A heating constant temperature device capable of automatic sample feeding and ash discharge

Abstract

The invention discloses a heating constant temperature device capable of automatic sampling and ash discharge, comprising a furnace body and a sampler, wherein a heating component and a quartz sample tube are arranged in the furnace body, the sampler comprises a crucible, a ceramic column and a sampler base, wherein the crucible is arranged at the top of the ceramic column, the ceramic column is arranged in the inner cavity of the sampler base, the crucible can accommodate a sample, the sampler base is arranged at the bottom of the furnace body, the sampler base is connected with a first driver, the first driver can drive the sampler base to reciprocate along a vertical direction, the sampler base can abut against the quartz sample tube, the ceramic column is connected with a second driver, the second driver can drive the ceramic column to reciprocate along a vertical direction, the ceramic column can extend into the quartz sample tube; the furnace body is provided with an analysis gas outlet and a carrier gas inlet, both of which are connected with the quartz sample tube, a gap is provided between the ceramic column and the inner wall of the sampler base to form an ash discharge port, and the ash discharge port is connected with the quartz sample tube.

Description

Technical Field

[0001] The invention relates to the technical field of solid inorganic material gas element analysis and testing, in particular to a heating constant temperature device capable of automatic sample feeding and ash discharge. Background Art

[0002] When testing and analyzing the content of certain elements in inorganic solid materials (including metals and non-metallic materials), it is usually necessary to decompose or oxidize them into gas components by heating, and then test the generated gas content. The traditional silicon carbon rod tube furnace not only has a slow heating and cooling speed, but also cannot realize different temperature control methods such as segmentation, slope, and step required in practical applications. When the traditional high-temperature tube furnace is used to test and analyze sample gas extraction, because the furnace needs to be in a high temperature state all the time, the gas elements will be volatilized instantly when the sample is injected, resulting in poor stability of the test data. Some also use high-frequency furnaces. The defect of high-frequency furnaces is that the decomposition of non-metallic samples is very unstable. Arc furnaces and electrode pulse furnaces also have the defects of being unable to accurately maintain a constant temperature and small injection volume (less than 1g). Moreover, the existing equipment currently all first injects the sample and then heats it, which makes the existing equipment unable to be used for accurate testing of the release rate at a specific temperature. When the above equipment is used for analysis and testing by thermal decomposition, these defects will have a direct impact on the test data. Secondly, most traditional silicon carbon rod tube furnaces use an open sample chamber. The negative pressure analysis gas is pumped into the infrared detector through a sampling pump to measure the content of the gas to be tested, which makes the analysis time long and the signal peak short, thereby increasing the impact of the noise signal background on the test results and reducing the test accuracy.

[0003] Therefore, how to change the current situation of poor testing accuracy caused by the open sample chamber of the heating device in the prior art has become an urgent problem to be solved by those skilled in the art. Summary of the invention

[0004] The purpose of the present invention is to provide a heating constant temperature device capable of automatic sample feeding and ash discharge, so as to solve the problems existing in the above-mentioned prior art, improve the working efficiency of the heating device, and improve the accuracy of subsequent tests.

[0005] To achieve the above-mentioned purpose, the present invention provides the following scheme: The present invention provides a heating constant temperature device capable of automatic sampling and ash discharge, comprising a furnace body and a sampler, wherein a heating component and a quartz sample tube are arranged in the furnace body, wherein the sampler comprises a crucible, a ceramic column and a sampler base, wherein the crucible is arranged at the top of the ceramic column, wherein the ceramic column is arranged in the inner cavity of the sampler base, wherein the crucible can accommodate a sample, wherein the sampler base is arranged at the bottom of the furnace body, wherein the sampler base is connected to a first driver, wherein the first driver can drive the sampler base to reciprocate in a vertical direction, wherein the sampler base can abut against the quartz sample tube, wherein the ceramic column is connected to a second driver, wherein the second driver can drive the ceramic column to reciprocate in a vertical direction, wherein the ceramic column can extend into the quartz sample tube; wherein the furnace body has an analysis gas outlet and a carrier gas inlet, wherein the analysis gas outlet and the carrier gas inlet are both connected to the quartz sample tube, wherein a gap is provided between the ceramic column and the inner wall of the sampler base to form an ash discharge port, wherein the ash discharge port is connected to the quartz sample tube.

