High-pressure anti-corrosion reaction device for digesting geological samples in batches

Abstract

The invention belongs to the technical field of sample digestion, and relates to a high-pressure anti-corrosion reaction device for batch digestion of geological samples, the high-pressure anti-corrosion reaction device comprises a digestion upper disc, a digestion lower disc and inner tanks, the digestion lower disc is provided with a plurality of placing holes for installing the inner tanks, and heat dissipation holes are formed in the placing holes; fixing holes matched with the placement holes in position and number are formed in the upper digestion disc, and screw holes are formed in the fixing holes; the upper digestion disc and the lower digestion disc are connected to form an integrated digestion disc; the inner tank comprises a cover and a tank body, the top end of the tank body is of a closing-in structure, and the cover is connected to the top end of the tank body in a sleeving mode and forms a closed hollow inner cavity with the tank body. The integrated digestion disc is adopted, overall sealing of the device can be completed through simple buckling, the workload and working time of experimenters are remarkably reduced, meanwhile, through the improved inner tank structure, the possibility of acid gas overflowing is reduced, and the service life of the digestion device is prolonged; the device can quickly complete the digestion work of multiple geological samples in the same batch, and is time-saving and labor-saving.

Description

Technical Field

[0001] The invention belongs to the technical field of sample digestion, and relates to a high-pressure digestion device for multiple samples, and in particular to a high-pressure anti-corrosion reaction device for batch digestion of geological samples. Background Art

[0002] In geological sample analysis, sample digestion is crucial to accurately determine the content of trace elements in geological samples, and the sample digestion process is one of the key factors restricting data quality. The methods commonly used in different laboratories to digest geological samples mainly include open container acid dissolution, microwave digestion, alkali fusion or high-pressure molten sample bomb digestion.

[0003] Among them, the method of placing an open container on a hot plate and adding acid to the sample has a good dissolution effect on some geological samples, but the digestion effect on rock samples containing insoluble minerals such as garnet, spinel, zircon, rutile, chromite, etc. is not ideal. Microwave digestion is difficult to digest insoluble minerals in different rock types, resulting in insufficient recovery of some elements and deviations in analytical test results. The alkali fusion method can effectively digest insoluble minerals in different rock types, but it requires the additional introduction of flux, which will result in higher background values ​​and TDS in the diluted solution after sample digestion. After the machine test, a high content of matrix material will be precipitated on the sample cone and intercepting cone of the instrument, causing the instrument to drift, affecting the accuracy of the data and the test precision.

[0004] High-pressure molten sample digestion is currently a widely used method for efficiently digesting geological samples. However, this type of digestion device still has the following defects during use:

[0005] (1) Easily corroded by acid vapor: Due to the complexity of geological samples and differences in particle size, when experimenters use high-pressure melting bombs to digest geological samples, they need to add a certain volume of concentrated acid, such as aqua regia and concentrated hydrofluoric acid, to the Teflon inner tank. During the high-temperature heating process, acid vapor will overflow. Since the common melting bomb digestion sleeve is mainly made of stainless steel, the small amount of volatilized acid vapor will cause serious corrosion to the inner wall of the digestion sleeve. The corrosive substances attached to the wall of the Teflon inner tank may contaminate the sample solution and affect the accuracy of the experimental data. Another disadvantage of acid gas corrosion is that the stainless steel digestion sleeve may rust and cannot be opened. At the same time, cleaning the corroded stainless steel digestion sleeve requires the use of a large volume container, which is difficult to clean. There is a risk of splashing cleaning liquid and corroding the laboratory floor during the soaking and cleaning process of adding a certain concentration of solution.

[0006] (2) Heavy weight: Since a single stainless steel digestion cover has a large weight, its use is time-consuming and labor-intensive. In the process of placing a whole tray of digestion covers in the oven, the covers may fall and injure the experimenters, which poses a certain safety hazard.

