CN112665960A

CN112665960A - Closed heating acid removing device and acid removing method

Info

Publication number: CN112665960A
Application number: CN202011477909.8A
Authority: CN
Inventors: 周利敏; 温宏利; 王书谟; 陶迪
Original assignee: National Geological Experimental Testing Center
Current assignee: National Geological Experimental Testing Center
Priority date: 2020-12-15
Filing date: 2020-12-15
Publication date: 2021-04-16

Abstract

The invention relates to a closed heating acid removing device and a closed heating acid removing method, belongs to the technical field of sample dissolving devices, and solves the problems that the existing sample dissolving device is incomplete in acid vapor discharge, easy to generate dust pollution, harmful to the health of experimenters, cross pollution among samples, complex in operation steps, high in operation strength and low in efficiency. This acid device is driven in airtight heating includes: the device comprises a sample dissolving tank, a heating table and an acid vapor collecting and processing assembly, wherein the heating table is provided with a plurality of sample dissolving tank mounting holes for heating the sample dissolving tank; the acid vapor collection and treatment assembly includes an acid vapor collection plate for collecting and treating the generated acid vapor. The invention realizes acid removal, acid vapor collection and treatment in a closed environment, realizes zero emission of toxic gas, has simple structure, less used equipment, low operation intensity, high experimental efficiency and low cross contamination risk, conforms to the development concept of green, efficient and convenient analysis and test technology, and has wide application prospect.

Description

Closed heating acid removing device and acid removing method

Technical Field

The invention relates to the technical field of sample dissolving devices, in particular to a closed heating acid removing device and a method.

Background

Modern analytical instruments such as light and mass spectrometry mostly need to convert a solid sample into a solution form before measurement, so sample digestion is a key step of geological sample analysis. The digestion techniques commonly used at present mainly include acid dissolution, burning, melting and the like. Among them, the acid dissolution method has the longest history and the highest frequency of use. The method utilizes the action of heat and/or acid to decompose a solid sample, so that elements contained in the sample are released from a complex matrix and converted into a simple chemical form.

The process of acid-dissolving the digested sample can be performed under both open and closed conditions. The acid dissolution method under an open system is the most simple and feasible, but the biggest defect of the method is that the digestion temperature is limited by the boiling point of an acid reagent, for example, the boiling point of nitric acid is 122 ℃, the boiling point of hydrofluoric acid is 112 ℃, the temperature is too low for some difficultly soluble minerals, complete digestion is difficult, high-boiling-point acids such as phosphoric acid and sulfuric acid can be added to increase the decomposition temperature, but the introduction of the acids can generate interference and influence on instrument tests to different degrees. Other problems with open systems include: the sample dissolving vessel is easy to be polluted by air floating dust and samples after being opened for a long time; volatile elements are lost. In a closed system, after heating, the pressure in the closed vessel is increased, the boiling point of acid is correspondingly improved, the digestion capability of acid is enhanced, indissolvable minerals can be digested more thoroughly, the dosage of acid reagents for closing a dissolved sample is small, the risk of air floating dust pollution and cross pollution among samples is reduced, and the loss of volatile elements (such As As, B, Cr, Cd, Hg, Sb, Se, Sn and Pb) is avoided. Due to the advantages, the closed acid dissolution has become a common sample digestion means when silicate rock sample trace elements and isotopes are analyzed in production and scientific research laboratories of the geological and mining industries.

However, the existing sample sealing and dissolving device adopts a structure that a polytetrafluoroethylene inner container is combined with a metal outer sleeve (an inner container and an outer steel sleeve), and the operation process is as follows: 1) adding a sample and an acid reagent into a Polytetrafluoroethylene (PTFE) sample-dissolving liner, then placing the liner into a metal sleeve, tightly pressing an upper cover of the liner by adopting a metal cover-screwing mode, placing the liner into an oven for heating, and digesting the sample; 2) after heating, unscrewing the metal sleeve, opening the upper cover of the inner container, and placing on an electric heating plate to heat and remove acid; 3) adding acid solution with proper concentration and volume, sealing the inner container and the metal sleeve again, and putting the inner container and the metal sleeve into an oven for heating to redissolve residues; 4) after heating, the metal sleeve is unscrewed, the inner container is opened, and the instrument is used for measurement after dilution and volume fixing. Therefore, the existing closed sample dissolving device with the structure of the inner container and the outer steel sleeve and the matched sample digestion process have the following defects:

1) the sealing devices need to be assembled and disassembled one by one, the steps are complicated, and the operation intensity is high when samples are processed in a large batch; 2) the outer sleeve is made of metal materials, so that the outer sleeve is easy to corrode, and metal elements contained in the outer sleeve can pollute a sample when the outer sleeve is not operated properly; 3) when the electric heating plate is opened to catch acid, a large amount of acid steam is generated to pollute air and harm the health of operators; when the inner container is placed too densely or the heating temperature is too high, cross contamination among samples is easily caused; 4) various devices/devices such as an oven, an electric heating plate, a sealed steel sleeve, a ventilation safety cabinet and the like are required, and the occupied space is large.

Disclosure of Invention

In view of the above analysis, the present invention aims to provide a closed heating acid-removing device and an acid-removing method, so as to solve one or more of the problems that the acid vapor discharge of the closed sample-dissolving device of the existing "inner container + outer steel sleeve" structure is not thorough, flying dust pollution is easy to occur to harm the health of experimenters and cross contamination between samples, the operation steps are complicated, the operation strength is high, the outer steel sleeve is easy to corrode, the used equipment/device is various, and the occupied space is large.

The purpose of the invention is mainly realized by the following technical scheme:

in one aspect, a closed heating acid-dispelling device is provided, which includes:

the sample dissolving tank comprises a tank body and a cover body;

the heating table is provided with a plurality of sample dissolving tank mounting holes and is used for heating the sample dissolving tanks loaded in the sample dissolving tank mounting holes;

the acid steam collecting and processing assembly comprises an acid steam collecting plate, and the acid steam collecting plate is detachably mounted on the heating table and can seal the tank opening of the tank body; the acid vapor collecting plate is provided with an acid vapor collecting channel which is communicated with the tank body and used for collecting and treating the generated acid vapor.

The invention further comprises a fixed sealing assembly, and the fixed sealing assembly is used for sealing the tank body and the cover body when the sample is dissolved.

According to a preferred embodiment of the invention, the fixed sealing assembly comprises a fixed cover plate, a fixed bolt and a closed bolt, wherein the fixed cover plate is connected with the metal base through the fixed bolt, and the fixed cover plate is in a suspended state relative to the metal base; the fixed cover plate is provided with first screw holes with the same number as the sample dissolving tank mounting holes, and the sealing bolt tightly pushes the cover body through the first screw holes to seal the tank body and the cover body.

In a preferred embodiment of the present invention, the acid vapor collection and treatment device includes a buffer bottle, an alkaline solution bottle, and a jet pump, and the buffer bottle, the alkaline solution bottle, and the jet pump are sequentially disposed along an acid vapor outflow direction.

In a preferred embodiment of the present invention, the acid vapor collecting channel includes:

a needle valve used for adjusting air inflow is arranged at one end of the main pipeline, and the other end of the main pipeline is communicated with the acid steam treatment device;

the first end of the branch pipeline is communicated with the main pipeline, and the second end of the branch pipeline is communicated with the tank body.

In a preferred embodiment of the present invention, the branch pipe has a branch pipe inlet and a branch pipe outlet, and the acid vapor enters the branch pipe through the branch pipe inlet and enters the main pipe through the branch pipe outlet; the cross section of the outlet of the branch pipeline is of an inverted splayed structure.

According to a preferred embodiment of the invention, an outer flange structure is arranged at the opening of the tank body, the outer diameter of the outer flange structure is larger than the aperture of the sample dissolving tank mounting hole, and the outer diameter of the tank body is equal to the aperture of the sample dissolving tank mounting hole; the bottom surface of sour steam collecting plate is equipped with jar mouth packaging structure, and jar mouth packaging structure includes sealed annular, and outer flange structure can seamless installation in sealed annular.

In a preferred embodiment of the present invention, the top surface of the outer flange structure comprises a first top platform, a second top platform and a sloping wall which are connected in a transition manner; the first top surface platform is higher than the second top surface platform, the first top surface platform is positioned at the outer side, and the second top surface platform is positioned at the inner side.

In a preferred embodiment of the present invention, the heating stage includes: the sample dissolving tank mounting holes are uniformly distributed on the metal base, and the fixed cover plate is detachably connected with the metal base; the heating device is provided with a heating space, the metal base is detachably arranged in the heating space, and the heating device is used for heating the sample dissolving tank on the metal base; and the controller controls the heating device to heat according to a set program.

In a preferred embodiment of the present invention, the heating device includes a bottom wall and a side wall, the bottom wall and the side wall enclosing a heating space; the bottom wall and/or the side wall are provided with electric heating plates.

In a preferred embodiment of the invention, the bottom wall is provided with an electric heating plate, and the side wall is a polytetrafluoroethylene vertical plate; mounting holes are formed in the periphery of the electric heating plate on the bottom wall, and the side wall of the electric heating plate is inserted into the mounting holes; the height of the polytetrafluoroethylene vertical plate is more than or equal to that of the metal base.

In a preferred embodiment of the invention, the closed heating acid-dispelling device further comprises a heating cover plate, and the heating cover plate is detachably mounted above the acid steam collecting plate and used for heating during acid discharge.

In a preferred embodiment of the present invention, a backing plate made of teflon is further disposed on the top surface of the metal base, and the backing plate is located between the lower end of the outer flange structure and the top surface of the metal base.

On the other hand, the integrated closed sample dissolving method is also provided, and the closed heating acid removing device comprises the following steps:

sealing the sample dissolving tank on the metal base by using a fixed sealing assembly, starting a heating switch, dissolving the sample according to a preset program, and closing the heating switch after completing the sample dissolving;

the fixed sealing assembly is detached, the cover body is opened, the tank body is fixed on the metal base in a sealing mode through the acid vapor collecting plate, and the acid vapor treatment device is connected to an acid outlet of the acid vapor collecting plate;

and opening a heating switch to finish acid removal according to a preset heating program.