[0006] Preferably, the heating assembly includes an infrared heating element and a reflector, the infrared heating element is arranged between the inner wall of the furnace body and the quartz sample tube, the reflector is arranged on the inner wall of the furnace body, and the reflector can reflect the infrared light emitted by the infrared heating element into the quartz sample tube.

[0007] Preferably, the quartz sample tube is coaxially arranged with the furnace body, the number of the infrared heating elements is four, and the four infrared heating elements are evenly distributed around the axis of the quartz sample tube; a temperature sensor is arranged on the side wall of the furnace body, and the probe of the temperature sensor is located between the infrared heating element and the quartz sample tube.

[0008] Preferably, the heating constant temperature device capable of automatic sampling and ash discharge also includes a fixed frame and a fixed plate, the furnace body and the first driver are arranged on the fixed frame, the first driver is connected to the fixed plate, the injector and the second driver are arranged on the fixed plate, the injector is slidably connected to the fixed frame, and the ceramic column is slidably connected to the fixed plate.

[0009] Preferably, the number of the first drivers is two, and the two first drivers are arranged on opposite sides of the furnace body, and the first driver and the second driver are both cylinders.

[0010] Preferably, a furnace head is connected to the top of the furnace body, and the analysis gas outlet and the carrier gas inlet are both arranged on the furnace head.

[0011] Preferably, the furnace head and the side wall of the furnace body are provided with built-in cooling circulation pipes, and the cooling circulation pipes can be communicated with an external cooling medium.

[0012] Preferably, a sealing element is provided between the injection base and the quartz sample tube.

[0013] Preferably, the crucible and the ceramic column are detachably connected.

[0014] Compared with the prior art, the present invention has achieved the following technical effects: the heating constant temperature device capable of automatic sampling and ash discharge of the present invention comprises a furnace body and a sample injector, a heating component and a quartz sample tube are arranged in the furnace body, the sample injector comprises a crucible, a ceramic column and a sample injection base, the crucible is arranged at the top of the ceramic column, the ceramic column is arranged in the inner cavity of the sample injection base, the crucible can accommodate the sample, the sample injection base is arranged at the bottom of the furnace body, the sample injection base is connected to a first driver, the first driver can drive the sample injection base to reciprocate in a vertical direction, the sample injection base can abut against the quartz sample tube, the ceramic column is connected to a second driver, the second driver can drive the ceramic column to reciprocate in a vertical direction, and the ceramic column can extend into the quartz sample tube; the furnace body has an analysis gas outlet and a carrier gas inlet, the analysis gas outlet and the carrier gas inlet are both connected to the quartz sample tube, a gap is provided between the ceramic column and the inner wall of the sample injection base to form an ash discharge port, and the ash discharge port is connected to the quartz sample tube. When the heating constant temperature device capable of automatic sampling and ash discharge of the present invention is working, the first driver drives the sample injector to move in the direction away from the furnace body, so that the crucible is located at the top of the ceramic column. When the analysis starts, the first driver drives the sample injector base to move in the direction of the furnace body, the sample base abuts against the quartz sample tube, and the external gas source simultaneously introduces carrier gas into the quartz sample tube through the carrier gas inlet and the ash discharge port, and the heating component is heated. When the temperature in the furnace body is stabilized at a set target value, the second driver drives the ceramic column to rise, and the sample in the crucible is sent into the quartz sample tube, which is located at the center line of the furnace body, and is heated. The released gas to be tested and the carrier gas are sent to the instrument for detection through the analysis gas outlet; after the sample analysis is completed, the second driver drives the ceramic column and the crucible to descend, the sample is returned, the external gas source blows air into the furnace body through the analysis gas outlet to increase the pressure in the furnace body, so that the dust is discharged from the ash discharge port, and the first driver drives the sample injector to move in the direction away from the furnace body, and the sample is taken out. The heating constant temperature device capable of automatic sampling and ash discharge of the present invention seals the quartz sample tube before sampling, so that negative pressure becomes positive pressure and the airflow is stable. Before sampling, a reference signal is firstly collected under the carrier gas environment. After the temperature in the furnace body is stabilized, the sampler sends the sample into the heating zone in the furnace body in a closed environment, which greatly reduces the airflow fluctuation caused by sampling in a negative pressure state in the prior art and generates signal fluctuation. The integration efficiency of the positive pressure gas path can be increased by 10 times, so that the signal integration peak is more perfect and the test accuracy is higher. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative labor.

