CN113941384B

CN113941384B - Capsule type secondary centrifuge tube capable of being applied to rapid nondestructive analysis

Info

Publication number: CN113941384B
Application number: CN202111381378.7A
Authority: CN
Inventors: 朱文文; 郁川; 柴骏; 孙风俭
Original assignee: Luoyang Vocational and Technical College
Current assignee: Luoyang Vocational and Technical College
Priority date: 2021-11-21
Filing date: 2021-11-21
Publication date: 2022-11-01
Anticipated expiration: 2041-11-21
Also published as: CN113941384A

Abstract

The invention discloses a capsule type secondary centrifuge tube applicable to rapid nondestructive analysis, which comprises a columnar tube body, wherein a hollow bottom joint for sealing the columnar tube body is arranged outside the columnar tube body, a solid bottom joint for sealing the columnar tube body together with the hollow bottom joint is arranged outside the columnar tube body, external threads are arranged on one side of the columnar tube body, internal threads matched with the external threads are arranged inside the solid bottom joint and the hollow bottom joint, a solid bottom is arranged inside the solid bottom joint, and a filter membrane for filtering heavy metals in water body solution inside the columnar tube body and heavy metals in suspended particles is arranged on one side of the solid bottom. The method is simple to operate, does not need complex technical procedures, effectively saves the field emergency detection and analysis time of a large number of samples, and improves the working efficiency.

Description

Capsule type secondary centrifuge tube capable of being applied to rapid nondestructive analysis

Technical Field

The invention relates to the technical field of laboratory rapid analysis, in particular to a capsule type secondary centrifugal tube capable of being applied to rapid nondestructive analysis.

Background

The centrifugation method is one of the most common sample pretreatment methods in laboratories, is commonly used in chemical laboratories, biological laboratories and life science laboratories, and is used as one of the technical means for sample separation, enrichment, preparation and the like. The centrifugal technology mainly depends on different sedimentation coefficients of different substances, and achieves the purpose of substance separation under the action of a certain centrifugal force, and the most common application is sample solid-liquid separation operation. Compared with solid-liquid separation operations such as filtration and standing, the centrifugal method is widely applied to scientific research and production in industries such as biology, medicine, agriculture, bioengineering, biopharmaceutical and the like, especially in the fields of chemical analysis and pharmaceutical analysis due to convenient and rapid operation, good separation effect and convenient and easily-obtained required equipment.

In actual scientific research work, with increasingly prominent environmental problems, in order to deal with sudden heavy metal pollution events, a rapid quantitative analysis technology for on-site heavy metals needs to be developed. For a solid sample with a smooth surface, a handheld X-ray fluorescence spectrometer can complete signal response determination within 1 minute, and synchronous quantitative analysis of multiple metal parameters is realized, so that the device is widely applied to the fields of smelting, metal manufacturing, machining manufacturing, mineral deposit detection and the like. For collected environmental water samples, the content of heavy metals in a solution needs to be measured and the content information of the heavy metals in suspended particles needs to be known. If the X-ray fluorescence spectrometer is used for realizing the determination requirements, in the conventional operation, a fixed volume of an acquired environmental water sample is generally taken for field filtration, suspended particulate matters are intercepted on a filter membrane, and the filter membrane is taken for analysis by using the handheld X-ray fluorescence spectrometer, so that the content of heavy metals in the suspended particulate matters can be determined; meanwhile, adding an alkaline solution into the filtered water sample to enable metal in the solution to react with alkali to generate precipitate, filtering again, and analyzing by using a handheld X-ray fluorescence spectrometer to obtain the content of heavy metal in the water body. Although this operation can realize the detection objective, when nevertheless filtering turbid environment water sample, because the great water sample filter speed of turbidity is very slow, and whole operation need carry out twice and filter, under the more condition of sample size, need longer analysis time. Compared with filtration, centrifugation has the advantages of convenience, rapidness, good separation effect and the like. If the centrifugal method can be used for replacing filtration, the time for analyzing the sample can be greatly saved, and the working efficiency is improved.