Compared with the prior art, the invention has at least one of the following beneficial effects:

A) according to the closed heating acid-removing device, acid-removing, acid-collecting and acid-treating are realized in a closed environment by utilizing the pipeline system of the acid vapor collecting and treating component, so that all acid vapor is collected and treated, dependence on a ventilation safety cabinet is eliminated, and zero emission of toxic gas is basically realized; and simple structure, the processing degree of difficulty is low, small, use equipment is few, and the cross contamination risk is low, can carry out a plurality of samples simultaneously and dissolve the appearance and catch up with sour, and operating strength is low, promotes experiment efficiency of software testing by a wide margin, accords with green, high-efficient, convenient analysis and test technical development theory, has great popularization potentiality in the production of mining industry and scientific research laboratory.

B) According to the closed heating acid-removing device provided by the invention, the outer flange structure is arranged at the pipe orifice of the sample dissolving tank, the sealing ring groove which is matched with the outer flange structure in the direction towards the bottom surface of the acid steam collecting plate is arranged on the bottom surface of the acid steam collecting plate, the outer flange structure can be seamlessly arranged in the sealing ring groove, the first top surface platform, the second top surface platform and the inclined wall of the outer flange structure can bear pressure and are sealed, a three-level dense structure is formed with the bottom of the sealing ring groove, and the sealing contact area of the sealing ring groove and the mouth of the sample dissolving tank is far larger than that of the inner container of a common sample dissolving.

C) According to the closed heating acid removing device provided by the invention, the heating table adopts a well-type furnace structure, the heating table is provided with a plurality of sample dissolving tank mounting holes, and one heating table is used for completing heating digestion, acid removing and re-dissolving of a plurality of samples, so that the number of instruments/devices is reduced, the occupied space is reduced, the test efficiency is greatly improved, and the bolt can be rotated by using a pistol drill, so that the sample dissolving tank can be quickly closed and opened, and the operation intensity is reduced.

D) According to the closed heating acid-dispelling device provided by the invention, the heating cover plate is arranged above the acid vapor collecting plate, heating is carried out during acid dispelling, the heating temperature is higher than the boiling point of an acid reagent, so that condensation backflow of high-boiling-point acid in the acid vapor collecting channel due to too low temperature is effectively prevented, and the acid-dispelling effect is ensured.

E) According to the closed heating acid-dispelling device provided by the invention, the base plate made of polytetrafluoroethylene is arranged on the upper surface of the metal base, the outer flange structure of the tank opening of the tank body can be clamped on the polytetrafluoroethylene base plate, and the base plate made of polytetrafluoroethylene has the following effects and effects: on the first hand, the protective layer plays a role in buffering, so that the sealing contact between the outer flange structure at the opening of the tank and the base plate is better, the deformation of the outer flange structure of the sample dissolving tank is effectively prevented, and acid liquor is prevented from leaking to corrode the metal base; the second aspect is used as an isolation layer, so that the direct contact of the tank opening with the metal base when the sample solution is poured can be avoided, and the sample pollution risk is eliminated; and the third aspect is used as a heat-insulating layer, so that the heat loss of the top surface of the metal base is reduced, the temperature uniformity of the metal base is improved, and the energy consumption is reduced.

In the invention, the technical schemes can be combined with each other to realize more preferable combination schemes. Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and drawings.

Drawings

The drawings are only for purposes of illustrating particular embodiments and are not to be construed as limiting the invention, wherein like reference numerals are used to designate like parts throughout.

FIG. 1 is a schematic structural diagram of a closed heating digestion device in the embodiment of the invention;

FIG. 2 is a schematic structural diagram I of a sample dissolving tank mounted on a closed heating digestion device in the embodiment of the invention;

FIG. 3 is a schematic structural diagram II of a sample dissolving tank mounted on a closed heating digestion device in the embodiment of the invention;

FIG. 4 is a schematic structural diagram of a metal base according to an embodiment of the present invention;

FIG. 5 is a schematic view of a connection between a fixed cover and a metal base according to an embodiment of the present invention;

FIG. 6 is a schematic diagram of a position-limiting structure of the fixing cover plate and the metal base according to the embodiment of the present invention;

FIG. 7 is a schematic structural diagram of a sample dissolving tank according to an embodiment of the present invention;

FIG. 8 is a schematic structural view of a can body according to an embodiment of the present invention;

FIG. 9 is a schematic structural diagram of a cover according to an embodiment of the present invention;

FIG. 10 is a schematic diagram of a closed heating acid-removing device according to an embodiment of the present invention;

FIG. 11 is a cross-sectional view of a portion of a closed heating acid-removing device according to an embodiment of the present invention;

fig. 12 is a schematic structural diagram of a spout packaging structure of an acid vapor collecting plate according to an embodiment of the present invention.

Reference numerals:

1. a sample dissolving tank; 1-1, a tank body; 1-1-1, an outer flange structure; 1-1-1-1, a first vertical wall; 1-1-1-2, a second vertical wall; 1-1-1-3, inclined wall; 1-1-1-4, a first top platform; 1-1-1-5, a second top platform; 1-2, a cover body; 1-2-1, a first seal portion; 1-2-2, a second sealing part; 1-2-3, a first seal ring groove; 1-2-4, a first concave groove; 2. a metal base; 2-1, a sample dissolving tank mounting hole; 2-2, a second screw hole; 2-3, positioning a groove; 2-4, a limit inserting part; 3. a heating device; 4. a controller; 5. a base plate; 6. fixing the cover plate; 6-1, a first screw hole; 6-2, positioning protrusions; 6-3, a first positioning pin hole; 7. fixing the bolt; 7-1 card part; 7-2-nut; 7-3, supporting the sleeve; 7-4, a screwing part; 8. closing the bolt; 9. positioning pins; 10. an acid vapor collection plate; 10-1, a main pipeline; 10-2, branch pipelines; 10-2-1, a branch pipeline outlet; 10-3, a can opening packaging structure; 10-3-1, a third sealing part; 10-3-2, a fourth sealing part; 10-3-3, a second seal ring groove; 10-3-4, a second concave groove; 11. heating the cover plate; 12. a connecting pipe; 13. a buffer bottle; 14. alkali solution bottles; 15. a jet pump.

Detailed Description

The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate preferred embodiments of the invention and together with the description, serve to explain the principles of the invention and not to limit the scope of the invention.

Example 1

A specific embodiment of the present invention discloses a closed heating digestion apparatus, as shown in fig. 1 to 3, the closed heating digestion apparatus comprising: the device comprises a heating table, a sample dissolving tank 1 and a fixed sealing assembly; wherein, the heating table is provided with a plurality of sample dissolving tank mounting holes 2-1; the sample dissolving tank 1 comprises a tank body 1-1 and a cover body 1-2, the sample dissolving tank 1 is made of polytetrafluoroethylene materials, the sample dissolving tank 1 is detachably mounted in a sample dissolving tank mounting hole 2-1, and a heating table is used for heating a plurality of sample dissolving tanks 1 mounted in the sample dissolving tank mounting holes 2-1; the fixed sealing assembly comprises a fixed cover plate 6 and a sealing bolt 8, the fixed cover plate 6 is positioned above the heating table and connected with the heating table, the fixed cover plate 6 is provided with first screw holes 6-1 with the same number as the sample dissolving tank mounting holes 2-1, and the sealing bolt 8 penetrates through the first screw holes 6-1 to tightly push the cover body 1-2 so as to seal the tank body 1-1 and the cover body 1-2.

In this embodiment, the heating table includes a metal base 2, a heating device 3 and a controller 4, wherein the heating device 3 is provided with a heating space, and the metal base 2 is detachably mounted in the heating space; as shown in fig. 4, a plurality of sample dissolving tank mounting holes 2-1 are uniformly formed in a metal base 2, and a fixed cover plate 6 is connected with the metal base 2; the controller 4 is used for controlling the heating device 3 to heat the sample dissolving tank 1 on the metal base 2 according to a set program.

In this embodiment, the fixed sealing assembly further includes a positioning member, the metal base 2 is provided with a positioning slot 2-3 adapted to the positioning member, and the positioning member is installed in the positioning slot 2-3 to position the fixed cover plate 6.

Specifically, the positioning piece comprises the following two structures:

the positioning piece of the first structure is a positioning pin 9, the fixed cover plate 6 is provided with a first positioning pin hole 6-3, the diameter of the positioning pin 9 is equal to the groove diameter of the positioning groove 2-3 and the aperture of the first positioning pin hole 6-3, and the positioning pin 9 penetrates through the first positioning pin hole 6-3 and is arranged in the positioning groove 2-3 to position the fixed cover plate 6.

The positioning element of the second structure is a positioning protrusion 6-2, as shown in fig. 6, the positioning protrusion 6-2 is integrally formed on the bottom surface of the fixed cover plate 6, and the height of the positioning protrusion 6-2 is greater than the depth of the positioning groove 2-3 on the metal base 2. On one hand, the positioning bulge 6-2 and the fixed cover plate 6 are integrally formed, so that the number of parts is reduced, and the assembly and disassembly are more convenient; on the other hand, the height of the positioning bulge 6-2 is larger than the depth of the positioning groove 2-3, so that the fixed cover plate 6 is in a suspended state, the enough screwing-in distance of the sealing bolt 8 can be ensured, and the fixed cover plate can be matched with the fixing bolt 7, so that the connection stability of the fixed cover plate 6 and the metal base 2 is improved.