[0016] Figure 1 It is a structural schematic diagram of a heating thermostatic device capable of automatic sample feeding and ash discharge of the present invention;

[0017] Figure 2 It is a schematic cross-sectional structure diagram of a heating thermostatic device capable of automatic sample injection and ash discharge according to the present invention;

[0018] Figure 3 It is a schematic cross-sectional structure diagram of a crucible of a heating and thermostatic device capable of automatic sample feeding and ash discharge according to the present invention;

[0019] Among them, 1 is the furnace body, 2 is the injector, 3 is the heating component, 4 is the quartz sample tube, 5 is the crucible, 6 is the ceramic column, 7 is the injection base, 8 is the first drive, 9 is the second drive, 10 is the analysis gas outlet, 11 is the carrier gas inlet, 12 is the ash discharge port, 13 is the temperature sensor, 14 is the fixed frame, 15 is the fixed plate, and 16 is the furnace head. DETAILED DESCRIPTION

[0020] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0021] The purpose of the present invention is to provide a heating constant temperature device capable of automatic sample feeding and ash discharge, so as to solve the problems existing in the above-mentioned prior art, improve the working efficiency of the heating device, and improve the accuracy of subsequent tests.

[0022] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the present invention is further described in detail below with reference to the accompanying drawings and specific embodiments.

[0023] Please refer to Figure 1-3 ,in, Figure 1 It is a structural schematic diagram of the heating thermostat device capable of automatic sample feeding and ash discharge of the present invention, Figure 2 It is a schematic cross-sectional structure diagram of the heating thermostat capable of automatic sample feeding and ash discharge of the present invention. Figure 3 The cross-sectional structure diagram of the crucible of the heating constant temperature device capable of automatic sample feeding and ash discharge of the present invention.

[0024] The present invention provides a heating constant temperature device capable of automatic sample injection and ash discharge, comprising a furnace body 1 and a sample injector 2, wherein a heating component 3 and a quartz sample tube 4 are arranged in the furnace body 1, and the sample injector 2 comprises a crucible 5, a ceramic column 6 and a sample injection base 7, wherein the crucible 5 is arranged on the top of the ceramic column 6, and the ceramic column 6 is arranged in the inner cavity of the sample injection base 7, and the crucible 5 can accommodate a sample, and the sample injection base 7 is arranged at the bottom of the furnace body 1, and the sample injection base 7 is connected to a first driver 8, and the first driver 8 can drive the sample injection base 7 to move in a vertical direction. Reciprocating motion, the sampling base 7 can abut against the quartz sample tube 4, the ceramic column 6 is connected to the second driver 9, the second driver 9 can drive the ceramic column 6 to reciprocate along the vertical direction, and the ceramic column 6 can extend into the quartz sample tube 4; the furnace body 1 has an analysis gas outlet 10 and a carrier gas inlet 11, the analysis gas outlet 10 and the carrier gas inlet 11 are both connected to the quartz sample tube 4, there is a gap between the ceramic column 6 and the inner wall of the sampling base 7 and an ash discharge port 12 is formed, and the ash discharge port 12 is connected to the quartz sample tube 4.

