continued and the supernatant was removed. Deionized water was added to the remaining mixture of sediment and deionized water, and mixed evenly.

[0013] In step S2, the sample of siliceous bioshells to be separated from the sediment is placed in a siliceous bioshell separation device. By adjusting the volume of the graduated cylinder, controlling the sedimentation time, and performing multiple sedimentation operations, a variety of different particle sediments and siliceous bioshells are obtained through fractional separation after the operation, including:

[0014] Assemble the water tank, glass slide, and sedimentation measuring cylinder in sequence, add the sample in the centrifuge tube to the sedimentation measuring cylinder, rinse the centrifuge tube with deionized water, transfer the sample in the centrifuge tube to the sedimentation measuring cylinder, and cover it with a cover glass. After the sample has been allowed to rest, move the sedimentation measuring cylinder so that the solution in it flows into the water tank through the mixed solution outflow hole. The silicate rock with high density will first settle on the glass slide and be separated and removed.

[0015] Add the sample in the water tank back into the sedimentation measuring cylinder equipped with a new slide, let it stand, and repeat the above steps to separate the fine-grained sediment with high sediment density; then continue to transfer the sample in the sedimentation measuring cylinder to the water tank, and then add it to the sedimentation measuring cylinder equipped with a new slide, let it stand, and obtain the siliceous biological shells in the sediment.

[0016] Furthermore, if the sediment is deep-sea sediment, the sedimentation time will be extended.

[0017] Furthermore, the sedimentation measuring cylinder is equipped with an accessory measuring cylinder to increase the sedimentation time according to usage requirements.

[0018] Another object of the present invention is to provide a device for separating siliceous biological shells in sediments, which is used to separate siliceous biological shells in sediments. The device comprises:

[0019] The cover glass is placed on the top of the accessory measuring cylinder to seal the accessory measuring cylinder. The accessory measuring cylinder is inserted into the sedimentation measuring cylinder. The slide glass is placed at the bottom of the sedimentation measuring cylinder to carry the settled sediment and siliceous biological shells. The water tank is placed at the bottom of the slide glass. The sedimentation measuring cylinder is filled with a mixed solution of the sample; the slide glass is provided with a hole for the mixed solution to flow out.

[0020] Furthermore, the device for separating siliceous biological shells in sediments is used to separate siliceous biological shells of siliceous dinoflagellates in sediments.

[0021] Furthermore, the device for separating siliceous biological shells in sediments is used to separate siliceous biological shells of radiolarians.

[0022] Furthermore, the device for separating siliceous biological shells in sediments is used to separate diatom siliceous biological particles.

[0023] Furthermore, the device for separating siliceous biological shells in sediments is used to separate siliceous biological particles from sponge spicules.

[0024] In combination with all the above technical solutions, the beneficial effects of the present invention are as follows:

[0025] First, the present invention effectively separates siliceous bioshells from sediments through sediment pretreatment, settling, and fractionation, enabling subsequent compositional analysis (type, diversity, and content). This approach reduces sample loss and damage to the siliceous bioshells during operation, without altering their physical and chemical properties. The treated samples can be directly used for microscopic observation, electron microscopy sample preparation, and subsequent research, providing a solution for the efficient, convenient, and rapid separation of siliceous bioshells from nearshore and deep-sea sediments.

[0026] The present invention can be used to separate siliceous bioshells from marine sediments. Its advantages are that the sediment settling time can be controlled by regulating the sample settling height; sediments of different densities can be graded and separated; the physical and chemical properties of the siliceous bioshells are not changed; and the device is easy to assemble and carry, and can be used in the laboratory as well as for the collection and pretreatment of field samples.

[0027] Second, the device for separating siliceous bioshells from sediments, as converted by the present invention's technical solution, can be used as a standardized product to serve researchers in disciplines such as marine science, marine resources and environment, marine technology, paleoclimate, and paleoceanography, thus possessing high commercial value. Furthermore, the present invention's technical solution, after conversion, can improve related work efficiency, thus possessing high scientific research value. Furthermore, the successful authorization of the present invention's technical solution will facilitate the intellectual property protection and subsequent industrialization of the product.

[0028] The technical solution of the present invention fills the gap in the current standardized device for separating siliceous biological shells in sediments and the gap in the method for efficiently analyzing various siliceous biological shells such as diatoms, diatomaceous flagellates, radiolarians and sponge spicules in sediments.

