A high-pressure anti-corrosion reaction device for batch digestion of geological samples

Abstract

The present 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, which includes a digestion upper plate, a digestion lower plate and an inner tank. The digestion lower plate is provided with a plurality of placement holes for installing the inner tank, and heat dissipation holes are opened inside the placement holes. The digestion upper plate is provided with fixing holes that match the positions and quantities of the placement holes, and screw holes are opened inside the fixing holes; the digestion upper plate and the digestion lower plate are joined to form an integrated digestion plate; the inner tank includes a lid and a tank body. The top end of the tank body is a necked-in structure, and the lid is sleeved on the top end of the tank body and forms a sealed hollow inner cavity with the tank body. The present invention adopts an integrated digestion plate, and the overall seal of the device can be completed through simple buckling, significantly reducing the workload and working time of experimental personnel. 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; this device can quickly complete the digestion work of geological samples with multiple sample amounts in the same batch, saving time and effort.

Description

Technical Field

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

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

[0003] Among them, the method of adding acid to melt the sample in an open container placed on a hot plate has a good dissolution effect on some geological samples, but the digestion effect on rock samples containing refractory minerals such as garnet, spinel, zircon, rutile, chromite, etc. is not ideal. The microwave digestion method is difficult to digest refractory minerals in different rock types, resulting in insufficient recovery of some elements and deviation in analytical test results. The alkali fusion method can effectively digest refractory minerals in different rock types, but it requires additional introduction of a flux, which will result in a high background value and TDS in the diluted solution after sample digestion. After being tested on the machine, a high content of matrix substances will precipitate at the sample cone and intercept cone openings of the instrument, causing the instrument to drift and affecting the accuracy of data and test precision.

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

[0005] (1) Prone to acid vapor corrosion: Due to the complexity of geological samples and the difference in particle size, when experimental personnel use a high-pressure melting bomb to digest geological samples, a certain volume of concentrated acid, such as aqua regia and concentrated hydrofluoric acid, needs to be added 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, a small amount of volatilized acid vapor will cause serious corrosion of the inner wall of the digestion sleeve. The corrosion products adhering to the inner wall of the Teflon inner tank may contaminate the sample solution and affect the accuracy of experimental data. Another drawback 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 a large-volume container, which is difficult to clean. There is a risk of cleaning liquid splashing and corroding the laboratory floor during the process of adding a certain concentration of solution for soaking and cleaning.

[0006] (2) Heavy self-weight: Due to the large self-weight of a single stainless steel digestion sleeve, it is time-consuming and laborious during use. The process of putting a whole plate of digestion sleeves into the oven may cause them to fall and injure experimental personnel, posing 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 strong acids are commonly used in the geological sample digestion process, after a period of use, the sprayed anti-corrosion coating will peel off. Both the inner lining and the outer wall of the anti-corrosion digestion sleeve will be corroded by acid, and the anti-corrosion coating will shed slag. After a period of use, the anti-corrosion digestion sleeve needs to be returned to the factory for repair or replaced with a new digestion sleeve, resulting in a relatively high cost.

[0008] (4) Occupying a large amount of experimental space: Regardless of which digestion sleeve is used, each Teflon inner tank is equipped with a digestion sleeve. Storing a large number of digestion sleeves in the laboratory occupies a large amount of space.

[0009] (5) Complicated to use: The digestion process of the high-pressure melting sample bomb includes steps such as initial melting, acid expulsion, and re-melting. During the digestion process of each sample, the experimenter needs to repeatedly screw and unscrew the tank, repeating a large amount of physical activities, wasting valuable time.

[0010] In view of the disadvantages of the existing stainless-steel digestion sleeve, the present invention designs a high-pressure anti-corrosion reaction device that can quickly complete the digestion of multiple sample volumes 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 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 plate, and the overall seal of the digestion device can be completed through simple buckling, significantly reducing the workload and working time of the experimenter. 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 realizes the rapid completion of the digestion work of geological samples with multiple sample volumes in the same batch, saving time and effort.