[0025] When the heating thermostat capable of automatic sample injection and ash discharge of the present invention is working, the first driver 8 drives the sample injector 2 to move in a direction away from the furnace body 1, so that the crucible 5 is located at the top of the ceramic column 6. When the analysis starts, the first driver 8 drives the sample injection base 7 to move in the direction of the furnace body 1, and the sample base abuts against the quartz sample tube 4. The external gas source simultaneously introduces carrier gas into the quartz sample tube 4 through the carrier gas inlet 11 and the ash discharge port 12, and the heating component 3 is heated. When the temperature in the furnace body 1 is stabilized at the set target value, the second driver 9 The ceramic column 6 is driven to rise, and the sample in the crucible 5 is sent into the quartz sample tube 4, which is located at the center line of the furnace body 1, and is heated. The released gas to be tested and the carrier gas are sent to the instrument for detection through the analysis gas outlet 10; after the sample analysis is completed, the second driver 9 drives the ceramic column 6 and the crucible 5 to descend, and the sample is returned. The external gas source blows into the furnace body 1 through the analysis gas outlet 10 to increase the pressure in the furnace body 1, so that the dust is discharged from the ash discharge port 12, and the first driver 8 drives the sampler 2 to move in the direction away from the furnace body 1, and the sample is taken out. The ceramic column 6 is made of ceramic material, which is resistant to high temperature and has a stable structure. The heating constant temperature device capable of automatic sampling and ash discharge of the present invention seals the quartz sample tube 4 before sampling, so that the negative pressure becomes positive pressure and the airflow is stable. Before sampling, a reference signal is first collected under the carrier gas environment. After the temperature in the furnace body 1 is stabilized, the sample injector 2 delivers the sample into the heating zone in the furnace body 1 in a closed environment, which greatly reduces the airflow fluctuation caused by sampling in a negative pressure state in the prior art and generates signal fluctuations. The positive pressure gas path integration efficiency can be increased by 10 times, making the signal integration peak more perfect and the test accuracy higher.

[0026] Among them, the heating component 3 includes an infrared heating element and a reflector. The infrared heating element is arranged between the inner wall of the furnace body 1 and the quartz sample tube 4. The reflector is arranged on the inner wall of the furnace body 1. The reflector can reflect the infrared light emitted by the infrared heating element into the quartz sample tube 4 to improve the heating efficiency. The efficiency is high and the heating rate is fast. The temperature can rise by more than 1000°C in 1 minute. The curved surface shape of the reflector is determined according to the actual production conditions. After multiple reflections, the infrared light is focused on the sample in the quartz sample tube 4. The required temperature is set so that the heated substance is in a high-temperature state and some atoms escape and decompose, or all are melted. The size of the infrared focusing heating zone is huge, and a maximum of more than 200g of various materials can be heated at one time. It is suitable for various powders and solid non-metallic raw materials. The temperature inside the furnace body 1 is set and accurately controlled through a software program. It can instantly rise to the set temperature during heating, and the temperature control accuracy can reach 0.1°C. Therefore, it is very convenient to realize various temperature control modes such as step, linear, or stable temperature. The device for thermally extracting gas components during elemental composition testing in materials is very meaningful for studying the release degree of atoms and molecules at different temperatures.

[0027] In this specific embodiment, the quartz sample tube 4 is coaxially arranged with the furnace body 1, and the number of infrared heating elements is four. The four infrared heating elements are evenly distributed around the axis of the quartz sample tube 4 to improve the heating efficiency and uniformity; a temperature sensor 13 is arranged on the side wall of the furnace body 1, and the probe of the temperature sensor 13 is located between the infrared heating element and the quartz sample tube 4. The temperature sensor 13 is arranged to monitor the temperature inside the furnace body 1.

