Device for rapidly determining heavy metal content of animal skeleton sample by utilizing flame reaction
The device for rapidly determining the heavy metal content of animal bone samples through flame color reaction solves the problem of difficulty in conveniently monitoring atmospheric heavy metal pollution in existing technologies, realizes rapid and accurate detection of heavy metal concentrations, and has a simple and low-cost device.
Patent Information
- Application Number
- CN202510796529.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-11
- Publication Date
- 2025-09-19
AI Technical Summary
Existing technologies make it difficult to quickly and conveniently use the characteristics of air breathed by animals to monitor heavy metal pollution in the atmosphere. Biological detection methods are affected by plant species and growth environment and cannot accurately quantify heavy metal concentrations.
The device uses flame color reaction to quickly determine the heavy metal content of animal bone samples. The animal bones are ground into easily digestible bone powder using a sample grinder. Nitric acid digestion solution is added for digestion. The bones are placed in a stainless steel reactor for heating. After cooling, the samples are filtered and fixed to volume. The heavy metal element content is detected using a mass spectrometer.
It realizes the rapid and convenient monitoring of atmospheric heavy metal pollution. The device is simple, easy to operate, low-cost, and can accurately obtain the specific values of atmospheric heavy metal pollution.
Smart Images

Figure CN120668767A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to a device for rapidly determining the heavy metal content of animal bone samples by utilizing flame color reaction, and belongs to the technical field of atmospheric heavy metal pollution monitoring. Background Art
[0002] Currently, there are several main methods for monitoring atmospheric heavy metal pollution: membrane sampling-laboratory analysis, online monitoring, biological monitoring, passive sampling, high-flow sampling, and source apportionment. Among these, biological testing primarily utilizes certain plants that accumulate heavy metals, such as mosses, to analyze their heavy metal content, indirectly reflecting the status of atmospheric heavy metal pollution. This method is simple to operate and low-cost, but its monitoring results are affected by various factors, such as plant species and growth environment, and it is difficult to accurately quantify the concentration of heavy metals in the atmosphere. Domestic pigeons are a common bird species that soar through the air whenever they fly. Their dual-breathing lungs ensure that domestic pigeons are constantly exposed to the outside air. If heavy metals are inhaled into the body, they are difficult to metabolize and often deposit in the bones. If their bones can be removed, ground into bone powder, and then digested, the amount of heavy metal deposition can be rapidly analyzed using a flame reaction and an inductively coupled plasma mass spectrometer, thereby quickly obtaining accurate numerical values for atmospheric heavy metal pollution and understanding the specific status of local atmospheric heavy metal pollution. Regarding the methods and devices for flame color reaction detection, some people have actively developed a large number of flame color reaction related products and methods, such as a simple detection method for iron-based deoxidizer components, application number CN200610024672.1; a flame color reaction experimental device, application number CN201220738302.5; a flame color reaction demonstration device, application number CN201320727834.3; a hospital sewage component detection method, application number CN201410778713.0; a flame color reaction testing device, application number CN201520171413.6; a flame color reaction demonstration device, application number CN201620033558.4; a chemical experiment flame color reaction experimental stand, application number CN201620289638.6; a flame color reaction teaching demonstration device, application number CN201621273578.5; a high school chemistry Applications include: a flame color reaction device for chemical reactions, application number CN201720387734.9; a sensor-based soil environment monitoring device system, application number CN201720673807.0; an energy-saving and environmentally friendly chemical reaction flame color reaction device, application number CN201721700322.2; a chemical teaching demonstration device for flame color reaction, application number CN201820414924.X; an energy-saving and environmentally friendly chemical reaction flame color reaction device, application number CN201820420301.3; a teaching method and device for simulated chemical experiments displaying flame color reaction, application number CN201810414409.6; an energy-saving and environmentally friendly chemical reaction flame color reaction device and its use method, application number CN201810732023.X; and a method for detecting pesticide residues in agricultural products, application number CN201810962104.9; a chemical flame color reaction display device, application number CN201920248516.6; a portable flame color reaction device, application number CN201921790408.8; an intelligent voice interaction system for chemical flame color reaction teaching, application number CN202020534987.6; a metal element flame color reaction experimental device for easy observation and analysis, application number CN202120220116.1; the preparation and application of an integral torch combustion catalyst, application number CN202111221296.6; a method for testing trace mineral elements in feed, application number CN202210289462.4; a flame color test spectrometer, application number No. CN202321673570.8; a multifunctional on-site displacement fidelity test device and test method for core sampling, application number CN202311489919.7; a device, method, and application for identifying metal salt types, application number CN202311550789.3; a metal element flame color reaction experimental device, application number CN202323213950.6; a methanol flame color reaction component and igniter system, application number CN202311848300.0; an igniter system, application number CN202311850553.1; and a device and method for evaluating the flame color reaction of fireworks luminescent materials, application number CN202410936199.2. However, all these methods for monitoring atmospheric heavy metal pollution have various defects, and there is no particularly easy-to-operate and mature method. Therefore, how to use the characteristics of animal breathing air to quickly and conveniently monitor the heavy metal status in the atmosphere using flame color reaction has become a major problem that needs to be solved urgently. Therefore, the device for quickly determining the heavy metal content of animal bone samples using flame color reaction uses a sample grinder to quickly and accurately quantitatively grind the bones of animals such as domestic pigeons into bone powder that is easy to be digested by digestion solutions such as nitric acid, and quantitatively drop the bone powder into a digestion tube. Then, nitric acid and other digestion solutions are added in batches for digestion. After that, the digestion tube is taken out, the digestion tube cover is covered, and the digestion tube is placed in a stainless steel reactor for further digestion, that is, the digestion tube is placed in an oven at a controlled temperature of 190°C and heated for about 10 The powdered bone sample is completely dissolved in the nitric acid digestion solution for 1 hour, releasing the various elements in the sample into the nitric acid digestion solution. The digestion tube is then cooled and removed from the reactor. The nitric acid digestion solution in the digestion tube is filtered through a membrane filter. The filtrate is collected in a 50-ml flat-bottom plastic centrifuge tube and diluted to the 50-ml mark with deionized water to obtain a test solution within the linear range of the mass spectrometer. The mass spectrometer is then turned on to test the sample, quickly determining the specific content of each heavy metal element in the bone sample and, in turn, understanding the local atmospheric heavy metal pollution status. This achieves the goal of utilizing the characteristics of the air animals breathe to quickly and conveniently monitor the heavy metal status in the atmosphere using flame color reaction. Therefore, it is necessary to invent a device that uses flame color reaction to rapidly determine the heavy metal content of animal bone samples. Summary of the Invention
[0003] In order to overcome the problem of how to utilize the characteristics of the air breathed by animals to quickly and conveniently monitor the heavy metal status in the atmosphere by flame color reaction, the present invention provides a device for quickly determining the heavy metal content of animal bone samples by flame color reaction. The device for quickly determining the heavy metal content of animal bone samples by flame color reaction uses a sample grinding preparation device to quickly, accurately and quantitatively grind the bones of animals such as domestic pigeons into bone powder that is easily digested by digestion solutions such as nitric acid, and then quantitatively drop the bone powder into a digestion tube. Then, quantitatively add digestion solutions such as nitric acid in batches for digestion, then remove the digestion tube, cover the digestion tube with a digestion tube cover, and place the digestion tube in a stainless steel reactor for further digestion, that is, place the digestion tube in an oven to control the temperature at 19 The powdered bone sample is heated at 0°C for about 10 hours to completely dissolve the powdered bone sample under the action of the nitric acid digestion solution, and the elements in the sample are released into the nitric acid digestion solution. After that, the digestion cylinder is cooled and taken out from the reactor. The nitric acid digestion solution in the digestion cylinder is filtered using a filter membrane, and the filtrate is collected in a 50 ml flat-bottom plastic centrifuge tube. The volume is adjusted to 50 ml mark with deionized water to obtain a test solution within the linear range of mass spectrometer detection. The mass spectrometer is turned on to detect the sample, and the specific content of each heavy metal element in the bone sample can be quickly obtained, and then the local atmospheric heavy metal pollution status can be known, thereby achieving the purpose of using the characteristics of animal breathing air to quickly and conveniently monitor the heavy metal status in the atmosphere by flame color reaction.
[0004] The technical solution adopted by the present invention to solve its technical problem is:
[0005] The present invention uses a device for rapidly determining the heavy metal content of an animal bone sample using a flame color reaction. The method comprises the following steps: firstly, placing a bone sample 1 in a sample powder preparation device 55 for grinding and adding a nitric acid digestion solution 39 for digestion; then, removing a digestion tube 12 and covering it with a digestion tube cover 26; and placing the digestion tube 12 in a stainless steel reactor for further digestion. Specifically, the digestion tube 12 is placed in an oven and heated at a controlled temperature of 190° C. for about 10 hours, so that the powdered bone sample 1 is completely dissolved in the nitric acid digestion solution 39, and each element in the sample is released into the nitric acid digestion solution 39; then, cooling the digestion tube 12, removing it from the reactor, filtering the nitric acid digestion solution 39 in the digestion tube 12 using a filter membrane, and collecting the filtrate in a 50 ml flat-bottom plastic centrifuge tube. Deionized water is diluted to 50 ml mark to obtain the solution to be tested within the linear range of mass spectrometer 51. The mass spectrometer 51 is turned on to detect the sample, and the specific content of each heavy metal element in the bone sample 1 can be quickly obtained; the sample grinding preparation device 55 is composed of a bone sample 1, a hoop bone tube 2, a hoop bone tube hoop 3, a support bone tube 4, a top bone spring 5, a block cylinder block 6, a rotating cylinder shaft 7, a fixed axis rivet 8, a rotating ring 9, a support disk column 10, a digestion cylinder 12, a digestion cylinder disk 13, a digestion cylinder disk rotating motor 14, a digestion cylinder disk pointed cap 16, a powder falling funnel 17, a powder collecting funnel 18, a grinding wheel 19, a grinding wheel motor 20, a pointed top plate 27, a nitric acid digestion bottle 36, a fixed plate 52, and a buckle loop 53, characterized in that: the bone sample 1 is the animal to be tested Bone samples, such as the bones of birds such as domestic pigeons, the bones of mammals such as rabbits, the bones of amphibians such as toads, and the bones of reptiles such as geckos, usually use the femurs of these animals. Before testing, the femurs are cut into long segments with a length of 1-2 cm with a saw. If there is bone marrow in the femur, it is necessary to use tools such as tweezers to remove the bone marrow first, leaving only the relatively hard bone part; the hoop bone tube 2 is the cylindrical part above the support bone tube 4, and shares a fixed tube column 32 with the support bone tube 4 and is connected together through the fixed tube column 32. The height of the hoop bone tube 2 is 0.9-1.8 cm. The hoop bone tube 2 is composed of the fixed tube column 32, the inner side wall 33 of the hoop bone tube, the outer side wall 34 of the hoop bone tube, and the hoop bone tube cavity 35. The fixed tube column 32 is made of manganese steel and is shared by the hoop bone tube 2 and the support bone tube 4. The support column has a square cross-section with a side length of 3-5 mm. It is solid, with the upper end extending to the top edge of the hoop tube 2 and the lower end welded to the upper surface of the rotating cylinder shaft 7. The base of the hoop tube inner wall 33 and the hoop tube outer wall 34 of the hoop tube 2 are welded together, and the outer surface of the base is welded to one side of the fixed tube column 32. The outer surface of the simplified body of the support tube 4 is also welded to the same side. The hoop tube inner wall 33 is made of spring steel, with an arc-shaped cross-section, a base thickness of 2-3 mm, and a free end thickness of 0.5-1 mm. The free end of the hoop tube inner wall 33 extends to the inside of the free end of the hoop tube outer wall 34. The hoop tube outer wall 34 is made of spring steel, with an arc-shaped cross-section, a base thickness of 2-3 mm, and a free end thickness of 0.5-1 mm, the free end of the outer side wall 34 of the