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

[0013] A high-pressure anti-corrosion reaction device for batch digestion of geological samples, including a digestion upper plate, a digestion lower plate, and an inner tank disposed between the digestion upper plate and the digestion lower plate. The digestion lower plate is provided with a plurality of placement holes for installing the inner tank, and heat dissipation holes are opened inside the placement holes. The digestion upper plate is provided with fixing holes that match the positions and quantities of the placement holes, and screw holes are opened inside the fixing holes; the digestion upper plate and the digestion lower plate are joined to form an integrated digestion plate; the inner tank includes a lid and a tank body, the top end of the tank body is a necked-in structure, and the lid is sleeved on the top end of the tank body and forms a sealed hollow inner cavity with the tank body.

[0014] Due to the necked-in structure at the top end of the tank body, its diameter is smaller than the diameter of the lower end of the tank body. According to the force analysis, it can be obtained that after the necking size at the top end of the tank body becomes smaller, the pressure exerted by the lid on the tank body under the action of external force becomes larger, reducing the possibility of acid gas overflow.

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

[0016] The overall components of the above-mentioned digestion upper plate and digestion lower plate adopt aluminum alloy materials, abandoning stainless steel materials, mainly considering the advantages of light weight and strong thermal conductivity of aluminum alloy materials, which will greatly reduce the labor consumption of experimental personnel in carrying the digestion plate in and out of the oven during the digestion of geological samples;

[0017] Moreover, Teflon coatings are sprayed on the inner and outer walls of the aluminum alloy digestion lower plate and upper plate, which also combines the heat resistance and anti-corrosion properties of Teflon materials with the advantages of aluminum alloy materials, greatly improving the feasibility of using aluminum alloy materials for digesting geological samples and extending 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 the same as that 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 after the combination of the placement hole and the fixing hole is 1-5 mm smaller than the height of the inner tank. Such a design, on the premise of not affecting the overall fastening of the digestion device, also ensures that even if a very small amount of acid vapor overflows during use, it will be promptly sucked away by the exhaust device through the gap (i.e., the depth height difference) between the digestion lower plate and the digestion upper plate, reducing the possibility of acid vapor corrosion of the reaction device and extending the service life of the device.

[0020] Furthermore, the inclination angle of the top closing structure of the tank body is 60°-45°. The inclination angle can be any angle within the range of 60°-45°, such as 45°, 50°, 55° or 60°, etc., but is not limited to the listed values, and other unlisted angles within this range are equally applicable.

[0021] Furthermore, more than one spring duckbill buckle is provided 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 its lower part is fixedly connected to the digestion lower plate.

[0022] Furthermore, the digestion upper plate is a rectangular aluminum alloy plate, and the upper parts of the spring duckbill buckles are 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 parts of the spring duckbill buckles are arranged oppositely on both sides of the long side of the digestion lower plate;

[0023] By buckling and clamping the upper part and the lower part of the spring duckbill buckle, the digestion upper plate and the digestion lower plate are connected to form an integrated digestion plate.

[0024] Further, at least a pair of handles are installed on the digestion lower plate, and the handles are symmetrically arranged on both sides of the digestion lower plate.

[0025] Further, 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] Further, the heat dissipation holes are arranged at the center of the bottom of the placement holes, and the screw holes are arranged at the center of the top of the fixing holes.

[0027] Advantages of the present invention:

[0028] (1) The overall material of the digestion plate of the present invention is made of aluminum alloy, which has the advantages of being light and having strong heat conductivity. During the use by experimental personnel, unnecessary physical labor can be reduced; after corresponding placement holes and fixing holes are drilled on the digestion lower plate and the upper plate respectively, the inner and outer walls of the digestion lower plate, the upper plate, the placement holes and the fixing holes are integrally sprayed with Teflon material, so as to use the Teflon material 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 integrally buckle the outer cans (i.e., the digestion lower plate and the digestion upper plate) of the Teflon inner cans of the same batch, avoiding the work of screwing and unscrewing the cans for individual samples by repeatedly using stainless steel outer cans. The digestion plate can complete the digestion work of no less than 40 geological samples at one time in batches, greatly reducing the workload of experimental personnel.