[0028] Specifically, the heating constant temperature device capable of automatic sampling and ash discharge also includes a fixed frame 14 and a fixed plate 15, the furnace body 1 and the first driver 8 are arranged on the fixed frame 14, the first driver 8 is connected to the fixed plate 15, the sampler 2 and the second driver 9 are arranged on the fixed plate 15, the sampler 2 is slidably connected to the fixed frame 14, the ceramic column 6 is slidably connected to the fixed plate 15, the fixed frame 14 and the fixed plate 15 provide an installation basis for the furnace body 1 and the sampler 2, thereby improving the overall stability of the device.

[0029] In addition, there are two first drivers 8, which are arranged on opposite sides of the furnace body 1. The number of first drivers 8 is two, which improves the force uniformity and movement stability of the fixed plate 15. The first driver 8 and the second driver 9 are both cylinders, which have stable movement and a wide range of sources.

[0030] More specifically, the top of the furnace body 1 is connected with a furnace head 16, and the analysis gas outlet 10 and the carrier gas inlet 11 are both arranged on the furnace head 16. It should be noted that a metal dust filter is arranged between the analysis gas outlet 10 and the quartz sample tube 4, and the released gas to be tested and the carrier gas are discharged from the analysis gas outlet 10 after passing through the metal dust filter, and sent to the instrument detector to measure the content; after the analysis is completed, the pressurized back-blowing carrier gas still enters from the analysis gas outlet 10, back-blowing the metal dust filter to discharge dust, and the dust is discharged from the ash discharge port 12. In order to facilitate collection, the ash discharge port 12 can be connected to an external dust collection box.

[0031] Furthermore, the furnace head 16 and the side wall of the furnace body 1 are built with a cooling circulation pipeline, and the cooling circulation pipeline can be connected to an external cooling medium. The external cooling medium is passed into the cooling circulation pipeline, which can achieve high-speed heat dissipation of the furnace body 1, avoiding high-temperature damage to the furnace body 1 and scalding. At the same time, it can also make the furnace body 1 cool quickly, shorten the shutdown cooling time, and the water discharged after heat dissipation can also be used for water-heating heaters, and the cold end water can be reused to cool the furnace body 1, which is energy-saving and environmentally friendly.

[0032] In order to improve the sealing performance when the injection base 7 and the quartz sample tube 4 are in contact, a sealing element is arranged between the injection base 7 and the quartz sample tube 4. The sealing element is made of silicone rubber material to extend the service life of the sealing element.

[0033] Furthermore, the crucible 5 and the ceramic column 6 are detachably connected. In order to improve the stability of the crucible 5 when the ceramic column 6 moves, in other specific embodiments of the present invention, the crucible 5 is plugged into the ceramic column 6 to prevent the crucible 5 from slipping out of position.

[0034] When the heating thermostatic device capable of automatic sampling and ash discharge of the present invention is working, the first driver 8 drives the sampler 2 to move in a direction away from the furnace body 1, so that the crucible 5 is located at the top of the ceramic column 6. When the analysis starts, the first driver 8 drives the sampler base 7 to move in the direction of the furnace body 1, the sample base is in contact with the quartz sample tube 4, and the external gas source simultaneously introduces carrier gas into the quartz sample tube 4 through the carrier gas inlet 11 and the ash discharge port 12, and the heating component 3 is heated. When the temperature in the furnace body 1 is stabilized at a set target value, the second driver 9 drives the ceramic column 6 to rise, and the sample in the crucible 5 is sent into the quartz sample tube 4, which is located at the center line position of the furnace body 1, and heated. The gas to be measured and the carrier gas are output from the analysis gas outlet 10; after the sample analysis is completed, the second driver 9 drives the ceramic column 6 and the crucible 5 to descend, the sample is returned, and the external gas source blows into the furnace body 1 through the analysis gas outlet 10 to increase the pressure in the furnace body 1, so that the dust is discharged from the ash discharge port 12, and the first driver 8 drives the sampler 2 to move in a direction away from the furnace body 1, and the sample is taken out. The device of the present invention is also connected to an external cooling medium, and the external cooling medium is passed into the cooling circulation pipeline, which can achieve high-speed heat dissipation of the furnace body 1 and avoid high-temperature damage to the furnace body 1 and scalding.