hoop bone tube extends to the outside of the free end of the inner side wall 33 of the hoop bone tube; the hoop bone tube cavity 35 is a cavity surrounded by the inner side wall 33 of the hoop bone tube and the outer side wall 34 of the hoop bone tube, and the interior is used to place the bone sample 1; the support bone tube 4 is a cylindrical tube below the hoop bone tube 2, the support bone tube 4 is made of manganese steel, the tube wall thickness is 1-3 mm, the height is 3-5 cm, the inner cavity diameter is 1-5 cm, and a top bone spring 5 is set in the support bone tube 4. The lower end of the support bone tube 4 is welded to the upper surface of the free end of the rotating cylinder shaft 7, and the upper end is connected to the hoop bone tube 2 through the fixed tube column 32. The lower end of the fixed tube column 32 is also welded and fixed to the upper surface of the free end of the rotating cylinder shaft 7; the top bone spring 5 is an elastic spring fixed at the lower end to the inner surface of the tube wall of the bottom end of the support bone tube 4 Spring, a disc-shaped baffle is fixed at the upper end; the block cylinder block 6 is made of manganese steel, with an arc-shaped cross section, a height of 2.5-4 cm and a thickness of 3-5 mm. The lower end is welded and fixed to the upper surface of the fixed plate 52, and the upper end is free. The axis of the block cylinder 6 in the vertical direction is perpendicular to the diameter of the support tube 4 and is located in the plane where the diameter is located; one end of the rotating cylinder shaft 7 is welded and fixed to the side wall of the swivel 9, and the other end is free and the upper surface is welded to the support tube 4 and the lower end of the solid cylinder column 32. The rotating cylinder shaft 7 is made of manganese steel and has a rectangular cross section. The long side of the rectangular rotating cylinder shaft 7 is set horizontally with a length of 5-8 mm and a short side is set vertically with a length of 3-5 mm; the swivel 9 is made of manganese steel and the cross section of the ring body is a square with a side length of 2-5 mm. The ring body circumference The cylindrical inner cavity has a diameter of 5-8 mm; the fixed axis rivet 8 is made of manganese steel and is divided into upper and lower parts. The upper part of the fixed axis rivet 8 is hexagonal, the distance between the two opposite faces of the hexagonal prism is 7-13 mm, and the height of the hexagonal prism is 3-5 mm; the lower part of the fixed axis rivet 8 is cylindrical, the diameter of the cylinder is 4.5-7 mm, and the height is 1-2 cm. The lower part of the fixed axis rivet 8 is divided into upper and lower halves, and the upper half of the lower part of the fixed axis rivet 8 has a smooth surface; the lower half of the lower part of the fixed axis rivet 8 has a threaded surface, which is engaged with the thread of the inner surface of the groove provided at this location of the fixing plate 52; the support column 10 is made of manganese steel and is divided into upper and lower parts. The lower part of the support column 10 is cylindrical, with a diameter of 1-2 cm and a height of 3- 5 cm; the upper portion of the support column 10 is stepped, called the support column step head 29, which has three levels, and its diameter decreases step by step. The lower two levels are cylindrical, and the uppermost level is conical, also known as the support column tip 28. The pointed top of the conical support column tip 28 directly contacts the center of the lower surface of the pointed top plate 27. The pointed top plate 27 is a cylindrical pad set on the top of the support column step head rotating cylinder 15 in the center of the lower surface of the digestion cylinder pointed cap 16. It is made of manganese steel, with a diameter of 3-5 mm and a thickness of 3-5 mm. The digestion cylinder 13 is a disk for placing the digestion cylinder 12. It is divided into an inner and outer part. The outer part of the digestion cylinder 13 is annular, and the cross-section of the annular ring is rectangular. The length of the rectangle is 2-3 cm and the width is 1.5-2 cm, a plurality of cylindrical grooves with a cross-sectional diameter of 1-1.5 cm are arranged at equal intervals on the upper surface of the rectangular ring body, a digestion cylinder 12 is placed in each groove, the outer surface of the digestion cylinder 12 is close to the inner wall of the groove, and the width of the gap between the digestion cylinder 12 and the groove is 0.01-0.1 mm; the interior of the digestion cylinder disk 13 is conical, also known as the digestion cylinder disk pointed cap 16, the cylindrical structure with an opening to the lower surface just below the top is the support column ladder head rotating cylinder 15, the support column ladder head rotating cylinder 15 is divided into 4 levels, each of the upper 3 levels is engaged with the structure of the support column ladder head 29, the 3 levels of the support column ladder head rotating cylinder 15 are 0.5-1 mm away from the support column ladder head 29, and the lowest level is located at the support column 1 0, the outer surface of the lower part is cylindrical, and a digestion drum rotating motor 14 is provided at each end of a diameter along the central axis of the support drum column 10 between the lowest level of the support drum column ladder head rotating drum 15 and the lower part of the support drum column 10; the digestion drum rotating motor 14 is a well-known electric motor; the digestion drum rotating motor rotor 31 is the rotor of the digestion drum rotating motor 14, and has teeth on the surface, which can mesh with the teeth of the bite ring teeth 30; the bite ring teeth 30 are made of manganese steel and are annular as a whole. The outer surface of the bite ring teeth 30 is smooth and welded to the inner surface of the lowest level of the support drum column ladder head rotating drum 15, and the inner surface of the bite ring teeth 30 is provided with a gear, and the teeth of the gear mesh with the teeth of the digestion drum rotating motor rotor 31; the height of the digestion drum rotating motor rotor 31 is 3-5 mm, the height of the ring body of the bite ring teeth 30 is 5-8 mm; the upper surface of the outer ring body of the digestion cylinder disc 13 between two adjacent digestion cylinders 12 is provided with a groove with an arcuate cross section, and these grooves and the inner cavity of the digestion cylinder 12 together constitute the guide trough 11; the digestion cylinder 12 is made of polytetrafluoroethylene and is cylindrical. The digestion cylinder 12 consists of a numbered area 21, a digestion cylinder wall cavity 22, a digestion cylinder wall 23, a digestion cylinder cavity 24, a lifting cylinder concave hole 25, and a digestion cylinder cover 26. The digestion cylinder wall 23 is a wall around and at the bottom of the digestion cylinder 12 and has a double-layer structure consisting of an inner wall and an outer wall. The cavity between the inner wall and the outer wall is the digestion cylinder wall cavity 22; the height of the inner wall of the digestion cylinder wall 23 is lower than the height of the outer wall, so an inclined surface is formed on the upper edge of the digestion cylinder wall 23. A pair of lifting holes 25 are symmetrically arranged on the inclined surface. The lifting holes 25 are two horizontal grooves arranged on the upper inclined surface of the digestion cylinder 12. The two grooves are located at the ends of the cross-section of the digestion cylinder 12. The openings of the lifting holes 25 face inward, opening between the inner wall and the upper end of the outer wall of the digestion cylinder wall 23. The bottom of the lifting holes 25 is blocked. The buckle 53 is made of spring steel and has a circular cross-section with a diameter of 1-3 mm. The buckle 53 consists of a horizontal axis, a grip axis, a vertical axis, and a convex axis. There is only one horizontal axis, which is located at the top and innermost. Its length is determined by the distance between the openings of the two lifting holes 25, generally half the distance between the openings of the two lifting holes 25. The grip axis is a curved axis connected to the ends of the horizontal axis for easy grasping by the human hand, and is approximately shape or shape; the vertical axis is located at the lower end of the handle shaft in the vertical direction of the axis, a total of 2, the lower end of the vertical axis is connected to the inner end of the convex axis, the distance between the two vertical axes is equal to the distance between the openings of the two lifting tube recesses 25; the convex axis is the outermost two horizontal axes of the buckle loop 53; the digestion cylinder cavity 24 is surrounded by the digestion cylinder wall 23; the numbered area 21 is located in the center of the outer surface of the outer wall of the digestion cylinder wall 23, and is square. Different numbers are made in the numbered area 21; the digestion cylinder cover 26 is made of polytetrafluoroethylene and is curved. The highest point is 1-2 mm from the center of the plane circle where the bottom edge is located. , the diameter of the plane circle where the bottom edge is located is equal to the distance between the openings of the two lifting cylinder recesses 25; the powder falling funnel 17 is made of plastic with a wall thickness of 0.2-0.5 mm. The upper opening of the powder falling funnel 17 is located at the bottom edge of the powder collecting funnel 18, is circular, has a diameter of 3-5 cm, and is arranged horizontally; the lower opening of the powder falling funnel 17 is free and elliptical, the major diameter of the ellipse is 1-2 cm and the minor diameter is 0.5-1 cm, and is arranged at an angle of 45 ° to the horizontal direction. The lower end opening of the powder falling funnel 17 faces the direction of rotation of the digestion cylinder disc 13, and the wall of the opening extends into the digestion cylinder cavity 24 by about 0.5-1 mm; The powder collecting funnel 18 is located below the grinding wheel 19 and is made of plastic. The wall thickness is 0.2-0.5 mm. The powder collecting funnel 18 is divided into two parts, the upper part of the powder collecting funnel 18 is cylindrical, and the cylinder has no upper and lower bottoms, only walls around it. The height of the upper part of the powder collecting funnel 18 is 3-5 cm, and the lower edge of the cylindrical wall and the lower surface of the grinding wheel 19 are in the same plane; the lower part of the powder collecting funnel 18 is in the shape of an elephant trunk, and the upper edge of the lower part of the powder collecting funnel 18 is connected to the lower edge of the upper part, and then it shrinks and becomes smaller, converging towards the upper end of the powder falling funnel 17 and finally at the upper end of the powder falling funnel 17. An opening is also provided at the lower wall of the sample grinder 55 corresponding to the hoop tube 2, allowing the hoop tube 2 to extend into the powder collecting funnel 18; the grinding wheel 19 is a commercially available cylindrical grinding wheel with a diameter of 5-10 cm and a height of 5-20 mm. A manganese steel shaft is provided in the center of the upper surface of the grinding wheel 19; the grinding wheel motor 20 is a commercially available electric motor fixed to the inner surface of the top wall of the sample grinder 55; the upper end of the nitric acid digestion bottle 36 is fixed to the inner surface of the top wall of the sample grinder 55, and the lower end of the nitric acid digestion bottle 36 is free. The force claw 49 of the gravity switch 50 at the lower end of the nitric acid digestion bottle 36 extends into the digestion cylinder cavity 24 by approximately 0.5-1 mm, the nitric acid digestion bottle 36 is composed of a bottle body 54, a nitric acid digestion solution 39, a fixed switch 42, a nitric acid digestion pipe 43 and a gravity switch 50. The bottle body 54 includes a nitric acid digestion bottle wall 37, a nitric acid digestion bottle cavity 38, a nitric acid digestion bottle neck 40, and a nitric acid digestion bottle mouth 41. The nitric acid digestion bottle wall 37 is the outer wall of the bottle body 54, which is glassy and has a thickness of 1-2 mm; the nitric acid digestion bottle cavity 38 is the cavity surrounded by the nitric acid digestion bottle wall 37; the nitric acid digestion bottle neck 40 is the part where the lower part of the bottle body 54 tapers to the nitric acid digestion bottle mouth 41; the nitric acid digestion bottle mouth 41 is the opening at the lower end of the bottle body 54 for releasing the nitric acid digestion solution 39, the inner cavity diameter is 1-1.5 cm, and the lower end opening of the bottle body 54 is blocked by a bottle stopper; the fixed switch 42 is a valve set on the bottle stopper, and the size of the opening amplitude of the fixed switch 42 determines the nitric acid digestion solution 39 The flow rate of the nitric acid digestion bottle 41 is controlled by the nitric acid digestion solution 39, which can digest and convert heavy metals in bone powder into a single valence state. The nitric acid digestion tube 43 is made of glass. The upper end of the nitric acid digestion tube 43 is controlled by a fixed switch 42. The lower end of the nitric acid digestion tube 43 is an oblique opening with a rubber pad at the opening. The gravity switch 50 is made of spring steel and consists of a tube holding ring 44, an arm shaft 45, a force-guiding claw 46, a tube-blocking gravity ball 47, a force-bearing claw arm 48, and a force-bearing claw 49. The tube holding ring 44 is a ring tube surrounding the nitric acid digestion tube 43. The overall shape is a central drum with pointed ends. The nitric acid digestion tube 43 is located in the center of the central drum of the tube holding ring 44. One end of the tube holding ring 44 is connected to the arm shaft 45, and the other end is connected to the upper end of the force-bearing claw 46. The arm shaft 45 is the rotating axis that fixes the tube holding ring 44 and the force-bearing claw arm 48. The upper horizontal bar is the rotating shaft in the through-holes on both sides of one end of the tube holding ring 44, and the downward vertical bar is the supporting shaft extending inward from the center of one end of the tube holding ring 44, and the inner end of the vertical bar is fixed on the outer surface of the flowing nitric acid digestion tube 43; the force-guiding claw 46 is arc-shaped, with one end connected to one end of the tube holding ring 44 and the other end connected to the pipe-blocking gravity ball 47; the force-bearing claw arm 48 is the connecting arm between the tube holding ring 44 and the force-bearing claw 49, and is arc-shaped; the force-bearing claw 49 is a thin spring steel sheet.