The centrifugal tubes are used as common experiment consumables in a laboratory, are more in types and can be divided into large-volume centrifugal tubes, macro centrifugal tubes and micro centrifugal tubes according to capacity; according to the shape of the bottom of the centrifuge tube, the centrifuge tube can be divided into a pointed-bottom centrifuge tube, a flat-bottom centrifuge tube and a round-bottom centrifuge tube; according to the closing mode of the centrifugal tube cover, the centrifugal tube cover is divided into a gland type and a spiral type; and can be divided into plastic centrifuge tubes, stainless steel centrifuge tubes, etc. according to the material. However, in the above-mentioned analysis of the turbid environment water sample, a solid-liquid separation operation is performed using a currently commercially available centrifuge tube, and after centrifugation, the clear liquid is located at the upper part, and the suspended particles settle at the bottom of the centrifuge tube. After the supernatant is poured out, the solid at the bottom of the centrifugal tube is difficult to take out, the conditions that the sample is damaged and polluted are inevitable in the taking-out process, and even if the solid is taken out smoothly, the taken-out solid cannot be analyzed and measured by using an X-ray fluorescence spectrometer because the surface of the taken-out solid is uneven. And after alkaline solution is added into the poured supernatant to enable the metal in the solution to react with alkali to generate precipitate, the precipitate still needs to be filtered, and then can be analyzed by using a handheld X-ray fluorescence spectrometer. By doing so, the analysis operation time cannot be saved, but an unpredictable pollution risk is introduced to the analysis operation. Therefore, the centrifugal tube which can be applied to rapid nondestructive analysis is urgently needed to be designed, and the working efficiency is improved.

Disclosure of Invention

The invention aims to provide a capsule type secondary centrifugal tube applicable to rapid nondestructive analysis, so as to solve the problems in the background technology.

In order to achieve the purpose, the invention provides the following technical scheme: the utility model provides a can be applied to quick nondestructive analysis's capsule type secondary centrifuging tube, includes the column body, the outside of column body is equipped with the hollow bottom head that is used for sealed column body, the outside of column body is equipped with and carries out the solid bottom head that seals with hollow bottom head jointly to the column body, one side of column body is equipped with the external screw thread, solid bottom head all is equipped with the internal thread identical with the external screw thread with the inside of hollow bottom head, the inside of solid bottom head is equipped with at the bottom of the solid, one side at the bottom of the solid is equipped with the filter membrane that is arranged in filtering heavy metal in the inside water solution of column body and the heavy metal in the suspended particles thing.

Preferably, the outside of column body is equipped with the centrifugal sleeve that is used for loading the centrifuging tube in the centrifuge, centrifugal sleeve's inside is equipped with carries out extruded spacing subassembly to column body surface, spacing subassembly is including being located the inside turning block of centrifugal sleeve, centrifugal sleeve's inside is equipped with the confession turning block pivoted spacing groove, the inside of turning block is equipped with pivot one, the turning block includes inclined plane portion.

Preferably, one side of inclined plane portion is equipped with the centrifuging tube that carries out the lifting to the inside centrifugal sleeve and pops out the subassembly, pop out the subassembly including being located the inside stripper plate of centrifugal sleeve, one side of stripper plate is equipped with the supplementary piece that supplementary stripper plate pressed, the stripper plate can freely slide from top to bottom in the inside of centrifugal sleeve, one side of stripper plate is equipped with the connecting block, the inside of connecting block is equipped with pivot two, the outside of pivot two is equipped with the rotor plate, the inside of rotor plate is equipped with pivot three, one side of rotor plate is equipped with the connecting plate, one side of connecting plate is equipped with carries out the cambered plate that supports solid bottom end joint bottom.

Preferably, one side of the rotating block is shaped like an arc, and in the process that the cylindrical pipe body is inserted into the centrifugal sleeve, the arc part of the rotating block is in contact with the cylindrical pipe body.