[0007] (3) High maintenance cost: The inner lining surface of the stainless steel anti-corrosion digestion sleeve is sprayed with an anti-corrosion coating. Since concentrated acid is often used in the digestion process of geological samples, the sprayed anti-corrosion coating will fall off after a period of use. Both the inner lining and the outer wall of the anti-corrosion digestion sleeve will be corroded by the acid, and the anti-corrosion coating will fall off. After a period of use, the anti-corrosion digestion sleeve needs to be returned to the factory for repair or replaced with a new one, which is costly.

[0008] (4) Occupies a large amount of experimental space: Regardless of which digestion cover is used, each Teflon inner tank is equipped with a digestion cover. Storing a large number of digestion covers in the laboratory takes up a lot of space.

[0009] (5) Complicated use: The high-pressure melting bomb digestion process includes the steps of initial melting, acid removal, and re-melting. During each sample digestion process, the experimenter needs to repeatedly twist and disassemble the can, repeating a lot of physical activities, wasting precious time.

[0010] Aiming at the shortcomings of the existing stainless steel digestion sleeve, the present invention designs a high-pressure anti-corrosion reaction device which can quickly complete the digestion of multiple samples in the same batch, is easy to use and is not easily corroded. Summary of the invention

[0011] The purpose of the present invention is to solve the above-mentioned problems existing in the prior art, and proposes a high-pressure anti-corrosion reaction device for batch digestion of geological samples. The digestion device adopts an integrated digestion disk, and the overall sealing of the digestion device can be completed by simple buckling, which significantly reduces the workload and working time of the experimenters. At the same time, through the improved inner tank structure, the possibility of acid gas overflow is reduced, and the service life of the digestion device is extended; the device can quickly complete the digestion of multiple samples of the same batch of geological samples, saving time and effort.

[0012] The technical solution of the present invention is:

[0013] A high-pressure anti-corrosion reaction device for batch digestion of geological samples comprises an upper digestion plate, a lower digestion plate and an inner tank arranged between the upper digestion plate and the lower digestion plate, the lower digestion plate is provided with a plurality of placement holes for installing the inner tank, the placement holes are provided with heat dissipation holes, the upper digestion plate is provided with fixing holes matching the positions and number of the placement holes, the fixing holes are provided with screw holes; the upper digestion plate and the lower digestion plate are combined to form an integrated digestion plate; the inner tank comprises a cover and a tank body, the top end of the tank body is a closing structure, the cover is sleeved on the top end of the tank body and forms a closed hollow inner cavity with the tank body.

[0014] The closing structure at the top of the tank body makes its diameter smaller than that of the lower end of the tank body. According to the force analysis, it can be concluded that when the closing size of the top of the tank body becomes smaller, the pressure exerted by the lid on the tank body under the action of external force becomes greater, reducing the possibility of acid gas overflow.

[0015] Furthermore, the digestion upper plate and the digestion lower plate are made of aluminum alloy as a whole, and the surfaces of the digestion upper plate and the digestion lower plate are sprayed with Teflon material;

[0016] The above digestion upper plate and digestion lower plate are made of aluminum alloy instead of stainless steel, mainly considering the advantages of aluminum alloy material being light and having strong thermal conductivity, which will greatly reduce the manpower consumption required by the experimenters to carry the digestion plate in and out of the oven during the digestion of geological samples;

[0017] In addition, Teflon coating is sprayed on the inner and outer walls of the aluminum alloy digestion lower plate and upper plate, which combines the heat resistance and corrosion resistance of Teflon material with the advantages of aluminum alloy material, greatly improving the feasibility of using aluminum alloy material for digestion of geological samples and increasing the service life of the digestion plate.

[0018] The inner tank is a Teflon inner tank, and its inner wall is smooth.