[0006] The free ends of the inner side wall 33 and the outer side wall 34 of the hoop bone tube partially overlap and are not connected together. Therefore, after the bone sample 1 is placed in the hoop bone tube cavity 35, the diameter of the hoop bone tube cavity 35 can change with the size of the diameter of the bone sample 1. If the diameter of the bone sample 1 is large, the diameter of the hoop bone tube cavity 35 will be stretched and enlarged. If the diameter of the bone sample 1 is small, the diameter of the hoop bone tube cavity 35 will recover and become smaller due to the elasticity of the spring steel. Once the bone sample 1 is placed in the hoop bone tube cavity 35, the bone sample 1 will be fixed, and the diameter of the hoop bone tube cavity 35 will no longer change. Therefore, two upper and lower hoop bone tube hoops 3 are also provided on the hoop bone tube 2; the structure of the hoop bone tube hoop 3 is the same as the commercially available adjustable iron hoop, that is, the iron hoop is annular, and the inner surface of the ring body relative to the adjustment buckle is welded to the other surface of the fixed tube column 32 relative to the surface where the base of the inner side wall 33 and the outer side wall 34 of the hoop bone tube is located. The two parts can move relative to each other under the action of the fixed top buckle. Once they move to tightly clamp the hoop bone tube 2, they stop and are fixed together, and no longer move relative to each other, thereby firmly fixing the bone sample 1 in the hoop bone tube cavity 35 without tilting or expanding. At most, under the action of the top bone spring 5 in the support bone tube 4, the bone sample 1 can extend upward from the hoop bone tube cavity 35, and the upper end of the bone sample 1 extends to the lower surface of the grinding wheel 19. As the upper end of the bone sample 1 is ground into powder by the grinding wheel 19 and becomes shorter, the bone sample 1 is continuously pushed upward by the top bone spring 5 until it is almost completely worn out and pushed out of the hoop bone tube cavity 35 by the top bone spring 5. The ground bone sample 1 is thrown out under the action of centrifugal force and gravity, and falls into the powder collecting funnel 18 and the powder dropping funnel 17 to be collected. It then falls into the guide trough 11 or the digestion cylinder 12 along the powder dropping funnel 17. The rotation speed of the digestion cylinder disc 13 is controlled so that the amount of bone powder falling into each digestion cylinder 12 is 0.1 gram; during the rotation of the digestion tube 12, when a digestion tube 12 is transferred to the bottom of the nitric acid digestion bottle 36, 5 ml of nitric acid digestion solution 39 can be injected into the digestion tube 12, and the bone powder can be digested by the nitric acid digestion solution 39 in the digestion tube 12, and the metal elements in the sample are converted into a single valence state. When all the digestion tubes 12 around the periphery of a digestion tube plate 13 are injected with nitric acid digestion solution 39, the digestion tubes 12 with numbering on the tube wall are taken out in turn, and then the digestion tube cover 26 of the digestion tube 12 is covered, and the digestion tube 12 is placed in a stainless steel reactor and placed in an oven to control the temperature at 190°C and heated for about 10 hours to make the powdered bone sample 1 in the nitric acid digestion. The sample is completely dissolved under the action of the nitric acid digestion solution 39, and the various elements in the sample are released into the nitric acid digestion solution 39. Afterwards, the digestion cylinder 12 is cooled and removed from the reactor. The nitric acid digestion solution 39 in the digestion cylinder 12 is filtered through a filter membrane. The filtrate is collected in a 50 ml flat-bottom plastic centrifuge tube and the volume is adjusted to the 50 ml mark with deionized water. This gives a test solution within the linear range of the mass spectrometer 51. The mass spectrometer 51 is turned on to test the sample, and the specific content of each heavy metal element in the bone sample 1 can be quickly determined. The mass spectrometer 51 is a commercially available inductively coupled plasma mass spectrometer capable of rapid quantitative determination of heavy metals in bone samples.
[0007] The process of placing the bone sample 1, grinding it into bone powder, and collecting the bone powder is as follows: after the bone sample 1 is placed in the bone hoop 2, the bone support tube 4 is rotated and pushed into the depression in front of the retaining tube block 6. At the same time, the bone sample 1 is pressed downward so that the bone sample 1 is between the top bone spring 5 and the grinding wheel 19, so that when the grinding wheel 19 rotates, the bone sample 1 can be ground into bone powder little by little, and under the action of the centrifugal force generated during the rotation, it falls into the powder collecting funnel 18 and the powder dropping funnel 17 to be collected.
[0008] The specific way in which the bone powder in the powder falling funnel 17 falls onto the guide trough 11 is as follows: since the plastic wall thickness at the opening of the powder falling funnel 17 is 0.2-0.5 mm, which is relatively thin and elastic, during the rotation of the digestion cylinder disc 13, it can scrape the bone powder fallen from the guide trough 11 between two adjacent digestion cylinders 12 into the digestion cylinder 12 like a scraper. When it rotates to the upper end of the digestion cylinder cavity 24, with the help of the elasticity of the opening at the lower end of the powder falling funnel 17, the powder falling funnel 17 can also be shaken, thereby better shaking off the bone powder that may remain in the powder falling funnel 17.
[0009] The specific method of the nitric acid digestion bottle 36 controlling the nitric acid digestion solution 39 to flow out of the nitric acid digestion tube 43 is as follows: when the digestion cylinder disc 13 rotates and the force claw 49 is above the guide groove 11, since the force claw 49 is made of spring steel and has elasticity, the force claw 49 can slide along the guide groove 11, but the force between the force claw 49 and the guide groove 11 pushes the force claw 49 in the opposite direction of the rotation of the digestion cylinder disc 13, forming a thrust, and then the pipe blocking gravity ball 47 is tightly pressed against the opening at the lower end of the flow nitric acid digestion tube 43, blocking the opening, and the nitric acid digestion solution 39 flows out of the nitric acid digestion tube 43. 9 will not flow out; but when the digestion cylinder disc 13 rotates and the force claw 49 is above the digestion cylinder 12, the force claw 49 loses the thrust, and under the action of the gravity of the blocking gravity ball 47 itself, the blocking gravity ball 47 leaves the opening at the lower end of the flow nitric acid digestion tube 43, and the nitric acid digestion solution 39 can flow downstream of the nitric acid digestion tube 43 into the digestion cylinder 12. According to actual needs, adjust the rotation speed of the fixed switch 42 and the digestion cylinder disc 13 to fix the amount of nitric acid digestion solution 39 flowing into the digestion cylinder 12 at a set amount to ensure the accuracy of the calculated data.
[0010] The beneficial effects of the present invention are as follows: the device for rapidly determining the heavy metal content of animal bone samples by flame color reaction uses a sample grinding preparation device to rapidly and accurately and quantitatively grind the bones of animals such as domestic pigeons into bone powder that is easily digested by a digestion solution such as nitric acid, and quantitatively drops the bone powder into a digestion tube; then, quantitatively adding a digestion solution such as nitric acid in batches for digestion; then, taking out the digestion tube, covering the digestion tube with a digestion tube cover, and placing the digestion tube in a stainless steel reactor for further digestion, that is, placing the digestion tube in an oven at a controlled temperature of 190°C and heating for about 10 hours, so that the powdered bone sample is completely dissolved under the action of the nitric acid digestion solution, and the sample is free of heavy metals. The various elements are released into the nitric acid digestion solution; after that, the digestion cylinder is cooled and taken out from the reactor, the nitric acid digestion solution in the digestion cylinder is filtered using a filter membrane, the filtrate is collected in a 50 ml flat-bottom plastic centrifuge tube, and the volume is fixed to the 50 ml mark with deionized water to obtain a test solution within the linear range of the mass spectrometer detection. The mass spectrometer is turned on to detect the sample, and the specific content of each heavy metal element in the bone sample can be quickly obtained, and then the local atmospheric heavy metal pollution status can be known, thereby achieving the purpose of using the characteristics of the air breathed by animals to quickly and conveniently monitor the heavy metal status in the atmosphere using flame color reaction. The device used for the device for quickly determining the heavy metal content of animal bone samples using flame color reaction is simple to make, highly operable, low cost, and effective. BRIEF DESCRIPTION OF THE DRAWINGS
[0011] The present invention will be further described below with reference to the accompanying drawings.
[0012] Figure 1 This is a schematic diagram of the overall longitudinal section structure of the device for rapidly determining the heavy metal content of animal bone samples using flame color reaction according to the present invention.
[0013] Figure 2 This is a schematic diagram of the digestion cylinder structure of the device for rapidly determining the heavy metal content of animal bone samples using flame color reaction according to the present invention.
[0014] Figure 3 This is a schematic diagram of the longitudinal cross-section structure of the relationship between the support column and the digestion cylinder of the device for quickly determining the heavy metal content of animal bone samples using flame color reaction of the present invention.
[0015] Figure 4 This is a schematic diagram of the structure of the nitric acid digestion bottle of the device for quickly determining the heavy metal content of animal bone samples using flame color reaction according to the present invention.
[0016] Figure 5 This is a schematic diagram of the cross-sectional structure of the hoop tube of the device for rapidly determining the heavy metal content of animal bone samples using flame color reaction according to the present invention.
[0017] Figure 6 The figure is a schematic diagram of the buckle structure of the device for rapidly determining the heavy metal content of animal bone samples using flame color reaction according to the present invention.
[0018] Figure 7 The figure is a schematic diagram of the detection process of the device for rapidly determining the heavy metal content of animal bone samples using flame color reaction according to the present invention.