Preferably, the cambered surface of the cambered plate is matched with the bottom cambered surface of the solid bottom joint.

Preferably, the solid bottom comprises a convex part, the filter membrane comprises a concave part, and one side of the convex part of the solid bottom is shaped to be matched with the shape of the concave part of the filter membrane.

Preferably, the columnar pipe body, the hollow bottom joint and the solid bottom joint are all made of polytetrafluoroethylene or polypropylene.

The invention has at least the following beneficial effects:

the invention provides a capsule type secondary centrifugal tube capable of being applied to rapid nondestructive analysis. And the operation is simple, and complex technical procedures are not needed. The device can be applied to the research of the water environment heavy metal emergency rapid monitoring and analyzing method combining centrifugation and a handheld X-ray fluorescence spectrometer, a solid sample with a flat surface is rapidly obtained through centrifugation operation, nondestructive analysis is carried out by using the handheld X-ray fluorescence spectrometer, and the rapid determination of the content of heavy metals in the environment water solution and the content of heavy metals in suspended particles is realized. The field emergency detection and analysis time of a large number of samples is effectively saved, and the working efficiency is improved. Provides technical support for rapid detection of sudden water body heavy metal pollution.

Drawings

FIG. 1 is a partial schematic view of the structure of the present invention;

FIG. 2 is a partial cross-sectional view of the present invention;

FIG. 3 is a partial sectional view of the present invention;

FIG. 4 is a schematic structural view of the present invention;

FIG. 5 is a cross-sectional view of the pop-up assembly of the present invention;

FIG. 6 is a cross-sectional view of the pop-up assembly of the present invention;

FIG. 7 is an enlarged view of the structure of area A of FIG. 5 according to the present invention;

FIG. 8 is an enlarged view of the region B in FIG. 6 according to the present invention.

In the figure: 1-a cylindrical pipe body; 2-hollow bottom joint; 3-solid bottom joint; 4-solid bottom; 5-a filter membrane; 6-external thread; 7-internal threads; 8-a limiting component; 9-a pop-up assembly; 10-a centrifugal sleeve; 41-a boss; 51-a recess; 81-limiting groove; 82, a first rotating shaft; 83-turning block; 831-inclined plane part; 91-extruding a plate; 92-a connecting block; 93-a second rotating shaft; 94-a rotating plate; 95-rotating shaft III; 96-connecting plate; 97-arc panel; 98-auxiliary blocks.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Referring to fig. 1-8, the present invention provides a technical solution: the utility model provides a can be applied to quick nondestructive analysis's capsule type secondary centrifuging tube, includes column body 1, the outside of column body 1 is equipped with the hollow bottom head 2 that is used for sealed column body 1, the outside of column body 1 is equipped with and carries out sealed solid bottom head 3 to column body 1 jointly with hollow bottom head 2, one side of column body 1 is equipped with external screw thread 6, solid bottom head 3 all is equipped with the internal thread 7 identical with external screw thread 6 with the inside of hollow bottom head 2, and solid bottom head 3 and hollow bottom head 2 are located the both ends of column body 1 respectively, and all with 1 threaded connection of column body, the inside of solid bottom head 3 is equipped with at the bottom of the solid 4, and one side and 3 fixed connection of solid bottom head of the bottom of the solid 4, one side at the bottom of the solid 4 is equipped with the filter membrane 5 that is arranged in filtering heavy metal and the suspended particles in the 1 inside water solution of column body 1.

Before centrifugal operation is started, the hollow bottom connector 2 of the centrifugal tube is quickly connected with one end of the columnar tube body 1 through threads, and the connected shape is consistent with that of a common centrifugal tube. And (4) adding the collected environmental water sample into the connected centrifugal tube in a fixed volume. A filter membrane 5 with a diameter of 25mm is placed at the platform of the inner solid bottom 4 of the solid bottom joint 3 in the device. And then the solid bottom connector 3 is quickly connected with the other end of the columnar pipe body 1. The solid bottom adapter 3 here functions similarly to the cap of a conventional centrifuge tube.