[0019] Furthermore, the inner diameter of the placement hole is consistent with the inner diameter of the fixing hole, and the depth of the placement hole and the fixing hole is slightly smaller than the height of the inner tank. For example, the depth of the combination of the placement hole and the fixing hole is 1 to 5 mm smaller than the height of the inner tank. Such a design, without affecting the overall fit of the digestion device, also ensures that even if a very small amount of acid vapor overflows during use, it will be promptly drawn away by the exhaust device through the gap between the digestion lower plate and the digestion upper plate (i.e., the depth height difference), thereby reducing the possibility of acid vapor corroding the reaction device and extending the service life of the device.

[0020] Furthermore, the inclination angle of the closing structure at the top of the tank body is 60° to 45°. The inclination angle can be any angle within the range of 60° to 45°, for example, 45°, 50°, 55° or 60°, but is not limited to the listed values, and other angles not listed within the range are also applicable.

[0021] Furthermore, one or more spring duckbill buckles are provided at the connection between the digestion upper plate and the digestion lower plate, the upper part of the spring duckbill buckle is fixedly mounted on the digestion upper plate, and the lower part thereof is fixedly connected to the digestion lower plate.

[0022] Further, the digestion upper plate is a rectangular aluminum alloy plate, and the upper part of the spring duckbill buckle is arranged oppositely on both sides of the long side of the digestion upper plate; the digestion lower plate is a rectangular aluminum alloy plate, and the lower part of the spring duckbill buckle is arranged oppositely on both sides of the long side of the digestion lower plate;

[0023] The upper part and the lower part of the spring duckbill buckle are buckled and clamped to connect the digestion upper plate and the digestion lower plate to form an integrated digestion plate.

[0024] Furthermore, the digestion lower plate is equipped with at least one pair of handles, and the handles are symmetrically arranged on both sides of the digestion lower plate.

[0025] Furthermore, a first Teflon gasket and a second Teflon gasket are arranged in the fixing hole, a strong spring is placed between the two gaskets, and the first Teflon gasket, the strong spring and the second Teflon gasket are connected by screws arranged in the screw holes.

[0026] Furthermore, the heat dissipation hole is arranged at the bottom center position of the placement hole, and the screw hole is arranged at the top center position of the fixing hole.

[0027] Beneficial effects of the present invention:

[0028] (1) The digestion plate of the present invention is made of aluminum alloy as a whole, which has the advantages of being light and having strong thermal conductivity, and can reduce unnecessary physical labor during use by experimenters; after the corresponding placement holes and fixing holes are respectively opened in the digestion lower plate and the upper plate, the inner and outer walls of the digestion lower plate and the upper plate, the placement holes, and the fixing holes are sprayed with Teflon material as a whole, so that the Teflon material is used to protect the aluminum alloy material, improve the anti-corrosion performance of the digestion device, extend the service life of the digestion device, and reduce the maintenance cost of the laboratory.

[0029] (2) The present invention can buckle the outer tank (i.e., digestion lower plate and digestion upper plate) of the same batch of Teflon inner tanks as a whole, avoiding the work of repeatedly using the stainless steel outer tank to screw and disassemble a single sample. The digestion plate can complete the digestion of no less than 40 geological samples in batches at one time, greatly reducing the workload of the experimenter.

[0030] (3) The combined depth of the placement hole and the fixing hole is slightly smaller than the height of the Teflon inner tank, so that the overflowing acid vapor can be discharged in time, reducing the possibility of acid vapor corrosive to the reaction device and extending the service life of the digestion device.