[0035] The present invention uses specific examples to illustrate the principles and implementation methods of the present invention. The above examples are only used to help understand the method and core ideas of the present invention. At the same time, for those skilled in the art, according to the ideas of the present invention, there will be changes in the specific implementation methods and application scope. In summary, the content of this specification should not be understood as limiting the present invention.

Claims

1. A heating constant temperature device capable of automatic sample feeding and ash discharge, characterized in that: The invention comprises a furnace body and an injector, wherein a heating component and a quartz sample tube are arranged in the furnace body, and the injector comprises a crucible, a ceramic column and an injector base, wherein the crucible is arranged at the top of the ceramic column, the ceramic column is arranged in the inner cavity of the injector base, the crucible can accommodate a sample, the injector base is arranged at the bottom of the furnace body, the injector base is connected with a first driver, the first driver can drive the injector base to reciprocate in a vertical direction, the injector base can abut against the quartz sample tube, the ceramic column is connected with a second driver, the second driver can drive the ceramic column to reciprocate in a vertical direction, and the ceramic column can extend into the quartz sample tube; the furnace body has an analysis gas outlet and a carrier gas inlet, the analysis gas outlet and the carrier gas inlet are both connected with the quartz sample tube, a gap is provided between the ceramic column and the inner wall of the injector base to form an ash discharge port, and the ash discharge port is connected with the quartz sample tube; a sealing element is arranged between the injector base and the quartz sample tube.

2. The heating constant temperature device capable of automatic sample feeding and ash discharge according to claim 1 is characterized in that: The heating assembly includes an infrared heating element and a reflector. The infrared heating element is arranged between the inner wall of the furnace body and the quartz sample tube. The reflector is arranged on the inner wall of the furnace body. The reflector can reflect the infrared light emitted by the infrared heating element into the quartz sample tube.

3. The heating constant temperature device capable of automatic sample feeding and ash discharge according to claim 2 is characterized in that: The quartz sample tube is coaxially arranged with the furnace body, and the number of the infrared heating elements is four, and the four infrared heating elements are evenly distributed around the axis of the quartz sample tube in a circumferential shape; a temperature sensor is arranged on the side wall of the furnace body, and the probe of the temperature sensor is located between the infrared heating element and the quartz sample tube.

4. The heating constant temperature device capable of automatic sample feeding and ash discharge according to claim 1 is characterized in that: It also includes a fixed frame and a fixed plate, the furnace body and the first driver are arranged on the fixed frame, the first driver is connected to the fixed plate, the injector and the second driver are arranged on the fixed plate, the injector is slidably connected to the fixed frame, and the ceramic column is slidably connected to the fixed plate.

5. The heating constant temperature device capable of automatic sample feeding and ash discharge according to claim 4 is characterized in that: The number of the first drivers is two, and the two first drivers are arranged on two opposite sides of the furnace body. The first driver and the second driver are both cylinders.

6. The heating constant temperature device capable of automatic sample feeding and ash discharge according to claim 1 is characterized in that: A furnace head is connected to the top of the furnace body, and the analysis gas outlet and the carrier gas inlet are both arranged on the furnace head.

7. The heating constant temperature device capable of automatic sample feeding and ash discharge according to claim 6 is characterized in that: The furnace head and the side wall of the furnace body are provided with built-in cooling circulation pipelines, and the cooling circulation pipelines can be communicated with an external cooling medium.

8. The heating constant temperature device capable of automatic sample feeding and ash discharge according to claim 1 is characterized in that: The crucible is detachably connected to the ceramic column.

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