[0019] In the figure: 1. Bone sample, 2. Bone hoop, 3. Bone hoop, 4. Bone support, 5. Bone spring, 6. Bone stopper, 7. Rotating cylinder shaft, 8. Rivet for fixing the shaft, 9. Rotating ring, 10. Supporting plate column, 11. Material guide trough, 12. Digestion cylinder, 13. Digestion cylinder disk, 14. Digestion cylinder disk rotating motor, 15. Supporting plate column ladder-shaped head rotating cylinder, 16. Digestion cylinder disk pointed cap, 17. Powder drop funnel, 18. Powder collection funnel, 19. Grinding wheel, 20. Grinding wheel motor, 21. Labeling area, 22. Digestion cylinder wall cavity, 23. Digestion cylinder wall, 24. Digestion cylinder cavity, 25. Lifting hole, 26. Digestion cylinder cover, 27. Pointed top plate, 28. Supporting plate column tip, 29. Supporting plate column ladder shaped head, 30. occlusal ring teeth, 31. digestion cylinder disc rotating motor rotor, 32. fixed cylinder column, 33. inner wall of hoop tube, 34. outer wall of hoop tube, 35. hoop tube cavity, 36. nitric acid digestion bottle, 37. nitric acid digestion bottle wall, 38. nitric acid digestion bottle cavity, 39. nitric acid digestion solution, 40. nitric acid digestion bottle neck, 41. nitric acid digestion bottle mouth, 42. fixed switch, 43. nitric acid digestion tube, 44. tube holding ring, 45. arm shaft, 46. force-guiding claw, 47. tube-blocking gravity ball, 48. force-bearing claw arm, 49. force-bearing claw, 50. gravity switch, 51. mass spectrometer, 52. fixing plate, 53. buckle loop, 54. bottle body, 55. sample grinder preparation device. DETAILED DESCRIPTION
[0020] Example 1:
[0021] As shown in the figure, the present invention uses a device for rapidly determining the heavy metal content of an animal bone sample using a flame color reaction. First, the bone sample 1 is placed in a sample grinder 55 for grinding and adding a nitric acid digestion solution 39 for digestion. Then, the digestion tube 12 is removed and covered with a digestion tube cover 26. The digestion tube 12 is placed in a stainless steel reactor for further digestion. That is, the digestion tube 12 is placed in an oven and heated at a controlled temperature of 190° C. for about 10 hours, so that the powdered bone sample 1 is completely dissolved under the action of the nitric acid digestion solution 39, and the various elements in the sample are released into the nitric acid digestion solution 39. Then, the digestion tube 12 is cooled and removed from the reactor. The nitric acid digestion solution 39 in the digestion tube 12 is filtered using a filter membrane, and the filtrate is collected in a 50 ml flat-bottom plastic centrifuge tube. The volume is adjusted to the 50 ml mark with deionized water to obtain a test solution within the linear range of the mass spectrometer 51. The mass spectrometer 51 is turned on to detect the sample, and the specific content of each heavy metal element in the bone sample 1 can be quickly obtained. The sample grinding preparation device 55 comprises a bone sample 1, a bone hoop 2, a bone hoop 3, a bone support tube 4, a top bone spring 5, a tube block 6, a rotating cylinder shaft 7, a fixed shaft rivet 8, a rotating ring 9, a support plate column 10, a material guide trough 11, a digestion cylinder 12, a digestion cylinder disk 13, a digestion cylinder disk rotating motor 14, a support plate column ladder head rotating cylinder 15, a digestion cylinder disk pointed cap 16, a powder falling funnel 17, a powder collecting funnel 18, a grinding wheel 19, a grinding wheel motor 20, a labeling area 21, a digestion cylinder wall cavity 22, a digestion cylinder wall 23, a digestion cylinder cavity 24, a tube lifting concave hole 25, a digestion cylinder cover 26, a pointed top plate 27, and a support plate column tip 28. , the supporting plate column ladder head 29, the bite ring teeth 30, the digestion cylinder disc rotating motor rotor 31, the fixed cylinder column 32, the inner wall of the hoop bone cylinder 33, the outer wall of the hoop bone cylinder 34, the hoop bone cylinder cavity 35, the nitric acid digestion bottle 36, the nitric acid digestion bottle wall 37, the nitric acid digestion bottle cavity 38, the nitric acid digestion solution 39, the nitric acid digestion bottleneck 40, the nitric acid digestion bottle mouth 41, the fixed switch 42, the flow nitric acid digestion tube 43, the tube holding ring 44, the arm shaft 45, the force guide claw 46, the tube blocking gravity ball 47, the force claw arm 48, the force claw 49, the gravity switch 50, the mass spectrometer 51, the fixed plate 52, the buckle loop 53, and the bottle body 54. Bone sample 1 is a bone sample from the animal to be tested, such as the bones of birds like domestic pigeons, mammals like rabbits, amphibians like toads, and reptiles like geckos. The femur of these animals is typically used. Before testing, the femur is cut into 1-2 cm long segments using a saw. If there is bone marrow within the femur, it is removed using forceps or other tools, leaving only the harder bone.The hoop bone tube 2 is a cylindrical structure in which the bone sample 1 is fixed so that the grinding wheel 19 located at the top of the bone sample 1 can quickly grind the top of the bone sample 1 into powder when it rotates rapidly. The hoop bone tube 2 is the cylindrical part above the support bone tube 4. It shares a fixed tube column 32 with the support bone tube 4 and is connected together through the fixed tube column 32. The height of the hoop bone tube 2 is 0.9-1.8 cm. The hoop bone tube 2 consists of a fixed tube column 32, an inner wall 33 of the hoop bone tube, an outer wall 34 of the hoop bone tube, and a hoop bone tube cavity 35. The fixed tube column 32 is made of manganese steel. The support column shared by the support bone tube 4 has a square cross-section with a side length of 3-5 mm. It is solid, the upper end extends to the top edge of the hoop bone tube 2, and the lower end is welded and fixed to the upper surface of the rotating cylinder shaft 7. The base of the inner side wall 33 of the hoop bone tube and the outer side wall 34 of the hoop bone tube 2 are welded and fixed together, and the outer surface of the base is welded and fixed to one side of the solid tube column 32. The outer surface of the simplified outer surface of the support bone tube 4 is also welded on the same side. The inner side wall 33 of the hoop bone tube is made of spring steel, with an arc-shaped cross-section, a base thickness of 2-3 mm, and a free end thickness of 0.5-1 mm. m, the free end of the inner side wall 33 of the hoop bone tube extends to the inside of the free end of the outer side wall 34 of the hoop bone tube; the outer side wall 34 of the hoop bone tube is made of spring steel, has an arc-shaped cross-section, a base thickness of 2-3 mm, a free end thickness of 0.5-1 mm, and the free end of the outer side wall 34 of the hoop bone tube extends to the outside of the free end of the inner side wall 33 of the hoop bone tube; the hoop bone tube cavity 35 is a cavity surrounded by the inner side wall 33 and the outer side wall 34 of the hoop bone tube, and the interior is used to place the bone sample 1; because the free ends of the inner side wall 33 and the outer side wall 34 of the hoop bone tube partially overlap and are close together , are not connected together, so after the bone sample 1 is placed in the hoop bone tube cavity 35, the diameter of the hoop bone tube cavity 35 can change with the size of the diameter of the bone sample 1. If the diameter of the bone sample 1 is large, the diameter of the hoop bone tube cavity 35 will be stretched and enlarged. If the diameter of the bone sample 1 is small, the diameter of the hoop bone tube cavity 35 will recover and become smaller due to the elasticity of the spring steel. Once the bone sample 1 is placed in the hoop bone tube cavity 35, the bone sample 1 is fixed, and the diameter of the hoop bone tube cavity 35 can no longer change. Therefore, two upper and lower hoop bone tube hoops 3 are further provided on the hoop bone tube 2;The structure of the hoop bone tube hoop 3 is the same as the commercially available adjustable iron hoop, that is, the iron hoop is annular, and the inner surface of the ring body relative to the adjusting buckle is welded to the other surface of the fixed tube column 32 relative to the surface where the base of the inner wall 33 of the hoop bone tube and the outer wall 34 of the hoop bone tube are located. The two parts of the adjusting buckle can move relative to each other under the action of the fixed top buckle. Once they move to tightly clamp the hoop bone tube 2, they stop and are fixed together and no longer move relative to each other, thereby firmly fixing the bone sample 1 in the hoop bone tube cavity 35 without tilting or expanding. At most, the bone sample 1 can be moved to the outside under the action of the top bone spring 5 in the support bone tube 4. The hoop bone cylinder cavity 35 extends upward, and the upper end of the bone sample 1 extends to the lower surface of the grinding wheel 19. As the upper end of the bone sample 1 is ground into powder by the grinding wheel 19 and becomes shorter, the bone sample 1 is continuously pushed upward by the top bone spring 5 until it is almost worn out and pushed out of the hoop bone cylinder cavity 35 by the top bone spring 5. The ground bone sample 1 is thrown out under the action of centrifugal force and gravity, and falls into the powder collecting funnel 18 and the powder falling funnel 17 to be collected, and falls into the guide trough 11 or the digestion cylinder 12 along the powder falling funnel 17. The speed of the digestion cylinder disc 13 is controlled so that the amount of bone powder falling into each digestion cylinder 12 is 0 .1 gram; during the rotation of the digestion tube 12, when a digestion tube 12 is transferred to the bottom of the nitric acid digestion bottle 36, 5 ml of nitric acid digestion solution 39 can be injected into the digestion tube 12, and the bone powder can be digested by the nitric acid digestion solution 39 in the digestion tube 12, and the metal elements in the sample are converted into a single valence state. When all the digestion tubes 12 around the periphery of a digestion tube plate 13 are injected with nitric acid digestion solution 39, the digestion tubes 12 with numbers on the tube wall are taken out in turn, and then the digestion tube cover 26 of the digestion tube 12 is covered, and the digestion tube 12 is placed in a stainless steel reactor and placed in an oven to control the temperature 19 The powdered bone sample 1 is heated at 0°C for approximately 10 hours to completely dissolve in the nitric acid digestion solution 39, releasing the various elements in the sample into the nitric acid digestion solution 39. The digestion cylinder 12 is then cooled and removed from the reactor. The nitric acid digestion solution 39 in the digestion cylinder 12 is filtered using a membrane filter. The filtrate is collected in a 50 ml flat-bottom plastic centrifuge tube and diluted to the 50 ml mark with deionized water to obtain a test solution within the linear range of the mass spectrometer 51. The mass spectrometer 51 is then turned on to test the sample, quickly obtaining the specific content of each heavy metal element in the bone sample 1. The mass spectrometer 51 is a commercially available inductively coupled plasma mass spectrometer capable of rapid quantitative determination of heavy metals in bone samples. The bone support tube 4 is a cylindrical tube below the hoop tube 2. Made of manganese steel, the tube wall thickness is 1-3 mm, the height is 3-5 cm, and the inner diameter is 1-5 cm. A bone ejection spring 5 is located within the tube 4. Once the bone sample 1 is placed within the hoop tube 2, this spring can eject the bone sample 1 from the bottom up. The lower end of the bone support tube 4 is welded to the upper surface of the free end of the rotating shaft 7, and the upper end is connected to the hoop tube 2 via a fixing column 32. The lower end of the fixing column 32 is also welded to the upper surface of the free end of the rotating shaft 7.The process of grinding the bone sample 1 into bone powder and collecting the bone powder after it is placed is as follows: after the bone sample 1 is placed in the bone hoop tube 2, the bone support tube 4 is rotated and pushed into the depression in front of the blocking tube block 6. At the same time, the bone sample 1 is pressed downward so that the bone sample 1 is between the top bone spring 5 and the grinding wheel 19, so that when the grinding wheel 19 rotates, the bone sample 1 can be ground into bone powder little by little, and under the action of the centrifugal force generated during the rotation, it falls into the powder collecting funnel 18 and the powder dropping funnel 17 to be collected; the top bone spring 5 is a spring whose lower end is fixed to the inner surface of the bottom wall of the bone support tube 4, and a disc-shaped baffle is fixed on the upper end. In the natural state, after the top bone spring 5 is stretched, the top end of the top bone spring 5 blocks the The upper surface of the plate is flush with the top edge of the hoop bone tube 2, but when the bone sample 1 is inserted into the hoop bone tube 2, the top bone spring 5 is