[0031] (4) The device of the present invention adopts an integrated digestion tray. When there is no experimental work, the experimenter only needs to snap the digestion lower tray and the upper tray together to quickly complete the sorting and storage, which saves time and greatly reduces the occupation of laboratory space. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] Figure 1 It is a top view of the dissolution of the hanging plate;

[0033] Figure 2 It is a schematic diagram of the longitudinal section structure of the upper plate;

[0034] Figure 3 It is a top view of the digested footwall;

[0035] Figure 4 It is a schematic diagram of the longitudinal section structure of the digestion footwall;

[0036] Figure 5 It is a structural diagram of a spring duckbill buckle;

[0037] Figure 6 It is a schematic diagram of the component structure of the inner tank; among them, (a) is an integrated diagram of the inner tank; (b) is a disassembled diagram of the inner tank structure; (c) is a force analysis diagram of the inner tank;

[0038] Figure 7 It is a schematic diagram of the longitudinal section structure of the overall device of the present invention;

[0039] In the above figures, 1. placement hole; 2. heat dissipation hole; 3. handle; 4. spring duckbill buckle; 5. fixing hole; 6. screw hole; 7. first Teflon gasket; 8. strong spring; 9. second Teflon gasket; 10. inner tank; 101. lid; 102. tank body. DETAILED DESCRIPTION

[0040] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0041] In order to further understand the present invention, the present invention will be further described in conjunction with the accompanying drawings and embodiments.

[0042] The invention provides a high-pressure anti-corrosion reaction device for batch digestion of geological samples, comprising a digestion upper plate, a digestion lower plate, and an inner tank arranged between the digestion upper plate and the digestion lower plate. The inner tank used is a Teflon inner tank, and the surfaces of the digestion upper plate and the digestion lower plate are also sprayed with Teflon material.

[0043] In a specific embodiment, if Figure 1 and Figure 2 As shown, the digestion lower plate is a whole rectangular aluminum alloy plate, on which 40 placement holes 1 are opened, and the placement holes 1 are used to place the inner tank 10, and the inner wall thereof is sprayed with a Teflon coating, mainly for corrosion prevention. A heat dissipation hole 2 is drilled in the center of the bottom of the placement hole 1, and the heat dissipation hole 2 directly passes through the bottom of the digestion lower plate.

[0044] In a specific embodiment, if Figure 3 and Figure 4 As shown, the digestion upper plate is a whole rectangular aluminum alloy plate, on which 40 fixing holes 5 are drilled with the same inner diameter and position as the placement hole 1, and the inner wall of the fixing hole 5 is sprayed with Teflon coating for corrosion prevention. A screw hole 6 is drilled in the center of the top of the fixing hole 5.

[0045] In the specific application process, the number of placement holes 1 provided on the digestion lower plate is not strictly limited. According to the actual number of geological samples to be digested or the actual melting sample work requirements, the number of placement holes can be more than 40 or less than 40. Similarly, the number of fixing holes 5 on the digestion upper plate is consistent with the number of placement holes, which can be less than 40 or more than 40.

[0046] from Figure 7 As can be seen from the above, the digestion upper plate and the digestion lower plate are connected to form an integrated digestion plate. Specifically, at the connection between the digestion upper plate and the digestion lower plate, there is one or more spring duckbill buckles 4 for the overall closure of the digestion upper plate and the digestion lower plate. Figure 5 As shown, the upper part of the spring duckbill buckle 4 is provided with two circular holes, and the circular holes are used to weld the spring duckbill buckle 4 to the outer wall of the digestion upper plate, and the lower part thereof is fixedly connected to the digestion lower plate. By snapping and clamping the upper and lower parts of the spring duckbill buckle 4, the digestion upper plate and the digestion lower plate are connected to form an integrated digestion plate. It is understandable that the spring duckbill buckles 4 corresponding to the long sides of the digestion lower plate and the digestion upper plate are snapped together to ensure that the high pressure environment applied to the Teflon inner tank 10 between the digestion lower plate and the digestion upper plate is ensured, thereby ensuring that the geological sample can be quickly and efficiently digested into a clear solution, which is convenient for subsequent analysis and testing.

[0047] In a specific embodiment, the digestion upper plate is a rectangular aluminum alloy plate, and the upper part of the spring duckbill buckle 4 is welded on both sides of the long side of the digestion upper plate and is relatively arranged; the digestion lower plate is also a rectangular aluminum alloy plate, and the lower part of the spring duckbill buckle 4 is fixedly installed on both sides of the long side of the digestion lower plate and is relatively arranged.