In this embodiment, after the fixed cover plate 6 is connected and fixed with the metal base 2, the fixed cover plate 6 and the top surface of the metal base 2 have the following two positional relationships:

in the first position relation, a certain distance is reserved between the fixed cover plate 6 and the top surface of the metal base 2, the fixed cover plate 6 is in a suspended state, the distance is used for screwing the sealing bolt 8, the height of the tank body 1-1 is smaller than or equal to the hole depth of the sample dissolving tank mounting hole 2-1, after the sample dissolving tank 1 is filled into the sample dissolving tank mounting hole 2-1, the outer flange of the tank opening is clamped at the filling opening of the sample dissolving tank mounting hole 2-1, and a gap is reserved between the cover body 1-2 and the fixed cover plate 6. According to the structure, at least part of the tank body 1-1 is positioned above the top surface of the metal base 2, so that the sample dissolving tank 1 can be conveniently installed and taken out.

In the second position relation, the fixed cover plate 6 is in direct contact with the top surface of the metal base 2, the hole depth of the sample dissolving tank mounting hole 2-1 is larger than the overall height of the sample dissolving tank 1, the whole sample dissolving tank 1 can be completely filled into the sample dissolving tank mounting hole 2-1, the cover body 1-2 of the sample dissolving tank 1 is located a certain distance below the orifice of the sample dissolving tank mounting hole 2-1, and the distance is used for screwing in of the sealing bolt 8. According to the structure, the tank body 1-1 and the cover body 1-2 are both positioned in the sample dissolving tank mounting hole 2-1, and the cover body cannot deviate in the jacking process of the sealing bolt 8, so that the sealing effect is ensured.

In this embodiment, the connection manner of the fixed cover 6 and the metal base 2 includes, but is not limited to, the following connection manners:

the first connection relation of the fixed cover plate 6 and the metal base 2, the fixed cover plate 6 is connected with the metal base 2 through a fixing bolt 7. Specifically, the top surface of the metal base 2 is provided with a plurality of second screw holes 2-2, the number of the second screw holes 2-2 is 6, the second screw holes are dispersedly arranged on the top surface of the metal base 2, four corners of the top surface of the metal base 2 are respectively provided with 1, and the middle part of the top surface of the metal base 2 is uniformly distributed with 2; the fixed cover plate 6 is provided with a third screw hole matched with the second screw hole 2-2, and the fixed bolt 7 penetrates through the third screw hole of the fixed cover plate 6 to be fixedly connected with the metal base 2. Adopt fixing bolt 7 to be connected fixed apron 6 and metal base 2, dismouting convenient operation, spare part processing is simple, and cost of manufacture and device maintenance are with low costs.

The second connection relation of the fixed cover plate 6 and the metal base 2, and the fixed cover plate 6 is fixedly connected with the metal base 2 through a fastener. Specifically, the buckle piece comprises a buckle ring and a buckle column, the buckle column is fixedly arranged on the outer peripheral edge of the metal base 2, one end of the buckle ring is rotatably connected to the fixed cover plate 6, and the other end of the buckle ring is buckled with the buckle column. The mode that adopts the buckle to connect, convenient operation, the simple structure of buckle spare, the cost of manufacture is low, moreover buckle ring and buckle post respectively with fixed cover plate 6 on with metal base 2 on, can avoid the part to lose.

In a third connection relationship between the fixed cover plate 6 and the metal base 2, as shown in fig. 5, the metal base 2 is provided with two limit insertion parts 2-4, the two limit insertion parts 2-4 are arranged in parallel, the fixed cover plate 6 is connected with the metal base 2 through the limit insertion parts 2-4, and the limit insertion parts 2-4 are used for limiting the movement of the fixed cover plate 6 in the vertical direction. Specifically, two limiting insertion parts 2-4 are symmetrically arranged on two side edges of the top surface of the metal base 2, limiting sliding grooves are formed in the limiting insertion parts 2-4 and are parallel to the top surface of the metal base 2, and the fixed cover plate 6 is inserted into the limiting sliding grooves in a sliding mode.

In a preferred embodiment of the third connection relationship, the height of the limiting chute is equal to the thickness of the fixed cover plate 6, and the top surface and the bottom surface of the fixed cover plate 6 are in direct contact with the chute wall of the limiting chute; if a backing plate 5 is further arranged between the fixed cover plate 6 and the top surface of the metal base 2, the height of the limiting sliding groove is equal to the sum of the thicknesses of the fixed cover plate 6 and the backing plate 5. After the fixed cover plate 6 is arranged in the limiting insertion parts 2-4, the limiting sliding grooves can effectively limit the fixed cover plate 6 to move in the vertical direction, and the sealing effect is prevented from being influenced due to the fact that the fixed cover plate 6 moves in the vertical direction in the experiment process.

In a preferred embodiment of the third connection relationship, the limiting insertion-connection part 2-4 is a rectangular cylinder structure, the limiting sliding groove is arranged in the middle of the side surface of the rectangular cylinder, the side surface is perpendicular to the top surface of the metal base 2, the two limiting sliding grooves are oppositely arranged, and the distance between the two limiting sliding grooves is equal to the width of the fixed cover plate 6; fixed apron 6 slides and pegs graft in spacing spout after, the bottom surface of fixed apron 6 apart from 2 top surfaces of metal base by a certain distance, and the bottom surface of fixed apron 6 does not directly contact with the top surface of metal base 2, and fixed apron 6 is unsettled state for the top surface of metal base 2. During installation, two side edges of the fixed cover plate 6 are inserted into the limiting sliding grooves, the fixed cover plate 6 is pushed to slide in the limiting sliding grooves, along with continuous sliding of the fixed cover plate 6 along the limiting sliding grooves, when the first positioning pin holes 6-3 are aligned with the positioning grooves 2-3 at the corresponding positions on the metal base 2, the fixed cover plate 6 is installed in place, the positioning pins 9 are arranged into the first positioning pin holes 6-3 and the positioning grooves 2-3, and the two positioning pins are positioned.

In this embodiment, after the fixed cover plate 6 is connected and fixed with the metal base 2, when the fixed cover plate 6 has the first positional relationship with the top surface of the metal base 2, that is, a certain distance is formed between the fixed cover plate 6 and the top surface of the metal base 2, and the fixed cover plate 6 is in a suspended state.

When fixed apron 6 and metal base 2 adopt first connected mode, adopt fixing bolt 7 to be connected fixed apron 6 and metal base 2 promptly, fixing bolt 7 can adopt following three kinds of structures:

the fixing bolt of the first structure comprises a bolt rod, wherein the middle of the bolt rod is a smooth rod, the two ends of the bolt rod are respectively provided with a top screw rod and a bottom screw rod in an integrated mode, the rod diameter of the smooth rod is larger than that of the top screw rod and that of the bottom screw rod, a limiting boss is formed at the connecting end face of the smooth rod, the top screw rod is matched with a third screw hole in a fixing cover plate 6, and the bottom screw rod is matched with a second screw hole 2-2 in a metal base 2. During installation, the bottom end screw is firstly installed into the second screw hole 2-2 and screwed, the sample dissolving tank 1 is installed into the sample dissolving tank installation hole 2-1, then the third screw hole of the fixing cover plate 6 is sleeved on the top end screw, the nut is installed on the top end screw and screwed, the top end screw fixes the fixing cover plate 6 through the limiting boss and the nut to limit the up-and-down movement of the fixing cover plate 6, and therefore the connection of the fixing cover plate 6 and the metal base 2 is completed. Optionally, the nut is a butterfly tail nut, so that the hand can conveniently twist.

In the bolt with the second structure, as shown in fig. 2, the middle of the bolt rod is a smooth rod, the two ends of the bolt rod are respectively provided with a top end screw rod and a bottom end screw rod in an integrated manner, the upper part of the bolt rod is provided with a clamping part 7-1, the clamping part 7-1 is in an annular structure and is fixedly arranged on the outer circumference of the bolt rod, the clamping part 7-1 is positioned at the boundary between the top end screw rod and the middle smooth rod, the size of the clamping part 7-1 is larger than the aperture of a third screw hole, and the clamping part 7-1 can be clamped at one side of the. During installation, the bottom end screw of the bolt rod is firstly installed into the second screw hole 2-2 and screwed, the sample dissolving tank 1 is already installed into the sample dissolving tank installation hole 2-1, then the third screw hole of the fixing cover plate 6 is sleeved on the top end screw, the nut 7-2 is installed on the top end screw and screwed, the fixing cover plate 6 is fixedly limited between the nut 7-2 and the clamping part 7-1, and connection of the fixing cover plate 6 and the metal base 2 is completed.

In the fixing bolt with the third structure, as shown in fig. 3, the fixing bolt 7 comprises a bolt rod, a support sleeve 7-3 is sleeved outside the bolt rod, the outer diameter of the support sleeve 7-3 is larger than the aperture of the second screw hole 2-2 and the aperture of the third screw hole, external threads are arranged at least at two ends of the bolt rod, the rod diameter of the screw rod at the top end of the bolt rod is matched with the second screw hole 2-2, and the rod diameter of the screw rod at the bottom end of the bolt rod is matched with the third screw hole. During installation, the supporting sleeve 7-3 is arranged between the fixing cover plate 6 and the metal base 2, the fixing bolt 7 sequentially penetrates through the third screw hole and the supporting sleeve 7-3 and is screwed into the second screw hole 2-2, and finally, under the limiting action of the supporting sleeve 7-3, the nut is installed on the top end screw rod and is screwed tightly, so that the fixing cover plate 6 is connected with the metal base 2. In order to facilitate screwing of the fixing bolt 7, the top end of the bolt rod of the fixing bolt 7 is also provided with a screwing part 7-4, the size of the screwing part 7-4 is larger than that of the bolt rod, optionally, the screwing part adopts a butterfly tail structure, can be directly screwed by hand, and is convenient and rapid to disassemble and assemble.

In this example, the first end of the sealing bolt 8 is provided with a screwing operation portion, the screwing operation portion is of a hexagonal cylinder structure, the size of the screwing operation portion is smaller than the size of a screw rod of the sealing bolt 8, the hexagonal cylinder structure is penetrated by the first screw hole 6-1, and quick disassembly can be achieved by using a matched outer hexagonal wrench or an electric screwdriver.