[0029] Third, the technical solution of the present invention addresses the technical difficulties of easily losing siliceous bioshells and damaging their structure during the separation process. Due to technical and methodological limitations, previous studies have focused solely on separating a single type of siliceous bioshell. The technical solution of the present invention overcomes the technical difficulties of separating multiple siliceous bioshells from sediments, enabling rapid and efficient separation of multiple siliceous bioshells. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the present disclosure and, together with the description, serve to explain the principles of the present disclosure;

[0031] Figure 1 Schematic diagram of a device for separating siliceous biological shells from sediments provided by an embodiment of the present invention;

[0032] Figure 2 is a schematic diagram of a cover glass provided by an embodiment of the present invention;

[0033] Figure 3 is a schematic diagram of a glass slide provided by an embodiment of the present invention;

[0034] Figure 4 Schematic diagram of a sedimentation measuring cylinder provided in an embodiment of the present invention;

[0035] Figure 5 Schematic diagram of an accessory graduated cylinder provided by an embodiment of the present invention;

[0036] Figure 6 is a schematic diagram of a water tank provided by an embodiment of the present invention;

[0037] Figure 7 This is a schematic diagram of the assembly principle of the device for separating siliceous biological shells in sediments provided by an embodiment of the present invention;

[0038] Figure 8 This is a flow chart of a method for separating siliceous bioshells from sediments provided by an embodiment of the present invention;

[0039] Figure 9 This is a scanning electron microscope image of siliceous bioshells obtained by treating sediments with the device for separating siliceous bioshells from sediments provided by an embodiment of the present invention;

[0040] In the figure: 1. Cover glass; 2. Slide; 3. Sedimentation measuring cylinder; 4. Accessory measuring cylinder; 5. Water tank; 6. Mixed solution outflow hole. DETAILED DESCRIPTION

[0041] To make the above-mentioned objects, features, and advantages of the present invention more readily apparent, specific embodiments of the present invention are described in detail below with reference to the accompanying drawings. The following description sets forth numerous specific details to facilitate a full understanding of the present invention. However, the present invention can be implemented in many other ways than those described herein, and those skilled in the art may make similar modifications without departing from the scope of the present invention. Therefore, the present invention is not limited to the specific embodiments disclosed below.

[0042] The innovations of this invention lie in its ability to separate a variety of siliceous bioshells, including diatoms, diatom dinoflagellates, radiolarians, and sponge spicules, from sediments. The invention allows for the adjustment of the graduated cylinder volume and control of sediment settling time to grade and separate different particles. It does not involve high-temperature or screening treatments, and does not alter the physical and chemical properties of the siliceous bioshells in the sediments. The treated samples, placed on a glass slide, can be directly used for microscopic observation and subsequent analysis and research, including species identification and dimensional measurement. The invention is easy to assemble and carry, making it suitable for use in laboratories, the field, and research vessels. It also minimizes sample loss during operation and does not damage the physical structure of the siliceous bioshells.

[0043] Example 1, as Figures 1-6 As shown, the device for separating siliceous biological shells from sediments provided by the embodiment of the present invention includes: a cover glass 1, a glass slide 2, a sedimentation measuring cylinder 3, an accessory measuring cylinder 4 and a water tank 5. The assembly process of the device is as follows: Figure 7 shown.

[0044] The cover glass 1 is placed on top of the accessory measuring cylinder 4 to seal it. The measuring cylinder 4 is plugged into the sedimentation measuring cylinder 3. The slide glass 2 is placed at the bottom of the sedimentation measuring cylinder 3 to support the settled sediment and siliceous biological shells. The water tank 5 is placed at the bottom of the slide glass 2 to hold the sample in the sedimentation measuring cylinder 3 and serves as the base of the entire device. The sedimentation measuring cylinder 3 contains a mixed solution of the sample; the slide glass 2 has a hole 6 for the mixed solution to flow out.

[0045] Example 2, as Figure 8 As shown, the method for separating siliceous biological shells from sediments provided by the embodiment of the present invention includes:

[0046] S1, removing carbonate rocks and organic matter from the sediment to obtain a sample of siliceous biological shells to be separated from the sediment;

[0047] S2, placing the sample of siliceous bioshells to be separated from the sediment into a siliceous bioshell separation device in sediment, adjusting the volume of the graduated cylinder, controlling the sediment settling time, and performing sediment settling operations multiple times; after the operations, a plurality of different particle sediments and siliceous bioshells are obtained by fractionation and separation;

[0048] S3, performing scanning electron microscopy on the separated siliceous bioshell to detect the degree of damage to the siliceous bioshell.

[0049] For example, in step S1, the removal of carbonate and organic matter from sediments includes:

[0050] About 10 mg of sediment was weighed using a balance and placed in a 15 mL plastic centrifuge tube. The sediment was treated with 1 mol / L hydrochloric acid (1 mL) to remove the carbonate rocks in the sediment.