After the connection is completed, the centrifuge tube is placed in a centrifuge upside down, namely the solid bottom connector 3 is positioned at the bottom of the centrifuge tube, the hollow bottom connector 2 is positioned at the top of the centrifuge tube, and the hollow bottom connector 2 has a function similar to that of a tube cover of a common centrifuge tube. The benefit of preceding two-step operation is because the inside of solid end fitting 3 is solid, leads to the whole inside volume of centrifuging tube to diminish, so the operation then can avoid the inside volume that leads to diminishes owing to solid end fitting 3, effectively guarantees the volume of centrifugation sample.

And (3) starting the centrifugal machine to carry out centrifugal operation, completing solid-liquid separation of suspended particles in the water body sample under the action of centrifugal force, and storing the suspended particles on a built-in filter membrane 5 of a platform at the bottom of the solid bottom joint 3. At the moment, the centrifugal tube is taken out, the solid bottom connector 3 is turned upside down again, the solid bottom connector 3 is unscrewed, the built-in filter membrane 5 is taken out, the filter membrane 5 already contains suspended particles and is flat in surface, and the content information of the heavy metals in the suspended particles can be obtained by directly irradiating the filter membrane by using the handheld X-ray fluorescence spectrometer. And the sample is not destroyed and can be stored for other parameter analysis.

A new filter membrane 5 with a diameter of 25mm is again placed on the solid bottom 4 platform of the solid bottom adapter 3. And adding a certain volume of alkaline solution into the centrifuged solution, wherein the alkaline solution reacts with metal ions in the centrifuged sample to generate flocculent precipitate. Then the solid bottom joint 3 with the new filter membrane 5 is quickly connected with the other end of the columnar pipe body 1.

After the connection is completed, the centrifuge tube is placed in the centrifuge upside down again, i.e. the solid bottom sub 3 is located at the bottom of the centrifuge tube and the hollow bottom sub 2 is located at the top of the centrifuge tube.

And (4) starting the centrifuge again to carry out secondary centrifugation operation, completing solid-liquid separation on the flocculent precipitate generated by the reaction of the metal ions in the water sample and the alkaline solution under the action of centrifugal force, and storing the flocculent precipitate on the built-in filter membrane 5 of the platform at the bottom of the solid bottom joint 3. The foregoing operation steps are repeated. Taking out the centrifuge tube, turning upside down again to make the solid bottom joint 3 face upwards, unscrewing the solid bottom joint 3, taking out the built-in filter membrane 5, obtaining the content information of the heavy metal in the flocculation precipitation by directly using the irradiation of the handheld X-ray fluorescence spectrometer, and obtaining the content of the heavy metal in the solution by volume conversion.

Through the operation, the content information of the heavy metals in the environmental water sample solution and the heavy metals in the suspended particles can be quickly obtained, and the quick monitoring and analysis of the emergency property of the heavy metals in the water environment can be realized. The whole operation process is short in time consumption, simple to operate and good in separation effect, the field emergency detection and analysis time of a large number of samples can be effectively saved, and the working efficiency is improved. Provides technical support for rapid detection of sudden water body heavy metal pollution.

The outside of column body 1 is equipped with the centrifugal sleeve 10 that is used for loading the centrifuging tube in the centrifuge, the inside of centrifugal sleeve 10 is equipped with and carries out extruded spacing subassembly 8 to column body 1 surface, spacing subassembly 8 is including being located the turning block 83 that a plurality of intervals inside centrifugal sleeve 10 are equal, the inside of centrifugal sleeve 10 is equipped with a plurality of confessions turning block 83 pivoted spacing groove 81, the inside of turning block 83 is equipped with pivot 82, the both ends of pivot 82 all with centrifugal sleeve 10 fixed connection, turning block 83 rotates with pivot 82 and is connected, turning block 83 includes inclined plane portion 831, and the self material of turning block 83 is for having certain elastic rubber, inserts centrifugal sleeve 10's in-process at the centrifuging tube that the experimenter will be equipped with the detection water sample, and one side of solid bottom head 3 will contact with turning block 83 earlier, under the elastic action of turning block 83 self, and turning block 83 will be to the inside shrink of spacing groove 81 until turning block 83 crosses solid bottom head 3 completely, and rebound and each orientation to column body 1 carries out extrusion to each solid orientation this moment, and extrusion bottom head 3 when the centrifuge increases the inside stability of each column body, and the centrifuge, and slide to each other at this moment, and go on the centrifuge.