In order to improve the sealing performance of the sample dissolving tank, the second end of the sealing bolt 8 is provided with a limiting plate, the limiting plate and the sealing bolt 8 are integrally formed to ensure the connection strength, the limiting plate is perpendicular to the screw rod of the sealing bolt 8, and the area of the bottom surface of the limiting plate is greater than or equal to 1/2 of the area of the top surface of the cover body 1-2. After the sealing bolt 8 and the sealing tank 1 are installed, the planar projection of the limiting plate is at least partially overlapped with the projection of the top surface of the cover body 1-2, and the limiting plate has the same center, so that the acting force of the limiting plate on the cover body 1-2 is more uniform, the pressure acting on the cover body 1-2 can be reduced, the sealing effect is ensured, and meanwhile, the cover body 1-2 is prevented from deforming due to overlarge local pressure to influence the sealing effect.

In a preferred embodiment of this embodiment, the top surface of the cover body 1-2 is provided with a first alignment structure, the bottom surface of the limiting plate is provided with a first alignment structure matching portion, and the first alignment structure matching portion are matched to enable the center line of the cover body 1-2 to coincide with the center line of the sealing bolt 8, so that the cover body 1-2 and the limiting plate can be quickly and accurately mounted.

Specifically, the first alignment structure of the cover body 1-2 is a cover bulge, the first alignment structure matching part of the limiting plate is a closed limiting groove, the cover bulge can be seamlessly installed in the closed limiting groove, the cover bulge is arranged at the center of the top surface of the cover body 1-2, and the closed limiting groove is arranged at the center of the bottom surface of the limiting plate; or the first alignment structure of the cover body 1-2 is a cover groove, the first alignment structure matching part of the limiting plate is a closed limiting bulge, the closed limiting bulge is seamlessly installed in the cover groove, the cover groove is formed in the center of the cover body 1-2, and the closed limiting bulge is formed in the center of the bottom surface of the limiting plate. The design structure is simple, the processing is convenient, the manufacturing cost is low, the rapid and accurate contraposition installation of the limiting plate and the cover body 1-2 can be realized only by aligning the cover bulge and inserting the closed limiting groove or aligning the closed limiting bulge and inserting the closed limiting groove during the installation, and the operation is very convenient.

In a preferred embodiment of this embodiment, the first alignment structure is provided with a second alignment structure, and correspondingly, the first alignment structure engagement portion is provided with a second alignment structure engagement portion.

Specifically, when the first alignment structure is a cover bulge and the first alignment structure matching part is a closed limiting groove, the second alignment structure is a first central groove arranged at the center of the cover bulge, the second alignment structure matching part is a first central bulge arranged at the center of the closed limiting groove, and the first central bulge is matched with the first central groove; when the first alignment structure is a cover groove and the first alignment structure matching part is a closed limiting protrusion, the second alignment structure is a second central protrusion arranged at the center of the cover groove, the first alignment structure matching part is a second central groove arranged at the center of the closed limiting protrusion, and the second central protrusion is matched with the second central groove.

Through setting up the two-stage alignment structure, realized limiting plate and lid 1-2 accurate, quick counterpoint installation, guaranteed lid 1-2's atress distribution homogeneity, and then guaranteed sealed effect, the two-stage alignment structure adopts arch and recess cooperation moreover, simple structure, and the preparation is convenient, and is with low costs.

In this embodiment, as shown in fig. 7, the sample dissolving tank 1 includes a tank body 1-1 and a cover body 1-2, and the sample dissolving tank 1 is made of polytetrafluoroethylene and has a volume of 10-20ml, preferably 15 ml.

In a preferred embodiment of this embodiment, as shown in fig. 8, the mouth of the can body 1-1 is provided with an outer flange structure 1-1-1, the outer flange structure 1-1-1 can be clamped on the sample dissolving can mounting hole 2-1, the outer flange structure 1-1-1 is an annular structure having an inner side wall surface, an outer side wall surface and a top surface, the outer diameter of the outer flange structure 1-1-1 is greater than the outer diameter of the can body 1-1, and the outer diameter of the can body 1-1 is equal to the aperture of the sample dissolving can mounting hole 2-1; as shown in FIG. 9, a first sealing part 1-2-1 is arranged on the bottom surface of the cover body 1-2, the first sealing part 1-2-1 is of an annular structure, and the outer diameter of the first sealing part 1-2-1 is equal to the inner diameter of the opening of the can body 1-1. When the sample dissolving tank 1 is arranged in the base mounting hole 2-1, the outer flange structure 1-1-1 is clamped on the polytetrafluoroethylene base plate 5, so that the sample dissolving tank 1 is convenient to take and place, and the contact between a tank opening and a heating table can be avoided, thereby avoiding sample pollution; the outer flange structure 1-1-1 is sealed by the annular structure first sealing part 1-2-1 on the bottom surface of the cover body 1-2, a wide sealing area is formed by the outer flange structure, the sealing effect is better, only the outer flange part of the tank opening is stressed when the sealing bolt is pressurized, the side wall and the bottom of the tank body are not stressed, and the deformation of the tank body is effectively avoided.

In a preferred embodiment of this embodiment, as shown in fig. 9, the bottom surface of the lid body 1-2 is further provided with a second sealing portion 1-2-2, the second sealing portion 1-2-2 is an annular structure, the second sealing portion 1-2-2 and the first sealing portion 1-2-1 form a first sealing ring groove 1-2-3 for accommodating the outer flange structure 1-1-1, and the bottom of the first sealing ring groove 1-2-3 applies downward pressure to the top of the outer flange structure 1-1-1 under the pressurization effect of the closing bolt 8 by the lid body 1-2, so that the side wall and the bottom of the first sealing ring groove 1-2-3 are in sealing contact with the inner and outer side wall surfaces and the top surface of the outer flange structure 1-1-1. When the closing bolt 8 downwards extrudes the cover body 1-2, the first sealing part 1-2-1 applies an outward acting component force to the outer flange structure 1-1-1, meanwhile, the second sealing part 1-2-2 applies an inward acting component force to the outer flange structure 1-1-1, and the groove bottom of the first sealing ring groove 1-2-3 applies a downward acting component force to the outer flange structure 1-1-1, so that the sealing contact area between the sealing structure of the cover body 1-2 and the opening of the sample dissolving tank 1 is increased by arranging the first sealing ring groove 1-2-3 on the bottom surface of the cover body 1-2, and the sealing effect is greatly improved.

In a preferred embodiment of this embodiment, on a longitudinal section, the top of the outer flange structure 1-1-1 is configured to be an upward convex arc structure, and the bottom of the first sealing ring groove 1-2-3 is configured to be an inward concave arc structure, that is, the top surface of the outer flange structure 1-1-1 is an upward convex arc surface, and the bottom of the first sealing ring groove 1-2-3 is an inward concave arc surface. The top of the outer flange structure 1-1-1 and the bottom of the first sealing ring groove 1-2-3 are arranged to be of matched arc structures, so that the sealing contact area between the sealing ring groove 1-2-3 of the cover body 1-2 and the opening of the sample dissolving tank 1 is further increased, and the sealing effect is improved.

In a preferred embodiment of this embodiment, the groove bottom concave arc structure of the first sealing ring groove 1-2-3 is an asymmetric structure, the lowest concave point of the concave arc structure is located on one side of the centerline of the concave arc structure and is close to the second sealing portion 1-2-2, and correspondingly, the convex arc structure at the top of the outer flange structure 1-1-1 is an asymmetric structure and is adapted to the first sealing ring groove 1-2-3 with an asymmetric structure. Specifically, the lower part of the outer side wall of the outer flange structure 1-1-1 is provided with a first vertical wall 1-1-1-1, the lower part of the inner side wall of the outer flange structure 1-1-1 is provided with a second vertical wall 1-1-1-2, the length of the first vertical wall 1-1-1-1 is greater than that of the second vertical wall 1-1-1-2, the top end of the second vertical wall 1-1-1-2 is positioned below the top end of the first vertical wall 1-1-1-1, and the first vertical wall 1-1-1 and the second vertical wall 1-1-1-2 are in transition connection through a circular arc surface; the inner side wall of the second sealing part 1-2-2 and the outer side wall of the first sealing part 1-2-1 are provided with vertical walls, and the lower end of the first sealing part 1-2-1 is lower than the lower end of the second sealing part 1-2-2; the top surface of the outer flange structure 1-1-1 comprises a first top surface platform 1-1-1-4, a second top surface platform 1-1-1-5 and an inclined wall 1-1-1-3, the first top surface platform 1-1-4 is higher than the second top surface platform 1-1-1-5, the first top surface platform 1-1-1-4 is positioned at the outer side, the second top surface platform 1-1-5 is positioned at the inner side, the groove bottom of the first sealing ring groove 1-2-3 is provided with a first plane, a second plane and an inclined surface which are matched with the first top surface platform 1-1-4, the second top surface platform 1-1-1-5 and the inclined wall 1-1-1-3, the three parts of the outer flange structure can be sealed in a pressure-bearing mode, and a first top surface platform 1-1-1-4, a second top surface platform 1-1-1-5, an inclined wall 1-1-1-3 and a first sealing ring groove 1-2-3 of a cover body 1-2 form a three-level dense structure. After the outer flange structure 1-1-1 of the tank body 1-1 is arranged in the first sealing ring groove 1-2-3 of the cover body 1-2, the lower end of the first sealing part 1-2-1 extends into the tank opening of the tank body 1-1; the lower end of the second sealing part 1-2-2 is higher than the lower end face of the outer edge of the outer flange structure 1-1-1, the bottom of the first sealing ring groove 1-2-3 applies downward pressure to the top face of the outer flange structure 1-1-1 by the cover body 1-2 under the pressurization effect of the sealing bolt 8, so that the first top surface platform 1-1-1-4, the second top surface platform 1-1-5 and the inclined wall 1-1-1-3 of the outer flange structure 1-1-1 extrude the bottom of the first sealing ring groove 1-2-3, the three parts can be sealed under pressure, the area of the sealing area is far larger than the sealing area of the inner container of the conventional sample dissolving bomb, and the sealing effect is better.