[0051] Then, 0.5 g / L sodium alkylbenzene sulfonate (4 mL) and 5 mL of 30% hydrogen peroxide were added to disperse the particulate matter in the sediment and remove the organic matter in the sediment. After standing at room temperature for 30 minutes, the test tube was shaken with an ultrasonic shaker for 3 minutes, and then the test tube was placed in a centrifuge (3000 rpm) for 3 minutes, and 9 mL of supernatant in the centrifuge tube was removed.

[0052] Add 9 mL of deionized water to the centrifuge tube and mix thoroughly with the sediment. Continue centrifugation and remove 9 mL of supernatant. Repeat this step twice to remove residual hydrochloric acid, hydrogen peroxide, and sodium alkylbenzene sulfonate. Add 14 mL of deionized water to the remaining 1 mL of sediment and deionized water mixture and mix thoroughly.

[0053] Exemplarily, in step S2, the sample of siliceous biological shells to be separated from the sediment is placed in a siliceous biological shell separation device in sediments. By adjusting the volume of the graduated cylinder, controlling the sedimentation time, and performing multiple sedimentation operations, a plurality of different particle sediments and siliceous biological shells are obtained through fractional separation after the operation, including:

[0054] Assemble the water tank 5, glass slide 2, and sedimentation cylinder 3 in sequence. Add 15 mL of the sample from the centrifuge tube to the sedimentation cylinder 3, rinse the centrifuge tube with 5 mL of deionized water, transfer the sample from the centrifuge tube to the sedimentation cylinder 3, and cover with a coverslip 1. After the sample has rested for 10 minutes, move the sedimentation cylinder 3 so that the solution within it flows into the water tank 5 through the mixed solution outflow hole 6. The denser silicate rocks settle on the glass slide 2 (this step separates the silicate rocks from the larger sediment particles in the sediment) and are removed. The sample from the water tank 5 is re-added to the sedimentation cylinder 3 equipped with a new glass slide 2. After resting for 30 minutes, repeat the above steps to separate the sediment particles from the denser, finer sediment particles. The sample from the sedimentation cylinder 3 is then transferred to the water tank 5 and then added to the sedimentation cylinder 3 equipped with a new glass slide 2. After resting for 3 hours, the siliceous bioshells in the sediment are obtained. If the sediment is deep-sea sediment, extend the sedimentation time in this step to 5 hours. The sample on slide 2 can be directly used for microscopic observation. The fractionation step in this method can be adjusted to increase the number of fractions or extend the sedimentation time, depending on the application. During the fractionation process of the present invention, deionized water can be added to maintain the liquid scale in the sedimentation cylinder level with the cylinder. The present invention includes an accessory graduated cylinder 4, which can be added as needed to increase sediment settling time and improve the efficiency of separating siliceous bioshells from other sediment components.

[0055] In the above embodiments, the description of each embodiment has its own focus. For parts that are not described or recorded in detail in a certain embodiment, reference can be made to the relevant description of other embodiments.

[0056] To further illustrate the effects of the embodiments of the present invention, the following experiments were conducted.

[0057] The present invention utilizes the difference in the settling rate of particles in the sediment to grade and separate the siliceous biological shells ( Figure 9 The various parts of the device can be disassembled and assembled, and the sedimentation cylinders can be stacked to increase the sedimentation distance.

[0058] The present invention first pre-treats the sediment to remove carbonate rocks and organic matter and disperses particles in the sediment by adding a surfactant.

[0059] The treated sediment is washed and diluted before being placed in a pre-installed device. By controlling the settling time, the solution is transferred and repeated in stages, ultimately yielding multiple slides containing silicate rocks, siliceous bioshells, and more.

[0060] The device and method are applicable to offshore, open ocean and freshwater (such as river and lake) sediments, and can also be used for water samples (for separating siliceous organisms in water bodies: such as planktonic diatoms, radiolarians in the ocean, etc.).

[0061] The device causes little damage to the silicon shell during operation ( Figure 9 This is a scanning electron microscope image of a siliceous biological shell obtained by treating sediment using the device and method of the present invention. Figure 9 Figure A shows diatoms, Figure B shows diatoms and diatom dinoflagellates, Figure C shows sponge spicules of various shapes, and Figure D shows radiolarians. The existing device (CN201911177169) primarily focuses on processing phytoplankton and diatom samples in water, but is less applicable to complex systems like sediments (which have more complex compositions, a wide variety of siliceous bioshells with low net content, the presence of multiple minerals, or variable particle sizes). The device of the present invention can be used to separate different siliceous bioshells from various types of sediment, offering a wider range of applications.