pressed down to form spring potential energy, so that the entire bone sample 1 has the force to be completely pushed out of the hoop bone tube 2. With the help of this force, the bone sample 1 can gradually move upward as it is worn and eventually be ground into bone powder; the baffle block 6 is a baffle that blocks the support bone tube 4 to prevent the thrust generated by the grinding wheel 19 during rotation from throwing the bone sample 1 out and causing the position to move. The baffle block 6 is made of manganese steel, has an arc-shaped cross-section, a height of 2.5-4 cm and a thickness of 3-5 mm. The lower end is welded and fixed to the upper surface of the fixed plate 52, and the upper end is free. The central axis of the baffle block 6 in the vertical direction is perpendicular to the diameter of the support bone tube 4. , located in the plane of the diameter, so that the blocking block 6 can play the best blocking role; the rotating cylinder shaft 7 is connected to the rotating ring 9 and the bone support tube 4, so that the bone sample 1 can be more conveniently placed in the hoop bone tube 2 after the bone support tube 4 leaves the grinding wheel 19. One end of the rotating cylinder shaft 7 is welded and fixed to the side wall of the rotating ring 9, and the other end is free and the upper surface is welded to the bone support tube 4 and the lower end of the fixed tube column 32. The rotating cylinder shaft 7 is made of manganese steel and has a rectangular cross-section. The long side of the rectangular rotating cylinder shaft 7 is set horizontally with a length of 5-8 mm and the short side is set vertically with a length of 3-5 mm; the rotating ring 9 is a circular ring that the rotating cylinder shaft 7 rotates around the fixed shaft rivet 8, so that the bone support tube 4 can approach or move away from the blocking cylinder block 6, the rotating ring 9 The ring body is made of manganese steel, and the cross-section of the ring body is a square with a side length of 2-5 mm. The diameter of the cylindrical inner cavity surrounded by the ring body is 5-8 mm. The fixed axis rivet 8 is enlarged at the upper part, and the lower end of the lower part is fixed to the upper surface of the fixed plate 52 by a bolt structure. The fixed axis rivet 8 is made of manganese steel and is divided into upper and lower parts. The upper part of the fixed axis rivet 8 is in the shape of a hexagonal prism, the distance between the two opposite faces of the hexagonal prism is 7-13 mm, and the height of the hexagonal prism is 3-5 mm; the lower part of the fixed axis rivet 8 is cylindrical, the diameter of the cylinder is 4.5-7 mm, and the height is 1-2 cm. The lower part of the fixed axis rivet 8 is divided into upper and lower halves. The upper half of the lower part of the fixed axis rivet 8 has a smooth surface so that the swivel 9 can rotate around it.The lower half of the lower part of the fixed axis rivet 8 has a threaded surface, which is engaged with the thread on the inner surface of the groove provided at this location of the fixing plate 52, so as to fix the entire fixed axis rivet 8 on the fixing plate 52. The support column 10 is a pillar that supports the digestion cylinder 13 and allows the digestion cylinder 13 to rotate. It is made of manganese steel and is divided into two parts, the lower part of the support column 10 is cylindrical, with a diameter of 1-2 cm and a height of 3-5 cm; the upper part of the support column 10 is ladder-shaped, called the support column ladder head 29. The support column ladder head 29 has 3 levels, and its diameter decreases step by step. The lower 2 levels are cylindrical, and the uppermost level is conical, also known as the support column tip 28. The pointed top of the conical support column tip 28 directly abuts against the center of the lower surface of the pointed top plate 27. The pointed top plate 27 is a cylindrical support column ladder head rotating cylinder 15 provided at the top of the central lower surface of the digestion cylinder pointed cap 16. The pad is made of manganese steel with a diameter of 3-5 mm and a thickness of 3-5 mm. Since the support column tip 28 and the top plate 27 are both made of manganese steel and the contact area is small, the friction between the two is small, and the digestion cylinder disc 13 can be driven to rotate around the support column 10 with a small force; the digestion cylinder disc 13 is a disc on which the digestion cylinder 12 is placed, and is divided into an inner and an outer part. The outer part of the digestion cylinder disc 13 is annular, and the cross-section of the annular ring body is rectangular. The length of the rectangle is 2-3 cm and the width is 1.5-2 cm. A plurality of cylindrical grooves with a cross-sectional diameter of 1-1.5 cm are evenly spaced on the upper surface of the rectangular cross-sectional ring body. A digestion cylinder 12 is placed in each groove, and the outer surface of the digestion cylinder 12 is close to the inner wall of the groove. The width of the gap between the digestion cylinder 12 and the groove is 0.01-0.1 mm. As the digestion cylinder disc 13 rotates, the digestion cylinder 12 passes through the lower end of the powder falling funnel 17 in turn, and the bone powder formed by the grinding wheel 19 grinding the bone sample 1 falls into the digestion cylinder 12. Since the rotation speed of the grinding wheel 19 and the digestion cylinder disc 13 is constant, the amount of bone powder falling into each digestion cylinder 12 is constant and almost equal; the interior of the digestion cylinder disc 13 is conical, also known as the digestion cylinder disc pointed cap 16, which is to set the entire digestion cylinder disc 13 above the support disc column tip 28 And it can accept the power generated by the digestion cylinder disc rotating motor 14 to rotate. The cylindrical structure with an opening to the lower surface just below the top is the support disc column ladder head rotating cylinder 15. The support disc column ladder head rotating cylinder 15 is divided into 4 levels. Each of the upper 3 levels is engaged with the structure of the support disc column ladder head 29. The 3 levels of the support disc column ladder head rotating cylinder 15 are 0.5-1 mm apart from the support disc column ladder head 29. The lowest level is located outside the lower part of the support disc column 10 and is cylindrical. A digestion cylinder disc rotating motor 14 is provided at each end of a diameter along the central axis of the support disc column 10 between the lowest level of the support disc column ladder head rotating cylinder 15 and the lower part of the support disc column 10.The digestion cylinder disc rotating motor 14 is a well-known electric motor, which can rotate under the action of electric energy transmitted from the power line set on the surface or inside of the support disc column 10. A commercially available frequency conversion modulator is also set on the power line to adjust the speed of the digestion cylinder disc rotating motor 14. According to the specific conditions of different bone samples 1, the speed of the digestion cylinder disc rotating motor 14 is adjusted to allow a specific amount of bone powder to fall into the digestion cylinder 12; the digestion cylinder disc rotating motor rotor 31 is the rotor of the digestion cylinder disc rotating motor 14, and has teeth on the surface, which can mesh with the teeth of the bite ring teeth 30. When the digestion cylinder disc rotating motor 14 is working and the digestion cylinder disc rotating motor rotor 31 rotates, it can drive the bite ring teeth 30 to rotate, thereby making the entire digestion cylinder disc 13 rotate around the support disc. The column tip 28 rotates; the occlusal ring teeth 30 are made of manganese steel and are annular in shape as a whole. The outer surface of the occlusal ring teeth 30 is smooth and welded to the inner surface of the lowest step-shaped rotating cylinder 15 of the support column. The inner surface of the occlusal ring teeth 30 has a gear, and the teeth of the gear mesh with the teeth of the digestion cylinder disc rotating motor rotor 31; the height of the digestion cylinder disc rotating motor rotor 31 is 3-5 mm, and the height of the occlusal ring teeth 30 ring body is 5-8 mm; the upper surface of the outer ring body of the digestion cylinder disc 13 between the two adjacent digestion cylinders 12 is provided with a groove having an arc-shaped cross section, and these grooves and the inner cavity of the digestion cylinder 12 together form a guide trough 11 so that the fallen bone powder can smoothly enter the digestion cylinder 12; the digestion cylinder 12 is made of polytetrafluoroethylene and is cylindrical. The tube 12 is composed of a numbered area 21, a digestion tube wall cavity 22, a digestion tube wall 23, a digestion tube cavity 24, a tube lifting recess 25, and a digestion tube cover 26. The digestion tube wall 23 is the wall around and at the bottom of the digestion tube 12. It is a double-layer structure, consisting of an inner wall and an outer wall. The cavity between the inner wall and the outer wall is the digestion tube wall cavity 22. The setting of the digestion tube wall cavity 22 can reduce the weight of the digestion tube 12 on the one hand, and on the other hand, it can facilitate the setting of other structures in the digestion tube wall cavity 22, such as the tube lifting recess 25; the height of the inner wall of the digestion tube wall 23 is lower than the height of the outer wall, so an inclined surface is formed on the upper edge of the digestion tube wall 23 to facilitate the digestion tube cover 26 to cover the upper mouth of the digestion tube 12, and at the same time, a pair of tube lifting recesses 25 are symmetrically arranged on the inclined surface for convenient buckle use. The loop 53 lifts the digestion cylinder 12 out of the groove; the lifting cylinder concave hole 25 is two grooves arranged horizontally on the upper inclined surface of the digestion cylinder 12, and the two grooves are at both ends of a diameter of the cross section of the digestion cylinder 12. The opening of the lifting cylinder concave hole 25 faces inward, and the opening is between the inner wall and the upper end of the outer wall of the digestion cylinder wall 23. The bottom of the lifting cylinder concave hole 25 is blocked. When the two horizontally arranged convex shafts of the outermost side of the buckle loop 53 are inserted into the lifting cylinder concave hole 25, the entire buckle loop 53 is fixed to the upper position of the digestion cylinder 12. The buckle loop 53 can rotate in the lifting cylinder concave hole 25, and the buckle loop 53 stands up or falls on the upper mouth of the digestion cylinder 12. When the digestion cylinder 12 needs to be lifted, the buckle loop 53 can be lifted and the entire digestion cylinder 12 can be lifted out of the groove on the outer ring body of the digestion cylinder disc 13;The buckle 53 is made of spring steel and has a circular cross-section with a diameter of 1-3 mm. The buckle 53 consists of a horizontal axis, a grip axis, a vertical axis, and a convex axis. There is only one horizontal axis, which is located at the top and innermost part. Its length is determined by the distance between the openings of the two lifting tube recesses 25, and is generally half the distance between the openings of the two lifting tube recesses 25. The grip axis is a curved axis that is convenient for people to hold with their hands. The upper end is connected to the two ends of the horizontal axis and is approximately; shape or The shape of the handle, when holding the handle by hand, can bring the convex shafts on both sides closer, narrowing the distance between the lower ends of the two vertical shafts, so that the convex shafts can be more conveniently inserted into the lifting tube recessed hole 25; the vertical shaft is the shaft located in the vertical direction at the lower end of the handle, a total of 2, the lower end of the vertical shaft is connected to the inner end of the convex shaft, the distance between the two vertical shafts is equal to the distance between the openings of the two lifting tube recessed holes 25; the convex shaft is the shaft arranged in the two horizontal directions on the outermost side of the buckle 53, when the convex shaft is inserted into the lifting tube recessed hole 25, the entire buckle 53 is naturally located at the upper position of the digestion tube 12; the digestion tube cavity 24 is a cavity surrounded by the digestion tube wall 23, and is also the inner cavity where the bone powder is digested in the digestion tube 12 after the digestion substance is added; label