In a preferred embodiment of this embodiment, the bottom of the can body 1-1 is an inwardly concave arc-shaped bottom, the bottom surface of the cover body 1-2 is provided with a first concave groove 1-2-4, and the wall of the first concave groove 1-2-4 forms a first sealing portion 1-2-1. The tank bottom of the tank body 1-1 and the bottom surface of the cover body 1-2 are arranged to be of concave arc structures, so that the volume is increased, the stress surface is enlarged, the concave arc tank bottom has stronger structural integrity, the pressure applied to the arc top can be distributed to the edge, the stress is dispersed, the pressure is reduced, and the structure of the tank body is firmer; the concave arc-shaped tank bottom can enable a small amount of residual liquid to be gathered at the concave tank bottom, so that the liquid can be easily used up, the liquid is not left, the sample utilization rate is improved, no dead angle exists in the sample dissolving tank, and the sample dissolving tank is convenient to clean.

In a preferred embodiment of this embodiment, a backing plate 5 is detachably mounted between the metal base 2 and the fixed cover plate 6, the backing plate 5 is made of polytetrafluoroethylene, the backing plate 5 is provided with a sample dissolving tank through hole corresponding to the sample dissolving tank mounting hole 2-1, and an outer flange structure 1-1-1 at a tank opening of the tank body 1-1 can be clamped on the sample dissolving tank through hole. The polytetrafluoroethylene backing plate 5 has the following functions and effects: on the first hand, the protective layer plays a role in buffering, so that the sealing contact between the outer flange structure at the opening of the tank and the base plate is better, the deformation of the outer flange structure of the sample dissolving tank is effectively prevented, and acid liquor is prevented from leaking to corrode the metal base; the second aspect is used as an isolation layer, so that the direct contact of the tank opening with the metal base when the sample solution is poured can be avoided, and the sample pollution risk is eliminated; and the third aspect is used as a heat-insulating layer, so that the heat loss of the top surface of the metal base is reduced, the temperature uniformity of the metal base is improved, and the energy consumption is reduced.

Of course, it can be understood that a plurality of through holes/screw holes can be adaptively formed on the backing plate 5 according to the connection and limiting manner of the fixing cover plate 6 and the metal base 2. Illustratively, the backing plate 5 is provided with a positioning through hole and a fourth screw hole which correspond to the positioning groove and the second screw hole 2-2 on the metal base 2, and a thermocouple temperature measuring hole can be arranged according to temperature measuring requirements.

In this embodiment, the heating table is provided with a thermocouple for measuring the temperature of each part of the metal base 2; the controller 4 has a programming control function and an over-temperature power-off protection function, and the controller 4 is connected with the thermocouple and the heating device 3 through a signal line, collects temperature measurement information of the thermocouple, and controls the heating device 3 to heat. Wherein, the heating device 3 can be provided with a heating switch alone, and the controller 4 can also be used for controlling the on and off of the heating device 3.

In a preferred embodiment of this embodiment, two sets of independently controllable heating components are disposed at the periphery and middle of the electric heating plate, and 2-3 sets of temperature thermocouples are disposed at the edge and middle of the metal base 2, so as to measure and control temperature respectively, compensate heat loss at the periphery of the metal base 2, and improve consistency of sample dissolving effect.

In a preferred embodiment of this embodiment, the heating device 3 of the heating platform comprises a bottom wall and a side wall, the bottom wall and the side wall enclose a heating space to form a well-type heating furnace structure, and the bottom wall and/or the side wall of the heating device 3 are/is provided with electric heating plates.

In a preferred embodiment of the present invention, an electric heating plate is laid on the bottom wall of the heating device 3, or the electric heating plate is used as the bottom wall of the heating device 3; the diapire electric plate set up the mounting hole all around, and the lateral wall cartridge is at the mounting hole, and wherein, the lateral wall adopts the polytetrafluoroethylene riser, the height more than or equal to metal base 2 of polytetrafluoroethylene riser for the polytetrafluoroethylene riser forms the well formula structure of surrounding metal base 2, and the polytetrafluoroethylene riser plays thermal-insulated effect, can reduce base 2 heat loss all around, improves the temperature homogeneity of base 2, guarantees that 2 each positions of base dissolve the appearance effect unanimously, and processing is simple moreover, and is with low costs.

In a preferred embodiment of the present invention, the bottom wall and the side walls of the heating device 3 are provided with electric heating plates, the electric heating plates of the bottom wall and the side walls surround the base 2, that is, the heating space is defined by the side electric heating plates and the bottom electric heating plate, the base 2 is installed in the heating space and contacts with the inner wall of the rectangular heating space, and the height of the electric heating plates of the side walls is the same as that of the base 2. Through the bottom at base 2 with set up the hot plate all around, can guarantee that base 2's each position temperature is unanimous basically for it is even to dissolve appearance jar 1 and be heated, guarantees even heating and dissolves an appearance effect. The outer walls of the side electric heating plates and the bottom electric heating plate are wrapped with heat insulation material layers so as to reduce heat loss.

In a preferred embodiment of this embodiment, the metal base 2 is a cylinder structure, and the heating space is a cylindrical space, or the metal base 2 is a cuboid structure, and the heating space is a cuboid space, and the heating space of the heating device 3 is matched with the structural size of the base 2. Optionally, the metal base 2 is of a cuboid structure, the number of the metal bases 2 is two, the volume of the two metal bases 2 is equal to the volume of the heating space, the two metal bases 2 can adopt the same fixed cover plate 6, and the fixed cover plate 6 can be independently arranged for each metal base 2. For example, 20 sample dissolving tank mounting holes are formed in the metal base 2, and 20 sample dissolving tanks can be mounted, so that a sample dissolving process of 20 samples can be simultaneously realized at one time. More groups of samples can be dissolved simultaneously by arranging the two metal bases 2, so that the test efficiency is greatly improved.

In this embodiment, fixed apron 6, metal base 2 all adopt the aluminum alloy material, and anodic oxidation is done on the surface and is handled, have guaranteed metal base 2 and fixed apron 6 joint strength, can also avoid metal oxidation, corruption, have promoted sealed effect and have prolonged life.

The closed heating digestion device for sample dissolution comprises the following steps:

the method comprises the following steps: adding an acid reagent and a solid sample to be dissolved into a sample dissolving tank 1, and packaging by using a cover body 1-2; a plurality of sample dissolving pots 1 containing an acid reagent and a solid sample to be dissolved are fitted into sample dissolving pot fitting holes 2-1 of a metal base 2.

Step two: fixedly connecting a fixed cover plate 6 with a metal base 2, aligning a first screw hole 6-1 of the fixed cover plate 6 with a sample dissolving tank mounting hole 2-1, reserving a space between the fixed cover plate 6 and the top surface of the metal base 2, and enabling the fixed cover plate 6 to be in a suspended state relative to the top surface of the metal base 2;

step three: and (3) penetrating the sealing bolt 8 through the first screw hole 6-1 to prop against the cover body 1-2, and screwing the sealing bolt 8 by using a pistol drill to seal the tank body 1-1 and the cover body 1-2.

Step four: and (3) starting a heating switch of the electric heating plate 3, heating the sealed sample dissolving tank 1 through the metal base 2, starting to dissolve the sample, and heating to the preset time to complete sample dissolving.

Step five: after the sample is dissolved, the fixed cover plate 6 is detached, and subsequent acid removal and redissolution operations are carried out.

In the second step, the fixed cover plate 6 and the metal base 2 are fixedly connected by the following three connection methods: the fixed cover plate 6 is connected with the metal base 2 through a fixed bolt 7, the fixed cover plate 6 is fixedly connected with the metal base 2 through a buckle piece, and the fixed cover plate 6 is connected with the metal base 2 through a limiting insertion part 2-4 arranged on the metal base 2.

In the second step, in the process of fixedly connecting the fixed cover plate 6 with the metal base 2, a positioning element (such as a positioning pin 9 or a positioning protrusion 6-2) is inserted into a positioning groove 2-3 arranged on the metal base 2, and the fixed cover plate 6 is installed at a proper position to ensure that a first screw hole 6-1 of the fixed cover plate 6 is aligned with the sample dissolving tank installation hole 2-1.

In step three, if adopt the sealing bolt 8 that sets up the limiting plate, also the first end of sealing bolt 8 is equipped with soon twists the operation portion, and the second end of sealing bolt 8 sets up the limiting plate. During installation, the screwing operation part at the first end of the sealing bolt 8 penetrates through the first screw hole 6-1 from bottom to top, the center of the limiting plate is approximately aligned with the first alignment structure on the cover body 1-2, the position of the limiting plate is adjusted, the first alignment structure matching part arranged on the bottom surface of the limiting plate is aligned with the first alignment structure, the sealing bolt 8 is screwed after alignment, and the tank body 1-1 and the cover body 1-2 of the sample dissolving tank 1 are sealed under the action of the jacking force of the sealing bolt 8. And sealing operation of all the sample dissolving tanks 1 is completed in sequence.

In the fourth step, a heating program can be preset, and the system can automatically measure and control, and the temperature is raised in a programmed way, wherein the maximum temperature is 220 ℃. And (3) controlling the heating speed, digestion time and temperature according to different samples and acid reagents, such as: silicate sample, hydrofluoric acid-nitric acid system, temperature rise rate: 5 ℃/min, digestion temperature: digestion time at 210 ℃: 24 hours; sulfide sample, aqua regia system, rate of temperature rise: 3 ℃/min, digestion temperature of 200 ℃, digestion time: 24 hours; chromite and other insoluble oxides, and the temperature rise speed is as follows: 5 ℃/min, digestion temperature: digestion time at 220 ℃: 48 hours; plant sample, hydrofluoric acid-nitric acid system, temperature rise rate: 3 ℃/min, digestion temperature: digestion time at 180 ℃: for 12 hours. The closed heating digestion device can meet the requirement of digestion of various types of samples, and the digestion effect of the samples is better according to the setting of the parameters.