[0030] (3) The combined depth of the placement holes and the fixing holes is slightly smaller than the height of the Teflon inner can, so as to timely discharge the overflowing acid vapor, reduce the possibility of acid vapor corrosion of the reaction device, and extend the service life of the digestion device.

[0031] (4) The device of the present invention adopts an integrated digestion plate. When there is no experimental work, the experimental personnel only need to buckle the digestion lower plate and the upper plate, and then they can quickly complete the sorting, storage and storage, saving time and greatly reducing the occupation of laboratory space. Description of the drawings

[0032] Figure 1 is the top view of the digestion upper plate;

[0033] Figure 2 is the longitudinal sectional structure schematic diagram of the digestion upper plate;

[0034] Figure 3 is the top view of the digestion lower plate;

[0035] Figure 4 is the longitudinal sectional structure schematic diagram of the digestion lower plate;

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

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

[0038] Figure 7 is a schematic longitudinal sectional structure diagram 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 implementation manners

[0040] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

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

[0042] The present invention provides a high-pressure anti-corrosion reaction device for batch digestion of geological samples, including a digestion upper plate, a digestion lower plate, and an inner tank disposed 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, as Figure 1 and Figure 2 shown, the digestion lower plate is a whole rectangular aluminum alloy plate, and 40 placement holes 1 are opened on the plate. The placement holes 1 are used to place the inner tank 10, and their inner walls are sprayed with a Teflon coating, mainly for anti-corrosion purposes. A heat dissipation hole 2 is drilled at the center of the bottom of the placement hole 1, and the heat dissipation hole 2 leads directly to the bottom of the digestion lower plate.

[0044] In a specific embodiment, as Figure 3 and Figure 4 shown, the digestion upper plate is a whole rectangular aluminum alloy plate, and 40 fixing holes 5 with the same inner diameter and matching positions as the placement holes 1 are drilled on the plate. The inner walls of the fixing holes 5 are sprayed with a Teflon coating for anti-corrosion purposes. A screw hole 6 is drilled at 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 according to the actual needs of the sample melting work, 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 the same as the number of placement holes, and can be less than 40 or more than 40.

[0046] From Figure 7 It can be seen that after the digestion upper plate and the digestion lower plate are connected and combined, an integrated digestion plate is formed. Specifically, more than one spring duckbill buckle 4 is provided at the connection between the digestion upper plate and the digestion lower plate for the overall closing of the digestion upper plate and the digestion lower plate. As Figure 5 shown, two round holes are provided in the upper part of the spring duckbill buckle 4. The round holes are used to weld the spring duckbill buckle 4 to the outer wall of the digestion upper plate, and its lower part is fixedly connected to the digestion lower plate. By buckling 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 can be understood that buckling the spring duckbill buckles 4 corresponding to the two long sides of the digestion lower plate and the digestion upper plate ensures the high-pressure environment applied to the Teflon inner tank 10 between the digestion lower plate and the digestion upper plate, thus ensuring that the geological samples can be quickly and efficiently digested into a clear solution, facilitating subsequent analysis and testing work.

[0047] In a specific embodiment, the digestion upper plate is a rectangular aluminum alloy plate. The upper parts of the spring duckbill buckles 4 are welded on both long sides of the digestion upper plate and are arranged oppositely; the digestion lower plate is also a rectangular aluminum alloy plate. The lower parts of the spring duckbill buckles 4 are fixedly installed on both long sides of the digestion lower plate and are arranged oppositely.