[0022] Area 21 is an area located in the center of the outer surface of the outer wall of the digestion cylinder wall 23, which is square. Different numbers are made in the numbered area 21, which are determined according to the size of the outer ring of the digestion cylinder disk 13. For example, if 16 grooves are set, the numbered areas 21 are marked as 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, and 16 respectively. In this way, when the experiment is tested, the respective processing is recorded in the experimental record book, which will not cause confusion of the bone sample 1; the digestion cylinder cover 26 is a cover that is covered on the upper mouth of the digestion cylinder 12 so that the bone powder of the digestion cylinder 12 is digested. The digestion cylinder cover 26 is Polytetrafluoroethylene, in the shape of an arc, the highest point from the center of the plane circle where the bottom edge is located is 1-2 mm, the diameter of the plane circle where the bottom edge is located is equal to the distance between the openings of the two lifting cylinder recesses 25; the powder falling funnel 17 is a funnel that drains the bone powder collected by the powder collecting funnel 18 into the external guide trough 11 of the digestion cylinder plate 13, which is made of plastic and has a wall thickness of 0.2-0.5 mm. The upper opening of the powder falling funnel 17 is located at the bottom edge of the powder collecting funnel 18, is circular, has a diameter of 3-5 cm, and is arranged in the horizontal direction; the lower opening of the powder falling funnel 17 is free and elliptical, the long diameter of the ellipse is 1-2 cm, the short diameter is 0.5-1 cm, and is 45 to the horizontal direction. °The angle is set, the opening of the lower end of the powder falling funnel 17 faces the direction of rotation of the digestion cylinder disc 13, and the wall of the opening extends into the digestion cylinder cavity 24 by about 0.5-1 mm. The specific way in which the bone powder in the powder falling funnel 17 falls onto the guide trough 11 is as follows: since the plastic wall thickness at the opening of the powder falling funnel 17 is 0.2-0.5 mm, which is relatively thin and elastic, during the rotation of the digestion cylinder disc 13, the bone powder falling on the guide trough 11 between the two adjacent digestion cylinders 12 can be scraped into the digestion cylinder 12 like a scraper. When it rotates to the upper end of the digestion cylinder cavity 24, the elasticity of the opening at the lower end of the powder falling funnel 17 can also form an oscillation for the powder falling funnel 17, thereby And better shake off the bone powder that may remain in the powder falling funnel 17; the powder collecting funnel 18 is located below the grinding wheel 19, and the grinding wheel 19 is quickly rotated to grind the bone powder formed on the upper end of the bone sample 1 to collect the bone powder together and finally fall into the powder falling funnel 17 with the help of the bone powder's own gravity and the vibration formed at the lower end opening of the powder falling funnel 17. The funnel is made of plastic with a wall thickness of 0.2-0.5 mm. The powder collecting funnel 18 is divided into two parts, the upper part of the powder collecting funnel 18 is cylindrical, and the cylinder has no upper and lower bottoms, only walls around it. The height of the upper part of the powder collecting funnel 18 is 3-5 cm, and the lower edge of the cylindrical wall is at the same level as the lower surface of the grinding wheel 19. The powder collecting funnel 18 is in the shape of an elephant trunk at the bottom, and the upper edge of the lower part of the powder collecting funnel 18 is connected to the lower edge of the upper part, and then it shrinks and becomes smaller, converges toward the upper end of the powder falling funnel 17 and finally reaches the upper end of the powder falling funnel 17. An opening is also provided at the wall of the lower part of the powder collecting funnel 18 corresponding to the hoop bone tube 2, for the hoop bone tube 2 to extend into the powder collecting funnel 18, for the grinding wheel 19 to grind the bone sample 1 into bone powder; the grinding wheel 19 is a commercially available grinding wheel, which is cylindrical, with a diameter of 5-10 cm and a height of 5-20 mm. A manganese steel shaft is provided in the center of the upper surface of the grinding wheel 19, which can be fixed together with the rotor of the grinding wheel motor 20. When the motor 20 is working, it can drive the grinding wheel 19 to rotate rapidly, thereby grinding the bone sample 1 into bone powder. The grinding wheel motor 20 is a commercially available electric motor fixed to the inner surface of the top wall of the sample grinding and powder preparation device 55. When powered on, it can drive the grinding wheel 19 to rotate rapidly. The nitric acid digestion bottle 36 is a structure that contains nitric acid digestion solution 39 and releases the nitric acid digestion solution 39 into the digestion cylinder 12 in a quantitative manner as the digestion cylinder disc 13 rotates. The upper end of the nitric acid digestion bottle 36 is fixed to the inner surface of the top wall of the sample grinding and powder preparation device 55, and the lower end of the nitric acid digestion bottle 36 is free. The force claw 49 of the gravity switch 50 at the lower end of the nitric acid digestion bottle 36 extends into the digestion cylinder cavity 24 by about 0.5-1 mm, the specific method of the nitric acid digestion bottle 36 controlling the flow of the nitric acid digestion solution 39 out of the nitric acid digestion tube 43 is as follows: when the digestion cylinder 13 rotates and the force claw 49 is above the guide groove 11, since the force claw 49 is made of spring steel and has elasticity, the force claw 49 can slide along the guide groove 11, but the force between the force claw 49 and the guide groove 11 pushes the force claw 49 in the opposite direction of the rotation of the digestion cylinder 13, forming a thrust, thereby blocking the blockage. The pipe gravity ball 47 is tightly pressed against the opening at the lower end of the flowing nitric acid digestion pipe 43, blocking the opening, and the nitric acid digestion solution 39 will not flow out; but when the digestion cylinder disc 13 rotates and the force claw 49 is above the digestion cylinder 12, the force claw 49 loses the thrust, and under the action of the gravity of the pipe blocking gravity ball 47 itself, the pipe blocking gravity ball 47 leaves the opening at the lower end of the flowing nitric acid digestion pipe 43, and the nitric acid digestion solution 39 can flow down the nitric acid digestion pipe 43 into the digestion cylinder 12 According to actual needs, the fixed switch 42 and the rotation speed of the digestion cylinder disk 13 are adjusted to keep the amount of nitric acid digestion solution 39 flowing into the digestion cylinder 12 fixed at the set amount to ensure the accuracy of the calculated data; the nitric acid digestion bottle 36 consists of a bottle body 54, nitric acid digestion solution 39, a fixed switch 42, a nitric acid digestion flow pipe 43 and a gravity switch 50. The bottle body 54 includes a nitric acid digestion bottle wall 37, a nitric acid digestion bottle cavity 38, a nitric acid digestion bottle neck 40 and a nitric acid digestion bottle mouth 41. The nitric acid digestion bottle wall 37 is the outer wall of the bottle body 54, which is made of glass and has a thickness of 1-2 mm; the nitric acid digestion bottle cavity 38 is the cavity surrounded by the nitric acid digestion bottle wall 37 for holding the nitric acid digestion solution 39; the nitric acid digestion bottle neck 40 is the part of the lower part of the bottle body 54 that tapers to the nitric acid digestion bottle mouth 41; the nitric acid digestion bottle mouth 41 is the opening at the lower end of the bottle body 54 for releasing the nitric acid digestion solution 39, and the inner cavity diameter is 1-1.5 cm, and the lower end opening of the bottle body 54 is blocked by a bottle stopper; the fixed switch 42 is a valve set on the bottle stopper. The opening amplitude of the fixed switch 42 determines the speed at which the nitric acid digestion solution 39 flows out of the nitric acid digestion bottle mouth 41, and cooperates with the gravity switch 50 to accurately control the amount of nitric acid digestion solution 39 flowing into the digestion cylinder 12; the nitric acid digestion solution 39 is nitric acid, etc., which can digest and convert the heavy metals in the bone powder into a single valence state, so as to facilitate the subsequent use of flame color reaction to quickly detect the type and content of heavy metals contained in the bone sample 1 The digestion liquid; the flow nitric acid digestion tube 43 is an infusion tube for flowing the nitric acid digestion liquid 39 into the digestion cylinder 12, which is made of glass. The upper end of the flow nitric acid digestion tube 43 is controlled by the fixed switch 42 to open and close. The lower end of the flow nitric acid digestion tube 43 is an oblique opening, and a rubber pad is provided at the opening so that the gravity ball 47 of the gravity switch 50 can tightly block the opening at the lower end of the flow nitric acid digestion tube 43; the gravity switch 50 blocks the opening at the lower end of the flow nitric acid digestion tube 43 by means of the thrust between the force-bearing claw 49 and the guide trough 11, and the force When the claw 49 is above the digestion tube 12, due to the lack of thrust, under the gravity of the blocking gravity ball 47, the blocking gravity ball 47 leaves the opening at the lower end of the nitric acid digestion tube 43, and then the nitric acid digestion solution 39 flows into the switch of the digestion tube 12. The gravity switch 50 and the fixed switch 42 work together, coordinate and cooperate with each other to quantitatively release the nitric acid digestion solution 39 into the digestion tube 12; the gravity switch 50 is made of spring steel and is composed of a tube holding ring 44, an arm shaft 45, a guide claw 46, a blocking gravity ball 47, force claw arm 48, and force claw 49. The tube holding ring 44 is a ring tube surrounding the nitric acid digestion tube 43. Its overall shape is a central drum with pointed ends. The nitric acid digestion tube 43 is located in the center of the central drum of the tube holding ring 44. One end of the tube holding ring 44 is connected to the arm rotating shaft 45 and can move up and down around the arm rotating shaft 45. The other end is connected to the upper end of the force guiding claw 46. When the tube holding ring 44 is tilted upward, it can drive the force guiding claw 46 to rise. The arm rotating shaft 45 is the rotating shaft that fixes the tube holding ring 44 and the force claw arm 48. The upper horizontal bar is the rotating shaft in the through-holes on both sides of one end of the tube holding ring 44, and the downward vertical bar is the supporting shaft extending inward from the center of one end of the tube holding ring 44, and the inner end of the vertical bar is fixed on the outer surface of the flow nitric acid digestion tube 43; the guide claw 46 is arc-shaped, one end of which is connected to one end of the tube holding ring 44, and the other end is connected to the blocking gravity ball 47. When the tube holding ring 44 is lifted, the guide claw 46 can pull the blocking gravity ball 47 away from the opening at the lower end of the flow nitric acid digestion tube 43. When the tube holding ring 44 falls, the guide claw 46 can push the blocking gravity ball 47 to block the opening at the lower end of the flow nitric acid digestion tube 43; the force claw arm 48 is the connecting arm between the tube holding ring 44 and the force claw 49, and is arc-shaped. When the force claw 49 is aligned with the guide trough 11 When in contact, as the digestion cylinder disc 13 rotates, the force claw arm 48 extends forward, driving the pipe-blocking gravity ball 47 to block the opening at the lower end of the flowing nitric acid digestion tube 43; when the force claw 49 slides into the digestion cylinder 12, the force claw 49 is unable to push, and with the help of the gravity of the pipe-blocking gravity ball 47 itself, the pipe-blocking gravity ball 47 is pulled away from the opening at the lower end of the flowing nitric acid digestion tube 43; the force claw 49 is a thin spring steel sheet with strong elasticity and toughness. Although it extends into the digestion cylinder cavity 24 of the digestion cylinder 12 by about 0.5-1 mm, it can still bend elastically and slide freely in the material guide trough 11 as the digestion cylinder disc 13 rotates, and generates thrust during the sliding process, so that the pipe-blocking gravity ball 47 blocks the opening at the lower end of the flowing nitric acid digestion tube 43.
[0023] After measurement, the characteristic peaks of several common heavy metals after flame color reaction are shown in the table below.
[0024] Table: Common heavy metal characteristic peaks
[0025]
[0026] The above shows and describes the basic principles, main features and advantages of the present invention. It should be understood by those skilled in the art that the present invention is not limited to the above embodiments. The above embodiments and descriptions are merely illustrative of the principles of the present invention. Various changes and improvements may be made to the present invention without departing from the spirit and scope of the present invention. Such changes and improvements fall within the scope of protection claimed by the present invention, which is defined by the appended claims and their equivalents.