Compared with the prior art, the airtight heating digestion device that this embodiment provided, simple structure, it is small, required corollary equipment is few, can carry out a plurality of samples simultaneously and dissolve the appearance, and operating strength is low, has overcome that there is the defect such as loaded down with trivial details, operating strength is big, the outer steel bushing is easily corroded in current airtight heating digestion device of "inner bag + outer steel bushing" formula. Adopt fixed seal assembly to replace traditional outer steel bushing seal form, every dissolves a kind jar and adopts independent blind bolt to seal, greatly reduced operating strength, showing and promoting sealed effect, metal seal assembly does not dissolve a kind jar mouth direct contact moreover, can not corrode metal fixed seal assembly, therefore pollution-free sample guarantees the reliability of test result. In addition, an outer flange structure is arranged at the opening of the sample dissolving tank, the bottom surface of the cover body is provided with a first sealing ring groove structure matched with the outer flange structure, the sealing contact area of the sealing structure of the cover body and the opening of the sample dissolving tank is increased, and the sealing effect is greatly improved. The fixed seal assembly adopts the airtight appearance jar that dissolves of structure of "bolt + support", utilizes the rotary bolt of pistol drill, realizes dissolving quick airtight and the opening of appearance jar, has reduced manipulation strength.

Example 2

The invention further discloses a closed heating acid-removing device, which is matched with the closed heating digestion device in the embodiment 1 for use, and after the closed heating digestion device is used for completing sample digestion, the closed heating acid-removing device in the embodiment is used for carrying out acid-removing treatment on the solution in the sample dissolving tank 1.

A closed sample dissolving and acid removing device of the present embodiment, as shown in fig. 10 to 12, includes: the sample dissolving tank 1, the heating table and the acid vapor collecting and processing assembly; wherein, the metal base 2 of the heating table is provided with a plurality of sample dissolving tank mounting holes 2-1; the acid vapor collecting and processing assembly is arranged above the metal base 2, is communicated with the sample dissolving tank 1 and is used for collecting and processing acid vapor generated in the sample dissolving tank 1, the acid vapor collecting and processing assembly comprises an acid vapor collecting plate 10, the acid vapor collecting plate 10 is detachably arranged above the metal base 2, and the bottom surface of the acid vapor collecting plate 10 can seal the tank opening of the sample dissolving tank 1; the acid vapor collecting plate 10 is provided with an acid vapor collecting channel which is communicated with the interior of the sample dissolving tank 1 which is arranged in the sample dissolving tank mounting hole 2-1.

In this embodiment, the acid vapor collecting plate 10 is made of teflon. As shown in fig. 11, the acid vapor collecting channel includes a main pipe 10-1 and branch pipes 10-2, wherein each branch pipe 10-2 is communicated with the main pipe 10-1, each branch pipe 10-2 is communicated with one sample dissolving tank 1, and the acid vapor in the branch pipe 10-2 is gathered in the main pipe 10-1 and discharged from the main pipe 10-1.

In a preferred embodiment of this embodiment, the diameter of the main conduit 10-1 is greater than the diameter of the branch conduit 10-2. The pipe diameter of the main pipeline 10-1 is 10-15 mm, the pipe diameter of the branch pipeline 10-2 is 5-8 mm at one end communicated with the sample dissolving tank 1, and the diameter of the end connected with the main pipeline 10-1 is reduced to 2-3 mm. The structure arrangement is beneficial to forming larger negative pressure at the connecting part, improving the gas flow rate and facilitating the discharge of acid vapor; on the other hand, the cross contamination caused by the sample particles splashed into the acid discharge pipeline can be avoided to the maximum extent.

Further, the branch pipeline 10-2 is obliquely arranged, an included angle between the outflow direction of the acid steam of the branch pipeline 10-2 and the flow direction of the acid steam of the main pipeline 10-1 is an acute angle, the outflow direction of the acid steam of the branch pipeline 10-2 is provided with the branch direction in which the flow directions of the acid steam of the main pipeline 10-1 are the same, and the acid steam of the branch pipeline 10-2 can flow into the airflow of the flow of the acid steam of the main pipeline 10-1. This structural setting can avoid the condensation backward flow, promotes and arranges sour effect.

In this embodiment, the metal base 2 is used to heat and remove acid from the solution dissolved in the sample dissolving bottle 1, and the metal base having the same structure and function as those in embodiment 1 is used, and the specific structure, function, and process control process and the like are described in embodiment 1.

In this embodiment, as shown in fig. 12, the bottom surface of the acid vapor collecting plate 10 is provided with can opening sealing structures 10-3, the number of the can opening sealing structures 10-3 is the same as the number of the sample dissolving can mounting holes 2-1, the can opening sealing structure 10-3 is an annular groove structure, and the can opening sealing structure 10-3 is adapted to the can opening of the can body 1-1, so that the can opening of the sample dissolving can 1 can be directly sealed. Unless otherwise specified, the sample-dissolving tank 1 in the present embodiment refers to the tank body 1-1 and does not include the lid body 1-1.

In this embodiment, the structure and the effect of the tank opening packaging structure 10-3 are the same as those of the cover body 1-2 of the sample dissolving tank 1, and the difference between the two is that the tank opening packaging structure 10-3 is provided with an acid discharge channel, the tank body 1-1 is communicated with the acid vapor collection channel through the acid discharge channel, and the acid discharge channel is also a branch pipeline 10-2. Specifically, the can mouth sealing structure 10-3 includes a second sealing ring groove 10-3-3 (corresponding to the first sealing ring groove 1-2-3 of embodiment 1), and the outer flange structure 1-1-1 of the can body 1-1 can be seamlessly mounted on the second sealing ring groove 10-3-3. The inner side wall of the second seal ring groove 10-3-3 forms a third seal part 10-3-1 (corresponding to the first seal part 1-2-1 of the embodiment 1), and the outer diameter of the third seal part 10-3-1 is equal to the inner diameter of the opening of the tank body 1-1; the outer side wall of the second seal ring groove 10-3-3 constitutes a fourth seal portion 10-3-2 (corresponding to the second seal portion 1-2-2 of embodiment 1), and the fourth seal portion 10-3-2 and the third seal portion 10-3-1 constitute a second seal ring groove 10-3-3 for accommodating the outer flange structure 1-1-1; the structure of the bottom of the second sealing ring groove 10-3-3 is matched with the structure of the outer flange structure 1-1-1 of the tank opening, and the bottom of the second sealing ring groove 10-3-3 is provided with a third plane, a fourth plane and a second inclined plane which are matched with the first top surface platform 1-1-4, the second top surface platform 1-1-1-5 and the inclined wall 1-1-1-3 of the outer flange structure of the tank opening. When the second sealing ring groove 10-3-3 of the acid vapor collecting plate 10 downwards extrudes the can opening outer flange structure 1-1-1, the first top surface platform 1-1-1-4, the second top surface platform 1-1-5, the inclined wall 1-1-1-3 and the second sealing ring groove 10-3-3 of the outer flange structure 1-1-1 form a triple sealing effect, and further the sealing effect is greatly improved.

In a preferred real-time manner of this embodiment, the can opening packaging structure 10-3 further includes a second concave groove 10-3-4, and a groove wall of the second concave groove 10-3-4 forms a third sealing portion 10-3-1; the bottom of the second concave groove 10-3-4 is provided with an acid discharge port, the branch pipeline 10-2 is provided with a branch pipeline inlet and a branch pipeline outlet 10-2-1, the acid discharge port is the branch pipeline inlet, and the cross section of the branch pipeline outlet 10-2-1 is in an inverted splayed structure. The branch pipeline outlet 10-2-1 of the inverted splayed structure can prevent acid steam from condensing and refluxing and improve the acid discharge effect.

The acid device is still equipped with heating apron 11 to airtight heating, and heating apron 11 dismantles and installs in the top of sour steam collecting plate 10, heats when catching up with sour, and heating temperature is higher than sour reagent boiling point, prevents effectively that high boiling point acid from leading to the condensation backward flow because of the temperature is low excessively in sour steam collecting channel, guarantees to arrange sour effect.

In a preferred embodiment of the present invention, the heating cover plate 11 is made of an aluminum alloy, a heating pipe is disposed inside the heating cover plate 11, and the surface of the heating cover plate 11 is anodized.

In a preferred embodiment of this embodiment, the heating cover plate 11 is provided with a temperature thermocouple, which can independently control the heating time and temperature, and the heating cover plate 11 can be provided with an independent heating switch, and the controller 4 of the heating device 3 can also control the heating function of the heating cover plate 11 to be turned on or off.

In this embodiment, the acid vapor collecting and processing assembly further includes an acid vapor processing device, the acid vapor processing device is connected to the main pipe 10-1 through a connecting pipe 12, wherein the main pipe 10-1 is a through hole, one end of the main pipe is provided with a needle valve capable of adjusting air inflow, the other end of the main pipe is provided with an acid outlet, and the acid vapor processing device is communicated with the acid outlet of the main pipe 10-1 through the connecting pipe 12. The main pipeline 10-1 is arranged to be of a through hole structure, so that the acid steam collecting plate 10 is convenient to clean; the air suction quantity of the jet pump 15 is larger than the air inflow of the needle valve, high-speed airflow is formed in the main pipeline 10-1 besides the suction force of the pump, negative pressure is generated at the reducing connection part of the branch pipeline 10-2 and the main pipeline 10-1 due to the Bernoulli effect, acid steam is favorably discharged better, and the acid discharge effect of each position of the acid steam collecting plate 10 is ensured to be consistent.

In a preferred embodiment of this embodiment, an air pump is used to deliver high-speed air flow to the needle valve end, so that negative pressure is generated at the reduced diameter connection part of the branch pipe 10-2 and the main pipe 10-1, and acid vapor is pumped out. The advantage of this solution is that the risk of corrosion of the pump body parts due to incomplete access of acid vapour to the suction pump as a result of treatment is completely eliminated.