One side of inclined plane portion 831 is equipped with and carries out the pop-up subassembly 9 that lifts to the inside centrifuging tube of centrifugal sleeve 10, pop-up subassembly 9 is including being located the inside stripper plate 91 of centrifugal sleeve 10, one side of stripper plate 91 is equipped with the supplementary piece 98 that supplementary stripper plate 91 pressed, one side and stripper plate 91 fixed connection of supplementary piece 98, stripper plate 91 can freely slide from top to bottom in centrifugal sleeve 10 is inside, one side of stripper plate 91 is equipped with connecting block 92, one side and stripper plate 91 fixed connection of connecting block 92, the inside of connecting block 92 is equipped with two pivots 93, and the both ends of two pivots 93 all with centrifugal sleeve 10 fixed connection, the outside of two pivots 93 is equipped with rotor plate 94, and rotor plate 94 rotates with two pivots 93 to be connected, the inside of rotor plate 94 is equipped with three pivots 95, and three pivots 95 rotate to be connected, and the both ends of three pivots 95 all with the inner wall fixed connection of centrifugal sleeve 10, one side of the rotating plate 94 is provided with a connecting plate 96, one side of the connecting plate 96 is fixedly connected with the rotating plate 94, one side of the connecting plate 96 is provided with an arc panel 97 for supporting the bottom of the solid bottom connector 3, one side of the arc panel 97 is fixedly connected with the connecting plate 96, when the centrifuge tube needs to be taken out, the auxiliary block 98 can be pressed towards the bottom of the centrifuge sleeve 10, furthermore, one side of the extrusion plate 91 is abutted against the inclined plane part 831 of the rotating block 83, under the action of the extrusion force, the rotating block 83 rotates upwards and enters the limiting groove 81, so that the limiting effect of the rotating block 83 on the columnar tube body 1 is eliminated, meanwhile, the extrusion plate 91 can also drive the rotating plate 94 to move downwards, and due to the lever principle, the connecting plate 96 on one side of the rotating shaft three 95 can drive the arc panel 97 to lift upwards, so as to smoothly eject the centrifuge tube out of the centrifuge sleeve 10, make things convenient for the staff to take the centrifuging tube more, saved the time of taking the centrifuging tube, improved work efficiency.

One side of the rotating block 83 is shaped like an arc, in the process that the cylindrical pipe body 1 is inserted into the centrifugal sleeve 10, the arc surface part of the rotating block 83 is in contact with the cylindrical pipe body 1, and the arc surface part of the rotating block 83 is more beneficial to inserting the solid bottom joint 3 at one end of the cylindrical pipe body 1 into the centrifugal sleeve 10.

The solid bottom 4 comprises the convex part 41, the filter membrane 5 comprises the concave part 51, one side of the convex part 41 of the solid bottom 4 is matched with the concave part 51 of the filter membrane 5 in shape, when the filter membrane 5 is replaced, the solid bottom connector 3 can be placed on a flat fixed base firstly, so that the solid bottom connector is in a vertical state with a horizontal line, the concave part 51 of the filter membrane 5 is clamped by tweezers and then vertically fed into the solid bottom connector 3 until the concave part 51 is matched with the convex part 41 of the solid bottom 4, the filter membrane 5 at the moment is positioned at the central position of the surface of the solid bottom 4, the phenomenon that the side edge of the filter membrane 5 is bent when the filter membrane 5 is replaced is reduced, the time for replacing the filter membrane 5 is further reduced, and the working efficiency is improved.