Claims
1. A device for rapidly determining the heavy metal content of animal bone samples using flame color reaction, wherein the bone sample (1) is first placed in a sample grinding preparation device for grinding and adding nitric acid digestion solution (39) for digestion, then the digestion tube (12) is taken out and covered with the digestion tube cover (26) of the digestion tube (12), and the digestion tube (12) is placed in a stainless steel reactor for further digestion, that is, the digestion tube (12) is placed in an oven and heated at a controlled temperature of 190° C. for about 10 hours, so that the powdered bone sample (1) is completely dissolved under the action of the nitric acid digestion solution (39), and the various elements in the sample are released into the nitric acid digestion solution (39); then, the digestion tube (12) is cooled, taken out from the reactor, and the nitric acid digestion solution (39) in the digestion tube (12) is filtered using a filter membrane, and the filtrate is received in a 50 ml flat-bottom plastic centrifuge tube, and the filtrate is determined with deionized water. The sample powder preparation device is filled to the 50 ml mark to obtain a solution to be tested within the linear range of the mass spectrometer (51), and the mass spectrometer (51) is turned on to detect the sample, so as to quickly obtain the specific content of each heavy metal element in the bone sample (1); the sample grinding preparation device is composed of a bone sample (1), a hoop bone tube (2), a hoop bone tube hoop (3), a support bone tube (4), a top bone spring (5), a blocking tube block (6), a rotating cylinder shaft (7), a fixed axis rivet (8), a rotating ring (9), a support disk column (10), a digestion cylinder (12), a digestion cylinder disk (13), a digestion cylinder disk rotating motor (14), a digestion cylinder disk pointed cap (16), a powder dropping funnel (17), a powder collecting funnel (18), a grinding wheel (19), a grinding wheel motor (20), a pointed top plate (27), a nitric acid digestion bottle (36), a fixed plate (52), and a buckle loop (53), and is characterized in that: The bone sample (1) is a bone sample of an animal to be tested, such as the bones of birds such as domestic pigeons, the bones of mammals such as rabbits, the bones of amphibians such as toads, and the bones of reptiles such as geckos. The femurs of these animals are usually used. Before testing, the femurs are cut into long segments with a length of 1-2 cm with a saw. If there is bone marrow in the femur, the bone marrow needs to be removed with tools such as tweezers, leaving only the relatively hard bone part. The hoop bone tube (2) is the cylindrical part above the support bone tube (4), and shares a fixed tube column (32) with the support bone tube (4) and is connected together through the fixed tube column (32). The height of the hoop bone tube (2) is 0.9-1.8 cm. The hoop bone tube (2) is composed of The invention relates to a cylindrical support column (32), a hoop bone tube inner side wall (33), a hoop bone tube outer side wall (34), and a hoop bone tube cavity (35). The cylindrical support column (32) is made of manganese steel and is a supporting column shared by the hoop bone tube (2) and the support bone tube (4). The cross section is square, the side length of the square is 3-5 mm, the solid column, the upper end extends to the top edge of the hoop bone tube (2), and the lower end is welded and fixed to the upper surface of the rotating cylinder shaft (7). The base of the hoop bone tube inner side wall (33) and the hoop bone tube outer side wall (34) of the hoop bone tube (2) are welded and fixed together, and the outer surface of the base is welded and fixed on one side of the cylindrical support column (32). The outer surface of the cylinder of the support bone tube (4) is also welded on the same side. The inner wall (33) is made of spring steel, has an arc-shaped cross section, a base thickness of 2-3 mm, a free end thickness of 0.5-1 mm, and the free end of the inner wall (33) of the hoop bone tube extends to the inner side of the free end of the outer wall (34) of the hoop bone tube; the outer wall (34) of the hoop bone tube is made of spring steel, has an arc-shaped cross section, a base thickness of 2-3 mm, a free end thickness of 0.5-1 mm, and the free end of the outer wall (34) of the hoop bone tube extends to the outside of the free end of the inner wall (33) of the hoop bone tube; the hoop bone tube cavity (35) is a cavity surrounded by the inner wall (33) of the hoop bone tube and the outer wall (34) of the hoop bone tube, and the interior is used to place the bone sample (1); the support bone tube (4) is The cylindrical tube below the hoop tube (2) is a support tube (4) made of manganese steel, with a tube wall thickness of 1-3 mm, a height of 3-5 cm, and an inner cavity diameter of 1-5 cm. A top bone spring (5) is set in the support tube (4). The lower end of the support tube (4) is welded to the upper surface of the free end of the rotating cylinder shaft (7), and the upper end is connected to the hoop tube (2) through a fixed tube column (32). The lower end of the fixed tube column (32) is also welded and fixed to the upper surface of the free end of the rotating cylinder shaft (7); the top bone spring (5) is a spring whose lower end is fixed to the inner surface of the tube wall at the bottom end of the support tube (4), and a disc-shaped baffle is fixed to the upper end; the baffle block (6) is made of manganese steel, has an arc-shaped cross section, and a height of 2.5-4 cm, 3-5 mm thick, the lower end is welded and fixed on the upper surface of the fixed plate (52), the upper end is free, the middle axis of the block block (6) in the vertical direction is perpendicular to a diameter of the support tube (4), and is located in the plane where the diameter is located; one end of the rotating cylinder shaft (7) is welded and fixed on the side wall of the rotating ring (9), the other end is free and the upper surface is welded to the lower end of the support tube (4) and the fixed cylinder column (32), the rotating cylinder shaft (7) is made of manganese steel, and the cross section is rectangular, the long side of the rectangular rotating cylinder shaft (7) is set in the horizontal direction, the length is 5-8 mm, and the short side is set in the vertical direction, the length is 3-5 mm; the rotating ring (9) is made of manganese steel, and the cross section of the ring body is 2 -5 mm square, the diameter of the cylindrical inner cavity surrounded by the ring body is 5-8 mm; the fixed axis rivet (8) is made of manganese steel and is divided into upper and lower parts. The upper part of the fixed axis rivet (8) is in the shape of a hexagonal prism, the distance between the two opposite faces of the hexagonal prism is 7-13 mm, and the height of the hexagonal prism is 3-5 mm; the lower part of the fixed axis rivet (8) is in the shape of a cylinder, the diameter of the cylinder is 4.5-7 mm, and the height is 1-2 cm. The lower part of the fixed axis rivet (8) is divided into upper and lower halves, and the surface of the upper half of the lower part of the fixed axis rivet (8) is smooth; the surface of the lower half of the lower part of the fixed axis rivet (8) is threaded, and the thread is just in line with the groove provided in the fixing plate (52) The threads on the surface are meshed; the support column (10) is made of manganese steel and is divided into two parts, the lower part of the support column (10) is cylindrical, with a diameter of 1-2 cm and a height of 3-5 cm; the upper part of the support column (10) is ladder-shaped, called the support column ladder head (29), the support column ladder head (29) has 3 levels, and its diameter decreases step by step. The lower 2 levels are cylindrical, and the uppermost level is conical, also known as the support column tip (28). The top of the conical support column tip (28) directly contacts the center of the lower surface of the pointed top plate (27). The pointed top plate (27) is set at the top of the central support column ladder head rotating cylinder (15) on the lower surface of the digestion cylinder pointed top cap (16). The cylindrical pad is made of manganese steel, with a diameter of 3-5 mm and a thickness of 3-5 mm; the digestion cylinder disc (13) is a disc for placing the digestion cylinder (12), which is divided into an inner part and an outer part. The outer part of the digestion cylinder disc (13) is annular, and the cross section of the annular ring body is rectangular. The length of the rectangle is 2-3 cm and the width is 1.5-2 cm. A plurality of cylindrical grooves with a cross section diameter of 1-1.5 cm are evenly spaced on the upper surface of the rectangular ring body. A digestion cylinder (12) is placed in each groove. The outer surface of the digestion cylinder (12) is close to the inner wall of the groove. The width of the gap between the digestion cylinder (12) and the groove is 0.01-0.1 mm; the interior of the digestion cylinder (13) is conical, also known as the digestion cylinder pointed cap (16), and the cylindrical structure with an opening to the lower surface just below the top is the support column ladder head rotating cylinder (15), and the support column ladder head rotating cylinder (15) is divided into 4 levels, and each of the upper 3 levels is engaged with the structure of the support column ladder head (29). The 3 levels of the support column ladder head rotating cylinder (15) and the support column ladder head (29) are 0.5-1 mm apart, and the lowest level is located outside the lower part of the support column (10) and is cylindrical. A digestion cylinder rotating motor (14) is provided at each end of a diameter along the central axis of the support column (10) between the lowest level of the support column ladder head rotating cylinder (15) and the lower part of the support column (10); the digestion cylinder rotating motor The machine (14) is a well-known electric motor; the digestion cylinder disc rotating motor rotor (31) is the rotor of the digestion cylinder disc rotating motor (14), and has teeth on the surface, which can mesh with the teeth of the bite ring teeth (30); the bite ring teeth (30) are made of manganese steel and are annular in shape as a whole. The outer surface of the bite ring teeth (30) is smooth and welded to the inner surface of the lowest part of the support disc column ladder head rotating cylinder (15). The inner surface of the bite ring teeth (30) has a gear, and the teeth of the gear mesh with the teeth of the digestion cylinder disc rotating motor rotor (31); the height of the digestion cylinder disc rotating motor rotor (31) is 3-5 mm, and the height of the bite ring teeth (30) ring body is 5-8 mm; the upper surface of the outer ring body of the digestion cylinder disc (13) between two adjacent digestion cylinders (12) is provided with a gear. The digestion tube (12) is provided with grooves with an arcuate cross section, and these grooves and the inner cavity of the digestion tube (12) together form a material guide groove (11); the digestion tube (12) is made of polytetrafluoroethylene and is cylindrical. The digestion tube (12) is composed of a numbered area (21), a digestion tube wall cavity (22), a digestion tube wall (23), a digestion tube cavity (24), a tube lifting concave hole (25), and a digestion tube cover (26). The digestion tube wall (23) is a wall around and at the bottom of the digestion tube (12), and is a double-layer structure, consisting of an inner wall and an outer wall. The cavity between the inner wall and the outer wall is the digestion tube wall cavity (22); the height of the inner wall of the digestion tube wall (23) is lower than the height of the outer wall, so an inclined surface is formed on the upper edge of the digestion tube wall (23), and a pair of tube lifting concave holes (25) are symmetrically arranged on the inclined surface; the tube lifting concave holes (25) are two grooves arranged horizontally on the upper inclined surface of the digestion cylinder (12). The two grooves are located at the two ends of the cross section of the digestion cylinder (12). The opening of the lifting cylinder concave hole (25) faces inward and is between the inner wall and the upper end of the outer wall of the digestion cylinder wall (23). The bottom of the lifting cylinder concave hole (25) is blocked; the buckle (53) is made of spring steel, and the cross section is circular. The diameter of the circle is 1-3 mm. The buckle (53) consists of a horizontal axis, a grip axis, a vertical axis and a convex axis. There is only one horizontal axis, which is located at the top and the innermost part. Its length is determined by the distance between the openings of the two lifting cylinder concave holes (25), which is generally half the distance between the openings of the two lifting cylinder concave holes (25); the grip axis is a curved axis connected to the two ends of the horizontal axis for the convenience of human hand holding. shape or shape; the vertical axis is an axis in the vertical direction located at the lower end of the grip shaft, there are two of them, the lower end of the vertical axis is connected to the inner end of the convex axis, and the distance between the two vertical axes is equal to the distance between the openings of the two lifting tube recesses (25); the convex axis is the axis set in the two horizontal directions on the outermost side of the buckle (53); the digestion tube cavity (24) is a cavity surrounded by the digestion tube wall (23); the numbered area (21) is an area located in the center of the outer surface of the outer wall of the digestion tube wall (23), which is square, and different numbers are made in the numbered area (21); the digestion tube cover (26) is made of polytetrafluoroethylene and is in an arc shape. The distance between the highest point and the center of the plane circle where the bottom edge is located is 1-2 mm, and the bottom is 1-2 mm. The diameter of the plane circle where the edge is located is equal to the distance between the openings of the two lifting cylinder concave holes (25); the powder falling funnel (17) is made of plastic with a wall thickness of 0.2-0.5 mm. The upper opening of the powder falling funnel (17) is located at the bottom edge of the powder collecting funnel (18), is circular, has a diameter of 3-5 cm, and is set in the horizontal direction; the lower opening of the powder falling funnel (17) is free and elliptical, with a long diameter of 1-2 cm and a short diameter of 0.5-1 cm, and is set at an angle of 45° to the horizontal