In this embodiment, the acid vapor collection and treatment device includes a buffer bottle 13, an alkaline solution bottle 14 and a jet pump 15, and the buffer bottle 13, the alkaline solution bottle 14 and the jet pump 15 are sequentially arranged along the acid vapor outflow direction and are connected through a connecting pipe 12 made of PFA material. Acid steam is discharged from the main pipeline 10-1, firstly enters an empty buffer bottle through the connecting pipe 12 to avoid liquid backflow, then enters the alkaline solution bottle 14 through the connecting pipe 12, is absorbed and neutralized by alkaline solution in the alkaline solution bottle 14, and the jet pump 15 is arranged at the downstream of the alkaline solution bottle 14 and used for generating suction and accelerating discharge of the acid steam.

In a preferred embodiment of the present invention, a backing plate 5 is detachably mounted between the metal base 2 and the heating cover 11, and the backing plate 5 of the present embodiment has substantially the same structure and function as the backing plate 5 of embodiment 1, and is not described herein again.

Illustratively, the metal base 2 is provided with 20 sample dissolving tank mounting holes 2-1, correspondingly, 20 acid steam collecting branch pipes 10-2 and 2 acid steam collecting main pipes 10-1 are arranged inside the acid steam collecting plate 10, the tank body 1-1 is communicated with the main pipe 10-1 through the branch pipes 10-2, and the main pipe 10-1 is communicated with the buffer bottle 14 and the alkali liquor bottle 14 through the connecting pipe 12.

The acid removing method using the closed heating acid removing device of the embodiment includes the following steps:

the method comprises the following steps: the sample dissolving tank 1 is sealed and arranged in the sample dissolving tank mounting hole 2-1 by an acid vapor collecting plate 10.

Specifically, a cover body 1-2 of a sample dissolving tank 1 of a sample solution is taken down, and a tank body 1-1 filled with the sample solution is arranged in a sample dissolving tank mounting hole 2-1 on a metal base 2; buckling an acid vapor collecting plate 10 on a tank body 1-1 of a sample dissolving tank 1; placing a heating cover plate 11 on an acid vapor collecting plate 10, fixedly connecting the heating cover plate 11, the acid vapor collecting plate 10 and a metal base 2 by using a fixing bolt 7, and screwing down the fixing bolt 7 to seal a tank opening packaging structure 10-3 arranged on the bottom surface of the acid vapor collecting plate 10 with a tank opening of a sample dissolving tank 1;

step two: is connected with an acid steam treatment device.

After the sample dissolving tank 1 is installed and sealed, the acid vapor treatment device is connected with the main pipeline 10-1 of the acid vapor collecting plate 10 through the connecting pipe 12.

Step three: and opening a heating switch to finish acid removal according to a preset heating program.

And (3) starting a heating switch and a jet pump 15 switch, respectively heating the sample dissolving tank 1 and the acid steam collecting plate 10 by the metal base 2 and the heating cover plate 11 according to a preset heating program, and allowing acid steam to enter the acid steam treatment device through the acid steam collecting channel and the connecting pipe 12 for collection and neutralization treatment. And after the heating time is reached, acid is removed, the acid steam collecting plate 10 and the heating cover plate 11 are taken down, and the solution in the sample dissolving tank 1 is subjected to subsequent redissolution treatment.

Compared with the prior art, the closed acid dispelling device provided by the embodiment realizes the collection of acid steam and neutralization treatment under a closed condition, has a simple structure and a small volume, can be used for simultaneously dissolving a plurality of samples to dispel acid, has low operation strength, and greatly improves the experimental test efficiency; batch sealing of the sample dissolving tanks is realized by arranging a tank opening packaging structure on the bottom surface of the acid vapor collecting plate, so that the operation intensity is greatly reduced; and dissolve a jar mouth of pipe and be equipped with outward flange structure, the bottom surface of sour steam collecting plate is equipped with the jar mouth packaging structure with outward flange structure looks adaptation, realizes triple sealing, is showing to have promoted sealed effect, makes the whole collection of sour steam handle, has broken away from the reliance to the ventilation safety cabinet, realizes nontoxic gaseous emission, accords with green, high-efficient, convenient analysis and test technical development theory.

Example 3

Based on the disadvantages of the existing "inner container + outer steel sleeve" type closed sample dissolving device, the embodiment provides an integrated closed sample dissolving system integrating functions of closed sample dissolving, closed acid removing and sample redissolving, and the integrated closed sample dissolving system simultaneously has the functions of sample dissolving and redissolving of the closed heating digestion device of embodiment 1 and the functions of closed acid removing and heating of the closed heating digestion device of embodiment 2. Considering that there are a plurality of general components in the closed heating digestion apparatus of embodiment 1 and the closed heating acid-dispelling apparatus of embodiment 2, and in order to simplify the structure of the system and reduce the volume, this embodiment provides an integrated closed sample-dissolving system, which integrates the functions of sample dissolving, acid-dispelling and redissolution, and realizes sample dissolving, acid vapor collecting and redissolution under closed conditions, and the integrated closed sample-dissolving system includes: the device comprises a heating table, a sample dissolving tank 1, a fixed sealing assembly and an acid vapor collecting and processing assembly; it is also understood that the closed sample dissolving and acid removing device of the embodiment 2 further comprises the fixed sealing component of the embodiment 1, or the closed heating digestion device of the embodiment 1 further comprises the acid vapor collection and treatment component of the embodiment 2.

The heating table comprises a metal base 2, a heating device 3 and a controller 4, a plurality of sample dissolving tank mounting holes 2-1 are uniformly formed in the metal base 2, the metal base 2 is detachably mounted in a heating space of the heating device 3, and a fixed cover plate 6 and an acid vapor collecting plate 10 are connected with the metal base 2; the controller 4 controls the heating device 3 and the heating cover plate 11 to heat the metal base 2 according to a set heating program.

The heating table is provided with a plurality of sample dissolving tank mounting holes 2-1; the sample dissolving tank 1 comprises a tank body 1-1 and a cover body 1-2, the sample dissolving tank 1 is detachably mounted in a sample dissolving tank mounting hole 2-1, and the heating device 3 is used for heating a plurality of sample dissolving tanks 1 mounted in the sample dissolving tank mounting holes 2-1.

The fixed sealing assembly comprises a fixed cover plate 6 and a sealing bolt 8, the fixed cover plate 6 is positioned above the metal base 2 and detachably connected with the metal base 2, the fixed cover plate 6 is provided with first screw holes 6-1 with the same number as the sample dissolving tank mounting holes 2-1, and the sealing bolt 8 penetrates through the first screw holes 6-1 to tightly push the cover body 1-2 so as to seal the tank body 1-1 and the cover body 1-2.

The acid vapor collecting and processing assembly is communicated with the sample dissolving tank 1 and is used for collecting and processing acid vapor generated in the sample dissolving tank 1, the acid vapor collecting and processing assembly comprises an acid vapor collecting plate 10, the acid vapor collecting plate 10 is detachably mounted above the metal base 2, and the bottom surface of the acid vapor collecting plate 10 can seal the tank opening of the sample dissolving tank 1; the acid vapor collecting plate 10 is provided with an acid vapor collecting channel which is communicated with the interior of the sample dissolving tank 1 which is arranged in the sample dissolving tank mounting hole 2-1.

The structure, function, and usage of the heating table (metal base 2, heating device 3), the sample dissolving tank 1, and the fixing and sealing assembly in this embodiment are described in embodiment 1, and the structure, function, and usage of the acid vapor collecting and processing assembly are described in embodiment 2, and are not described herein again.

The integrated closed sample dissolving system of the embodiment is utilized to carry out the processes of sample dissolving, acid dispelling and redissolution, and comprises the following steps:

step S1: the sample dissolving tank 1 is sealed on the metal base 2 by using a fixed sealing component. The method specifically comprises the following steps:

step S11: adding an acid reagent and a solid sample to be dissolved into a sample dissolving tank 1, and packaging by using a cover body 1-2; a plurality of sample dissolving pots 1 containing an acid reagent and a solid sample to be dissolved are fitted into sample dissolving pot fitting holes 2-1 of a metal base 2.

Step S12: fixedly connecting a fixed cover plate 6 with a metal base 2, aligning a first screw hole 6-1 of the fixed cover plate 6 with a sample dissolving tank mounting hole 2-1, reserving a space between the fixed cover plate 6 and the top surface of the metal base 2, and enabling the fixed cover plate 6 to be in a suspended state relative to the top surface of the metal base 2;

step S13: and (3) penetrating the sealing bolt 8 through the first screw hole 6-1 to prop against the cover body 1-2, and screwing the sealing bolt 8 to seal the tank body 1-1 and the cover body 1-2.

Step S2: starting a heating switch of the heating device 3, heating the sample dissolving tank 1 on the metal base 2 by the heating device 3, and starting to dissolve the sample; after the sample is dissolved, the fixed cover plate 6 is detached, and the cover body 1-2 is opened. The method specifically comprises the following steps:

step S21: and (3) starting a switch of the electric heating plate 3, heating the sample dissolving tank 1 sealed on the metal base 2 by the heating device 3, starting to dissolve the sample, and heating to the preset time to complete sample dissolving.

Step S22: and after the sample is dissolved and the temperature is returned to the room temperature, the fixed cover plate 6 is detached, the cover body 1-2 is opened, and the acid removing operation step is carried out.

Step S3: the heating device 3 heats the sample dissolving tank 1 on the metal base 2, the tank body 1-1 is hermetically fixed on the metal base 2 by utilizing the acid vapor collecting plate 10, the acid outlet of the acid vapor collecting plate 10 is connected with the acid vapor treatment device, after the connection is finished, the heating switch is turned on, and the acid is removed according to a preset heating program. The method specifically comprises the following steps:

step S31: the acid vapor collecting plate 10 is fixedly connected with the metal base 2, and a tank opening packaging structure 10-3 of the acid vapor collecting plate 10 seals a tank opening of the sample dissolving tank 1 positioned in the sample dissolving tank mounting hole 2-1;

step S32: the acid steam treatment device is connected with an acid outlet of the main pipeline 10-1 of the acid steam collecting plate 10 through a connecting pipe 12;

step S33: and opening a heating switch to finish acid removal according to a preset heating program.