[0062] The above description is only a preferred specific implementation method of the present invention, but the scope of protection of the present invention is not limited thereto. Any modifications, equivalent substitutions and improvements made by any technician familiar with this technical field within the technical scope disclosed by the present invention and within the spirit and principles of the present invention should be covered by the scope of protection of the present invention.

Claims

1. A method for separating siliceous bioshells from sediments, characterized in that: The method includes: S1, removing carbonate rocks and organic matter from the sediment to obtain a sample of siliceous biological shells to be separated from the sediment; S2, placing the sample of siliceous bioshells to be separated from the sediment into a siliceous bioshell separation device in sediment, adjusting the volume of the graduated cylinder, controlling the sediment settling time, and performing sediment settling operations multiple times; after the operations, a plurality of different particle sediments and siliceous bioshells are obtained by fractionation and separation; S3, performing scanning electron microscopy analysis on the separated siliceous bioshell to detect the degree of damage to the siliceous bioshell.

2. The method for separating siliceous bioshells from sediments according to claim 1, wherein: In step S1, the carbonate and organic matter removal treatment of the sediment includes: First, the sediment was weighed and placed in a plastic centrifuge tube. The sediment was treated with hydrochloric acid to remove the carbonate rocks in the sediment. Then, sodium alkylbenzene sulfonate and hydrogen peroxide were added to disperse the particles in the sediment and remove the organic matter in the sediment. After standing at room temperature, the mixture was shaken with an ultrasonic shaker. The test tube was placed in a centrifuge and the supernatant was removed. Finally, deionized water was added to the centrifuge tube, and after being thoroughly mixed with the sediment, the centrifugation was continued and the supernatant was removed. Deionized water was added to the remaining mixture of sediment and deionized water, and mixed evenly.

3. The method for separating siliceous bioshells from sediments according to claim 1, wherein: In step S2, the sample of siliceous bioshells to be separated from the sediment is placed in a siliceous bioshell separation device. By adjusting the volume of the graduated cylinder, controlling the sedimentation time, and performing multiple sedimentation operations, a variety of different particle sediments and siliceous bioshells are obtained through fractional separation after the operation, including: Assemble the water tank, glass slide, and sedimentation measuring cylinder in sequence, add the sample in the centrifuge tube to the sedimentation measuring cylinder, rinse the centrifuge tube with deionized water, transfer the sample in the centrifuge tube to the sedimentation measuring cylinder, and cover it with a cover glass. After the sample has been allowed to rest, move the sedimentation measuring cylinder so that the solution in it flows into the water tank through the mixed solution outflow hole. The silicate rock with high density will first settle on the glass slide and be separated and removed. Add the sample in the water tank back into the sedimentation measuring cylinder equipped with a new slide, let it stand, and repeat the above steps to separate the fine-grained sediment with high sediment density; then continue to transfer the sample in the sedimentation measuring cylinder to the water tank, and then add it to the sedimentation measuring cylinder equipped with a new slide, let it stand, and obtain the siliceous biological shells in the sediment.

4. The method for separating siliceous bioshells from sediments according to claim 1, wherein: If the sediment is deep sea sediment, the sedimentation time will be extended.

5. The method for separating siliceous bioshells from sediments according to claim 1, wherein: The sedimentation measuring cylinder is equipped with an accessory measuring cylinder to increase the sedimentation time according to usage requirements.

6. A device for separating siliceous bioshells from sediments, characterized in that: The device is used to separate siliceous bioshells from sediments according to any one of claims 1 to 5, and comprises: A cover glass (1) is placed on the top of an accessory measuring cylinder (4) to seal the accessory measuring cylinder (4). The accessory measuring cylinder (4) is plugged into a sedimentation measuring cylinder (3). A slide glass (2) is placed at the bottom of the sedimentation measuring cylinder (3) to carry settled sediment and siliceous biological shells. A water tank (5) is placed at the bottom of the slide glass (2). The sedimentation measuring cylinder (3) is filled with a mixed solution of a sample. A mixed solution outflow hole (6) is opened on the slide glass (2).

7. The device for separating siliceous biological shells in sediments according to claim 6, characterized in that: The device for separating siliceous biological shells in sediments is used for separating siliceous biological shells of siliceous dinoflagellates in sediments.

8. The device for separating siliceous biological shells in sediments according to claim 6, characterized in that: The device for separating siliceous biological shells in sediments is used for separating siliceous biological shells of radiolarians.

9. The device for separating siliceous biological shells in sediments according to claim 6, characterized in that: The device for separating siliceous biological shells in sediments is used for separating diatom siliceous biological particles.

10. The device for separating siliceous biological shells in sediments according to claim 6, characterized in that: The device for separating siliceous biological shells in sediments is used for separating siliceous biological particles of sponge spicules.

Citation Information

Patent Citations

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    CN110987589B