[0048] When the digestion upper plate and the digestion lower plate are connected to form an integrated digestion plate, the depth of the combined placement hole 1 and the fixing hole 5 is slightly smaller than the height of the inner tank 10. In this way, even if a very small amount of acid vapor overflows during use, it can be promptly drawn away by the exhaust device through the gap between the digestion lower plate and the digestion upper plate, thereby reducing the possibility of corrosion of the reaction device by the acid vapor and extending the service life of the digestion device.

[0049] like Figure 2As shown, a screw hole 6 is drilled in the center of the top of the fixing hole 5. The experimenter needs to place the first Teflon gasket 7 in the fixing hole 5, and then place the strong spring 8 on the first Teflon gasket 7, and continue to place the second Teflon gasket 9 on the strong spring 8. Then, a fastener (such as a Teflon screw) is used to pass through the center hole of the second Teflon gasket 9, the strong spring 8, and the center hole of the first Teflon gasket 7 in sequence, and the Teflon screw is tightened with a screwdriver to fix it in the screw hole 6 of the digestion upper plate. The main purpose of setting the first Teflon gasket 7, the strong spring 8, and the second Teflon gasket 9 is to apply pressure to the Teflon inner tank 10 through the first Teflon gasket 7, the strong spring 8, and the second Teflon gasket 9 inside the integrated digestion tray after the digestion lower plate and the digestion upper plate are buckled, so as to effectively prevent the acid vapor of the concentrated acid from pushing open the cover 101 of the Teflon inner tank 10 after the digestion tray is placed in the oven and heated up, and prevent the concentrated acid in the Teflon inner tank 10 from generating acid vapor overflow due to the high-temperature heating process, thereby avoiding incomplete digestion of the sample.

[0050] The interior of the Teflon inner tank 10 used in this embodiment is a cavity for containing geological samples. Figure 6 As shown, the inner tank 10 is composed of a cover 101 and a tank body 102, and the cover 101 is sealed and plugged into the top of the tank body 102 to form a closed hollow inner cavity with the tank body 102. The axial cross-section formed by the cover 101 and the inside of the tank body 102 is elliptical, and the inner wall of the Teflon inner tank 10 is smooth, thereby ensuring that the acid vapor formed by the concentrated acid in the high-temperature and high-pressure melting process circulates inside the tank body 102 without hanging on the wall, thereby promoting the full dissolution of the sample.

[0051] In a specific embodiment, the volume of the Teflon inner tank 10 is 15 mL. According to the actual number of geological samples to be digested, the size of the Teflon inner tank 10 can be modified, and the specific volume can be greater or less than 15 mL.

[0052] from Figure 6 It can be seen that the top of the tank body 102 designed in this embodiment is closed, the diameter is reduced, and the inclination angle θ of the top closing structure is 60° to 45°. 压 =G×cosθ), it can be seen that when the closing size of the top of the can body 102 becomes smaller, the pressure exerted by the cover 101 on the lower can body 102 under the action of external force becomes larger.

[0053] For example, when the angle θ is 60°, the pressure F on the tank is 压 is 0.5G (G×cos60°). When the angle θ is reduced from 60° to 45° (corresponding to the reduction in the size of the top of the tank), the pressure F 压It changed from 0.5G (G×cos60°) to ~0.71G (G×cos45°), with an additional increase of ~0.21G, reducing the possibility of acid gas spillage.

[0054] like Figure 4 As shown, at least one pair of handles 3 are installed on both sides of the short side of the digestion lower plate, and the handles 3 on both sides are symmetrically arranged, and the entire digestion plate can be lifted and placed in the oven for heating by the handles 3. Of course, the same number of handles 3 can also be arranged at corresponding positions on the digestion upper plate, so that the device is more sealed and stable, and the handling operation is safer.