direction. The lower end opening of the powder falling funnel (17) faces the direction of rotation of the digestion cylinder disk (13), and the wall at the opening extends into the digestion cylinder cavity (24) by about 0.5-1 mm; the powder collecting funnel ( 18) is located below the grinding wheel (19), is made of plastic, and has a wall thickness of 0.2-0.5 mm. The powder collecting funnel (18) is divided into two parts, the upper part of the powder collecting funnel (18) is cylindrical, and the cylinder has no upper and lower bottoms, only walls around it. The height of the upper part of the powder collecting funnel (18) is 3-5 cm, and the lower edge of the cylindrical wall and the lower surface of the grinding wheel (19) are in the same plane; the lower part of the powder collecting funnel (18) is in the shape of an elephant trunk, and the upper edge of the lower part of the powder collecting funnel (18) is connected to the lower edge of the upper part, and then shrinks and becomes smaller, converging towards the upper opening of the powder falling funnel (17) and finally reaching the upper opening of the powder falling funnel (17). The lower part of the powder collecting funnel (18) is in the shape of an elephant trunk, and the upper edge of the lower part of the powder collecting funnel (18) is connected to the lower edge of the upper part, and then shrinks and becomes smaller, converging towards the upper opening of the powder falling funnel (17) and finally reaching the upper opening of the powder falling funnel (17). The wall of the upper portion is provided with an opening corresponding to the hoop tube (2) for the hoop tube (2) to extend into the powder collecting funnel (18); the grinding wheel (19) is a commercially available grinding wheel, cylindrical, with a diameter of 5-10 cm and a height of 5-20 mm, and a manganese steel shaft is provided in the center of the upper surface of the grinding wheel (19); the grinding wheel motor (20) is a commercially available motor, fixed to the inner surface of the top wall of the sample grinding preparation device; the upper end of the nitric acid digestion bottle (36) is fixed to the inner surface of the top wall of the sample grinding preparation device, and the lower end of the nitric acid digestion bottle (36) is free, and the force claw (49) of the gravity switch (50) at the lower end of the nitric acid digestion bottle (36) extends into the digestion cylinder cavity (24) by about 0.5-1 mm, the nitric acid digestion bottle (36) is composed of a bottle body (54), a nitric acid digestion solution (39), a fixed switch (42), a flow nitric acid digestion tube (43) and a gravity switch (50), the bottle body (54) includes a nitric acid digestion bottle wall (37), a nitric acid digestion bottle cavity (38), a nitric acid digestion bottleneck (40), and a nitric acid digestion bottle mouth (41), the nitric acid digestion bottle wall (37) is the outer wall of the bottle body (54), is glassy, and has a thickness of 1-2 mm; the nitric acid digestion bottle cavity (38) is the nitric acid digestion bottle wall (37) The cavity surrounded by the bottle wall (37); the nitric acid digestion bottle neck (40) is the part where the lower part of the bottle body (54) becomes thinner until the nitric acid digestion bottle mouth (41); the nitric acid digestion bottle mouth (41) is the opening at the lower end of the bottle body (54) for releasing the nitric acid digestion solution (39), the inner cavity diameter is 1-1.5 cm, and the lower end opening of the bottle body (54) is blocked by the bottle stopper; the fixed switch (42) is a valve set on the bottle stopper, and the size of the opening of the fixed switch (42) determines the nitric acid digestion solution (39). 9) the speed of the nitric acid digestion bottle mouth (41); the nitric acid digestion solution (39) is a digestion solution that can digest and convert heavy metals in bone powder into a single valence state; the nitric acid digestion tube (43) is made of glass, the upper end of the nitric acid digestion tube (43) is controlled to open and close by a fixed switch (42), the lower end of the nitric acid digestion tube (43) is an oblique opening, and a rubber pad is provided at the opening; the gravity switch (50) is made of spring steel, and is composed of a tube holding ring (44), an arm shaft (45), a force guide claw (46), The pipe-blocking gravity ball (47), the force-bearing claw arm (48), and the force-bearing claw (49) are composed of a pipe-holding ring (44) which is a ring pipe surrounding the nitric acid digestion pipe (43). The overall shape is a central drum with two pointed ends. The nitric acid digestion pipe (43) is located in the center of the central drum of the pipe-holding ring (44). One end of the pipe-holding ring (44) is connected to the arm rotating shaft (45), and the other end is connected to the upper end of the force-bearing claw (46). The arm rotating shaft (45) is the rotating shaft for fixing the pipe-holding ring (44) and the force-bearing claw arm (48). The horizontal bar on the top is the rotating shaft in the through-holes on both sides of one end of the tube holding ring (44), and the vertical bar pointing downward is the supporting shaft extending inward from the center of one end of the tube holding ring (44), and the inner end of the vertical bar is fixed on the outer surface of the nitric acid digestion tube (43); the force-guiding claw (46) is arc-shaped, one end of which is connected to one end of the tube holding ring (44) and the other end is connected to the pipe-blocking gravity ball (47); the force-bearing claw arm (48) is the connecting arm between the tube holding ring (44) and the force-bearing claw (49), and is arc-shaped; the force-bearing claw (49) is a thin spring steel sheet.
2. The device for rapidly determining heavy metal content in animal bone samples using flame color reaction according to claim 1, characterized in that: The free ends of the inner side wall (33) and the outer side wall (34) of the hoop bone tube partially overlap and are close to each other, but are not connected together. Therefore, after the bone sample (1) is placed in the hoop bone tube cavity (35), the diameter of the hoop bone tube cavity (35) can change with the size of the diameter of the bone sample (1). If the diameter of the bone sample (1) is large, the diameter of the hoop bone tube cavity (35) will be stretched and become larger. If the diameter of the bone sample (1) is small, the diameter of the hoop bone tube cavity (35) will return to a smaller size due to the elasticity of the spring steel. Once the bone sample (1) is placed in the hoop bone tube cavity (35), the diameter of the hoop bone tube cavity (35) will change with the size of the diameter of the bone sample (1). The bone sample (1) is placed in the hoop bone tube cavity (35), and the bone sample (1) is fixed. Subsequently, the diameter of the hoop bone tube cavity (35) cannot be changed. Therefore, two upper and lower hoop bone tube hoops (3) are provided on the hoop bone tube (2); the structure of the hoop bone tube hoops (3) is the same as that of the commercially available adjustable iron hoops, that is, the iron hoop is annular, and the inner surface of the ring body relative to the adjustment buckle is welded to the other surface of the fixed tube column (32) relative to the base of the hoop bone tube inner wall (33) and the hoop bone tube outer wall (34). The two parts of the adjustment buckle are Under the action of the fixed top buckle, it can move relatively. Once it moves to tightly clamp the hoop bone tube (2), it stops and is fixed together, and no relative movement occurs, thereby firmly fixing the bone sample (1) in the hoop bone tube cavity (35) without tilting or expanding. At most, under the action of the top bone spring (5) in the support bone tube (4), the bone sample (1) can extend upward from the hoop bone tube cavity (35), and the upper end of the bone sample (1) extends to the lower surface of the grinding wheel (19). As the upper end of the bone sample (1) is ground by the grinding wheel (19), The bone sample (1) is ground into powder and becomes shorter. The bone sample (1) is continuously pushed upward by the top bone spring (5) until it is almost worn out and pushed out of the hoop bone cylinder cavity (35) by the top bone spring (5). The ground bone sample (1) is thrown out under the action of centrifugal force and gravity, and falls into the powder collecting funnel (18) and the powder dropping funnel (17) to be collected. It falls into the guide trough (11) or the digestion cylinder (12) along the powder dropping funnel (17). The rotation speed of the digestion cylinder disc (13) is controlled so that the amount of bone powder falling into each digestion cylinder (12) is 0.1 gram; during the rotation of the digestion tube (12), when a digestion tube (12) is transferred to the bottom of the nitric acid digestion bottle (36), 5 ml of nitric acid digestion solution (39) can be injected into the digestion tube (12), and the bone powder can be digested by the nitric acid digestion solution (39) in the digestion tube (12), and the metal elements in the sample are converted into a single valence state. When all the digestion tubes (12) around the periphery of a digestion tube disk (13) are injected with nitric acid digestion solution (39), the digestion tubes (12) with numbers on the tube wall are taken out in turn, and then the digestion tube cover (26) of the digestion tube (12) is covered, and the digestion tube (12) is placed in a stainless steel reactor, placed in an oven, and heated at a controlled temperature of 190°C for about 10 hours to make the powdered bone sample ( 1) Completely dissolve under the action of nitric acid digestion solution (39), and each element in the sample is released into the nitric acid digestion solution (39); then, cool the digestion cylinder (12), take it out of the reactor, filter the nitric acid digestion solution (39) in the digestion cylinder (12) using a filter membrane, collect the filtrate in a 50 ml flat-bottom plastic centrifuge tube, and dilute it to the 50 ml mark with deionized water to obtain a test solution within the linear range of the mass spectrometer (51), turn on the mass spectrometer (51) to detect the sample, and quickly obtain the specific content of each heavy metal element in the bone sample (1); the mass spectrometer (51) is a commercially available inductively coupled plasma mass spectrometer that can quickly and quantitatively determine the heavy metals in the bone sample.
3. The device for rapidly determining heavy metal content in animal bone samples using flame color reaction according to claim 1, characterized in that: The process of grinding the bone sample (1) into bone powder and collecting the bone powder after it is placed is as follows: after the bone sample (1) is placed in the bone hoop tube (2), the bone support tube (4) is rotated and pushed into the depression in front of the retaining tube block (6). At the same time, the bone sample (1) is pressed downward so that the bone sample (1) is located between the top bone spring (5) and the grinding wheel (19), so that when the grinding wheel (19) rotates, the bone sample (1) can be ground into bone powder little by little, and under the action of the centrifugal force generated during the rotation, the bone sample (1) falls into the powder collecting funnel (18) and the powder dropping funnel (17) and is collected.
4. The device for rapidly determining heavy metal content in animal bone samples using flame color reaction according to claim 1, characterized in that: The specific method for the bone powder in the powder dropping funnel (17) to fall onto the guide trough (11) is as follows: since the plastic wall thickness at the opening of the powder dropping funnel (17) is 0.2-0.5 mm, which is relatively thin and elastic, during the rotation of the digestion cylinder disc (13), the bone powder falling from the guide trough (11) between two adjacent digestion cylinders (12) can be scraped into the digestion cylinder (12) like a scraper. When the powder dropping funnel (17) is rotated to the upper end of the digestion cylinder cavity (24), the elasticity of the opening at the lower end of the powder dropping funnel (17) can also form an oscillation for the powder dropping funnel (17), thereby better shaking off the bone powder that may remain in the powder dropping funnel (17).
5. The device for rapidly determining heavy metal content in animal bone samples using flame color reaction according to claim 1, characterized in that: The specific method of the nitric acid digestion bottle (36) controlling the nitric acid digestion solution (39) to flow out of the nitric acid digestion tube (43) is as follows: when the digestion cylinder disc (13) rotates and the force claw (49) is above the material guide groove (11), since the force claw (49) is made of spring steel and has elasticity, the force claw (49) can slide along the material guide groove (11), but the force between the force claw (49) and the material guide groove (11) pushes the force claw (49) in the opposite direction of the rotation of the digestion cylinder disc (13), forming a thrust, and then the pipe blocking gravity ball (47) is tightly pressed against the lower end opening of the nitric acid digestion tube (43), blocking the opening, and the nitric acid digestion solution ( 39) will not flow out; but when the digestion cylinder disc (13) rotates and the force claw (49) is above the digestion cylinder (12), the force claw (49) loses the thrust, and under the action of the gravity of the blocking gravity ball (47) itself, the blocking gravity ball (47) leaves the lower end opening of the flow nitric acid digestion tube (43), and the nitric acid digestion solution (39) can flow downstream of the nitric acid digestion tube (43) into the digestion cylinder (12). According to actual needs, the rotation speed of the fixed switch (42) and the digestion cylinder disc (13) is adjusted to fix the amount of nitric acid digestion solution (39) flowing into the digestion cylinder (12) at a set amount to ensure the accuracy of the calculated data.
Citation Information
Patent Citations
Method for detecting components of hospital sewage
CN104459073A
Teaching method for simulated chemistry experiment for displaying flame reaction and device
CN108766084A
Energy-saving environment-friendly chemical reaction flame reaction device and application method thereof
CN108877441A
Agricultural product pesticide residue detection method
CN109142322A
Preparation and application of integral torch combustion catalyst
CN113996292A