[0048] When the digestion upper plate and the digestion lower plate are connected to form an integrated digestion plate, the depth ratio of the combined placement holes 1 and fixing holes 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 timely sucked away by the exhaust device through the gap between the digestion lower plate and the digestion upper plate, reducing the possibility of acid vapor corrosion of the reaction device and prolonging the service life of the digestion device.

[0049] As 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, then place the strong spring 8 on the first Teflon gasket 7, continue to place the second Teflon gasket 9 on the strong spring 8, and then use fasteners (such as Teflon screws) to pass through the central small hole of the second Teflon gasket 9, the strong spring 8, and the central small hole of the first Teflon gasket 7 in sequence, and use a screwdriver to tighten the Teflon screw and 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 plate after the digestion lower plate and the digestion upper plate are buckled, which can effectively prevent the acid vapor generated by the gasification of the concentrated acid from pushing open the lid 101 of the Teflon inner tank 10 after the digestion plate is placed in the oven and heated, prevent the concentrated acid in the Teflon inner tank 10 from generating acid vapor overflow due to the high-temperature heating process, and avoid incomplete digestion of the sample.

[0050] In this embodiment, the inside of the Teflon inner tank 10 is a cavity for loading geological samples. As Figure 6 shown, the inner tank 10 is composed of a lid 101 and a tank body 102. The lid 101 is hermetically inserted at the top end of the tank body 102 and forms a closed hollow inner cavity with the tank body 102. The axial cross-section formed by the lid 101 and the inside of the tank body 102 is elliptical, and the inner wall of the Teflon inner tank 10 is smooth, so as to ensure that the acid vapor formed by the concentrated acid during the high-temperature and high-pressure sample melting process circulates inside the tank body 102 and does not stick to the wall, 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 than or less than 15 mL.

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

[0053] For example, when the included angle θ is 60°, the pressure F 压 received by the tank body is 0.5G (G×cos60°). When the included angle θ is reduced from 60° to 45° (corresponding to the reduction of the closing size at the top of the tank body), 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 includes a digestion upper plate, a digestion lower plate, and an inner tank disposed between the digestion upper plate and the digestion lower plate. The digestion upper plate and the digestion lower plate are integrally made of aluminum alloy, and the surfaces of the digestion upper plate and the digestion lower plate are both sprayed with Teflon material; the inner tank is a Teflon inner tank, and its inner wall is smooth; The digestion lower plate is provided with a plurality of placement holes for installing the inner tank. Heat dissipation holes are provided inside the placement holes. The digestion upper plate is provided with fixing holes that match the positions and quantities of the placement holes. Screw holes are provided inside the fixing holes; the depth of the placement holes and the fixing holes is slightly smaller than the height of the inner tank, and the inner diameter of the placement holes is the same as that of the fixing holes; The digestion upper plate and the digestion lower plate are joined together to form an integrated digestion plate; the inner tank includes a lid and a tank body. The top end of the tank body is a necked-in structure, and the inclination angle of the necked-in structure is 60° to 45°; the lid is sleeved on the top end of the tank body and forms a sealed hollow inner cavity with the tank body.

2. The device according to claim 1, wherein One or more spring duckbill fasteners are provided at the connection between the digestion upper plate and the digestion lower plate. The upper part of the spring duckbill fastener is fixedly installed on the digestion upper plate, and its lower part is fixedly connected to the digestion lower plate.

3. The device according to claim 2, characterized in that, The digestion upper plate is a rectangular aluminum alloy plate, and the upper parts of the spring duckbill fasteners are oppositely arranged 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 parts of the spring duckbill fasteners are oppositely arranged on both sides of the long side of the digestion lower plate; By buckling and clamping the upper part and the lower part of the spring duckbill fastener, the digestion upper plate and the digestion lower plate are connected to form an integrated digestion plate.

4. The device according to claim 1, characterized in that, At least a pair of handles are installed on the digestion lower plate, and the handles are symmetrically arranged on both sides of the digestion lower plate.

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

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

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