[0055] The method for using the high-pressure anti-corrosion reaction device for batch digestion of geological samples provided by the present invention comprises the following steps:

[0056] The experimenter weighs the geological sample into the Teflon inner tank 10, adds concentrated acid of different types and volumes (such as aqua regia, concentrated hydrofluoric acid, etc.), and then places the Teflon inner tank 10 in the placement hole 1 of the digestion lower plate, and checks whether the second Teflon gasket 9, the strong spring 8, the Teflon screw, and the first Teflon gasket 7 in the fixing hole 5 of the digestion upper plate have been installed accordingly. After checking that everything is correct, cover the digestion upper plate, and buckle the spring duckbill buckles 4 corresponding to the digestion lower plate and the digestion upper plate together. Finally, put the digestion plate with the Teflon inner tank 10 into the oven, set the appropriate heating temperature and time, and complete the digestion of the geological sample.

[0057] The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the above embodiments, those skilled in the art can still modify the technical solutions described in the above embodiments, or replace some of the technical features therein by equivalents. Any modification, equivalent replacement, modification, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A high-pressure anti-corrosion reaction device for batch digestion of geological samples, characterized in that: It comprises an upper digestion plate, a lower digestion plate and an inner tank arranged between the upper digestion plate and the lower digestion plate, the lower digestion plate is provided with a plurality of placement holes for installing the inner tank, the placement holes are provided with heat dissipation holes, the upper digestion plate is provided with fixing holes matching the positions and numbers of the placement holes, the fixing holes are provided with screw holes; the upper digestion plate and the lower digestion plate are combined to form an integrated digestion plate; the inner tank comprises a cover and a tank body, the top end of the tank body is a closing structure, the cover is sleeved on the top end of the tank body and forms a closed hollow inner cavity with the tank body.

2. The device according to claim 1, characterized in that The digestion upper plate and the digestion lower plate are made of aluminum alloy as a whole, and the surfaces of the digestion upper plate and the digestion lower plate are sprayed with Teflon material; The inner tank is a Teflon inner tank, and its inner wall is smooth.

3. The device according to claim 1, characterized in that The depths of the placement hole and the fixing hole are slightly smaller than the height of the inner tank, and the inner diameter of the placement hole is consistent with that of the fixing hole.

4. The device according to claim 1, characterized in that The inclination angle of the closing structure at the top of the tank body is 60° to 45°.

5. The device according to claim 1, characterized in that One or more spring duckbill buckles are arranged at the connection between the digestion upper plate and the digestion lower plate. The upper part of the spring duckbill buckle is fixedly installed on the digestion upper plate, and the lower part thereof is fixedly connected to the digestion lower plate.

6. The device according to claim 5, characterized in that The digestion upper plate is a rectangular aluminum alloy plate, and the upper part of the spring duckbill buckle is arranged oppositely on both sides of the long side of the digestion upper plate; the digestion lower plate is a rectangular aluminum alloy plate, and the lower part of the spring duckbill buckle is arranged oppositely on both sides of the long side of the digestion lower plate; The upper part and the lower part of the spring duckbill buckle are buckled and clamped to connect the digestion upper plate and the digestion lower plate to form an integrated digestion plate.

7. The device according to claim 1, characterized in that The digestion lower plate is equipped with at least one pair of handles, and the handles are symmetrically arranged on both sides of the digestion lower plate.

8. The device according to claim 1, characterized in that A first Teflon gasket and a second Teflon gasket are arranged in the fixing hole, a strong spring is placed between the two gaskets, and the first Teflon gasket, the strong spring and the second Teflon gasket are connected by screws arranged in the screw holes.

9. The device according to claim 1, characterized in that The heat dissipation hole is arranged at the bottom center position of the placement hole, and the screw hole is arranged at the top center position of the fixing hole.

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