Concretely, accomplish the installation that dissolves kind jar 1 and sealed back, open heating device 3 and the heating switch that heats apron 11, metal base 2 and heating apron 11 heat according to predetermined heating procedure dissolving kind jar 1 and sour steam collecting plate 10 respectively, sour steam collects the passageway through sour steam, connecting pipe 12 gets into in the sour steam treatment device and collects and neutralization treatment, reach after the heat time, the completion catches up with sour, take off sour steam collecting plate 10 and heating apron 11, the solution that dissolves in kind jar 1 carries out follow-up redissolution and handles.

In order to accelerate the discharge of acid vapor, a switch of a jet pump 15 is turned on while heating, the jet pump 15 starts to work to generate suction force to accelerate the discharge of the acid vapor, the acid vapor discharged from a plurality of branch pipelines 10-2 enters a main pipeline 10-1, the acid vapor is discharged from the main pipeline 10-1, and firstly enters an empty buffer bottle through a connecting pipe 12 to avoid liquid backflow, and then enters an alkali liquor bottle 14 through the connecting pipe 12 to be absorbed and neutralized by an alkali solution in the alkali liquor bottle 14.

Step S4: after the acid removing process is finished, the acid steam collecting plate 10 is detached, the sample dissolving tank 1 is sealed on the metal base 2 by using the fixed sealing assembly, and the heating switch of the heating device 3 is turned on to redissolve. The method specifically comprises the following steps:

step S41: removing the acid vapor collecting plate 10, adding a re-dissolved acid reagent into the sample dissolving tank 1, and packaging by using a cover body 1-2; a plurality of sample dissolving tanks 1 filled with a redissolved acid reagent and a sample digestion substance are arranged in sample dissolving tank mounting holes 2-1 of a metal base 2.

Step S42: fixedly connecting a fixed cover plate 6 with a metal base 2, aligning a first screw hole 6-1 of the fixed cover plate 6 with a sample dissolving tank mounting hole 2-1, reserving a space between the fixed cover plate 6 and the top surface of the metal base 2, and enabling the fixed cover plate 6 to be in a suspended state relative to the top surface of the metal base 2;

step S43: and (3) penetrating the sealing bolt 8 through the first screw hole 6-1 to prop against the cover body 1-2, and screwing the sealing bolt 8 to seal the tank body 1-1 and the cover body 1-2.

Step S44: and (3) starting a heating switch of the heating device 3, controlling the heating device 3 by the controller 4 to heat the sample dissolving tank 1 sealed on the metal base 2 according to a set heating program, starting redissolution, and heating to a preset time to complete redissolution. And after re-dissolution is completed and the temperature is restored to the room temperature, the fixed cover plate 6 is detached, the sample dissolving tank 1 is taken out, and the subsequent experiment process is carried out.

Compared with the traditional closed heating digestion device, the closed sample dissolving system of the embodiment has obvious advantages, not only occupies small area, but also thoroughly avoids sample cross contamination and environmental pollution, and treats the same amount of samples, so that the required time is shorter, the material consumption cost is lower, the labor intensity is lower, and the device is specifically shown in the following table 1.

Table 1 comparison of effects

The integrated form seals and dissolves a kind system that this embodiment provided, collect the processing unit including programmable control's electric hot plate, metal base, dissolve a kind jar, fixed seal assembly and sour steam, collect and dissolve kind, catch up with sour and redissolve the function in an organic whole, realized dissolving kind, sour steam collection under the closed condition and handle and redissolve, have simple structure, small, the use equipment is few, convenient operation, advantage that manipulation strength is low. Two groups of heating parts which can be independently controlled are arranged at the periphery and the middle part of the electric heating plate, and 2-3 groups of temperature measuring thermocouples are arranged at the edge and the middle part of the metal base, so that the temperature can be respectively measured, the temperature can be respectively controlled, the heat loss at the periphery of the metal base can be compensated, and the consistency of the sample dissolving effect can be improved; the heating cover plate is provided with the temperature thermocouple, and the heating time and the temperature can be independently controlled, so that the heating, acid dispelling and redissolution steps can be automatically controlled by a program, the heating temperature is uniform in all places, the acid steam discharge speed and the negative pressure are consistent, various experimental parameters are effectively controlled, the introduction difference of operators is eliminated, and the experimental conditions can be highly repeated. Utilize programmable controller can realize dissolving appearance, catch up with the unmanned on duty of sour and redissolution flow, reduce experiment flow cost, can handle big batch sample moreover simultaneously, reduce manipulation strength by a wide margin, show the promotion experiment efficiency of software testing.

When dissolving the appearance, adopt fixed seal assembly to replace traditional outer steel bushing sealing form, every dissolves the appearance jar and adopts independent blind bolt to seal, greatly reduced operating strength, showing and promoting sealed effect, the fixed seal assembly of metal material does not keep away fixed seal assembly with the jar mouth direct contact who dissolves the appearance jar moreover, can not corrode, therefore pollution-free sample guarantees the reliability of test result.

When acid is discharged, acid steam is discharged from an acid steam collecting channel arranged in the acid steam collecting plate, so that the acid steam is collected and neutralized under a closed condition, the emission of non-toxic gas is realized, and the development concept of a green, efficient and convenient analysis and test technology is met.

It can be understood that the integrated closed sample dissolving system of the present embodiment has both the sample dissolving and redissolving functions of the closed heating digestion apparatus of embodiment 1 and the closed acid removing function of the closed heating acid removing apparatus of embodiment 2, and has corresponding and even better beneficial effects.

The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.

Claims

1. A closed heating acid-dispelling device is characterized by comprising:

the sample dissolving tank (1), wherein the sample dissolving tank (1) comprises a tank body (1-1) and a cover body (1-2);

the sample dissolving tank heating device comprises a heating table, wherein the heating table is provided with a plurality of sample dissolving tank mounting holes (2-1), and is used for heating the sample dissolving tanks (1) which are arranged in the sample dissolving tank mounting holes (2-1);

the acid vapor collection and treatment assembly comprises an acid vapor collection plate (10), and the acid vapor collection plate (10) is detachably mounted on the heating table and can seal the tank opening of the tank body (1-1); the acid vapor collecting plate (10) is provided with an acid vapor collecting channel which is communicated with the tank body (1-1) and used for collecting and treating the generated acid vapor.

2. The closed heating acid-dispelling device according to claim 1, further comprising a fixed sealing component for sealing the tank body (1-1) and the cover body (1-2) when the sample is dissolved.

3. The closed heating acid-dispelling device according to claim 1, wherein the acid vapor collection and treatment device comprises a buffer bottle (13), an alkali liquor bottle (14) and a jet pump (15), and the buffer bottle (13), the alkali liquor bottle (14) and the jet pump (15) are arranged in sequence along the acid vapor outflow direction.

4. The apparatus as claimed in claim 1, wherein the acid vapor collecting channel comprises:

a main pipeline (10-1), wherein one end of the main pipeline 10-1 is provided with a needle valve for adjusting air inflow, and the other end of the main pipeline is communicated with the acid steam treatment device;

the first end of the branch pipeline (10-2) is communicated with the main pipeline (10-1), and the second end of the branch pipeline (10-2) is communicated with the tank body (1-1).

5. The closed heating acid-dispelling device according to claim 4, wherein said branch conduit (10-2) has a branch conduit inlet through which acid vapor enters said branch conduit (10-2) and a branch conduit outlet (10-2-1) from said branch conduit outlet (10-2-1) into said main conduit (10-1);

the cross section of the branch pipeline outlet (10-2-1) is of an inverted splayed structure.

6. The closed heating acid-dispelling device according to any one of claims 1 to 5, wherein the mouth of the tank body (1-1) is provided with an outer flange structure (1-1-1), the outer diameter of the outer flange structure (1-1-1) is larger than the aperture of the sample dissolving tank mounting hole (2-1), and the outer diameter of the tank body (1-1) is equal to the aperture of the sample dissolving tank mounting hole (2-1);

the bottom surface of the acid steam collecting plate (10) is provided with a tank opening packaging structure (10-3), the tank opening packaging structure (10-3) comprises a sealing ring groove, and the outer flange structure (1-1-1) can be seamlessly installed in the sealing ring groove.

7. The apparatus as claimed in claim 6, wherein the heating stage comprises:

the sample dissolving tank mounting holes (2-1) are uniformly distributed on the metal base (2), and the fixed cover plate (6) is detachably connected with the metal base (2);

the heating device (3) is provided with a heating space, the metal base (2) is detachably mounted in the heating space, and the heating device (3) is used for heating the sample dissolving tank (1) on the metal base (2);

and the controller (4), the controller (4) controls the heating device (3) to heat according to a set program.

8. The closed heating acid-dispelling device according to any one of claims 1 to 7, further comprising a heating cover plate (11), wherein the heating cover plate (11) is detachably mounted above the acid vapor collecting plate (10) for heating during acid-dispelling.

9. The closed heating acid-dispelling device according to claim 7, wherein a backing plate (5) made of polytetrafluoroethylene is further disposed on the top surface of the metal base (2), and the backing plate (5) is located between the lower end of the outer flange structure (1-1-1) and the top surface of the metal base (2).

10. An integrated closed sample dissolving method, characterized in that the closed heating acid-dispelling device of any one of claims 1 to 9 is used, and comprises the following steps:

sealing the sample dissolving tank (1) on the metal base (2) by using a fixed sealing assembly, starting a heating switch, dissolving samples according to a preset program, and closing the heating switch after completing the sample dissolving;

the fixed sealing assembly is detached, the cover body (1-2) is opened, the tank body (1-1) is fixed on the metal base (2) in a sealing mode through the acid vapor collecting plate (10), and an acid vapor treatment device is connected to an acid outlet of the acid vapor collecting plate (10);