The columnar tube body 1, the hollow bottom joint 2 and the solid bottom joint 3 are all made of polytetrafluoroethylene or polypropylene, and the polytetrafluoroethylene and the polypropylene have the characteristics of acid resistance, alkali resistance, various organic solvents resistance and high temperature resistance, so that the quality of the tube body of the centrifugal tube is ensured.

It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.

Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims

1. The utility model provides a can be applied to quick nondestructive analysis's capsule type secondary centrifuging tube, includes column body (1), its characterized in that: the device comprises a columnar pipe body (1), a hollow bottom connector (2) used for sealing the columnar pipe body (1) is arranged outside the columnar pipe body (1), a solid bottom connector (3) which is used for sealing the columnar pipe body (1) together with the hollow bottom connector (2) is arranged outside the columnar pipe body (1), external threads (6) are arranged on one side of the columnar pipe body (1), internal threads (7) which are matched with the external threads (6) are arranged inside the solid bottom connector (3) and the hollow bottom connector (2), the solid bottom connector (3) and the hollow bottom connector (2) are respectively arranged at two ends of the columnar pipe body (1) and are in threaded connection with the columnar pipe body (1), a solid bottom (4) is arranged inside the solid bottom connector (3), and a filter membrane (5) used for filtering heavy metals in a water body solution inside the columnar pipe body (1) and heavy metals in suspended particles is arranged on one side of the solid bottom (4);

a centrifugal sleeve (10) used for loading a centrifugal tube in a centrifugal machine is arranged outside the columnar tube body (1), a limiting assembly (8) for extruding the surface of the columnar tube body (1) is arranged inside the centrifugal sleeve (10), the limiting assembly (8) comprises a rotating block (83) located inside the centrifugal sleeve (10), a limiting groove (81) for the rotating block (83) to rotate is formed inside the centrifugal sleeve (10), a first rotating shaft (82) is arranged inside the rotating block (83), and the rotating block (83) comprises an inclined plane part (831);

one side of inclined plane portion (831) is equipped with and carries out the pop-up subassembly (9) that lifts to the inside centrifuging tube of centrifugal sleeve (10), pop-up subassembly (9) is including lieing in inside stripper plate (91) of centrifugal sleeve (10), one side of stripper plate (91) is equipped with supplementary piece (98) that supplementary stripper plate (91) pressed, stripper plate (91) can be inside freely from top to bottom sliding at centrifugal sleeve (10), one side of stripper plate (91) is equipped with connecting block (92), the inside of connecting block (92) is equipped with pivot two (93), the outside of pivot two (93) is equipped with rotor plate (94), the inside of rotor plate (94) is equipped with pivot three (95), one side of rotor plate (94) is equipped with connecting plate (96), one side of connecting plate (96) is equipped with cambered plate (97) that carry out the support to solid bottom connector (3) bottom.

2. The capsule type secondary centrifuge tube applicable to rapid nondestructive analysis according to claim 1, wherein: one side of the rotating block (83) is arc-shaped, and in the process that the cylindrical pipe body (1) is inserted into the centrifugal sleeve (10), the arc-shaped part of the rotating block (83) is in contact with the cylindrical pipe body (1).

3. The capsule type secondary centrifuge tube applicable to rapid nondestructive analysis according to claim 1, wherein: the cambered surface of the cambered plate (97) is matched with the bottom cambered surface of the solid bottom joint (3).

4. The capsule type secondary centrifuge tube applicable to rapid nondestructive analysis according to claim 1, wherein: the solid bottom (4) comprises a convex part (41), the filter membrane (5) comprises a concave part (51), and the shape of one side of the convex part (41) of the solid bottom (4) is matched with the shape of the concave part (51) of the filter membrane (5).

5. The capsule type secondary centrifuge tube applicable to rapid nondestructive analysis according to claim 1, wherein: the columnar pipe body (1), the hollow bottom joint (2) and the solid bottom joint (3) are all made of polytetrafluoroethylene or polypropylene.