CN213305795U - Hydride generator heating control device - Google Patents
Hydride generator heating control device Download PDFInfo
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- CN213305795U CN213305795U CN202021745066.0U CN202021745066U CN213305795U CN 213305795 U CN213305795 U CN 213305795U CN 202021745066 U CN202021745066 U CN 202021745066U CN 213305795 U CN213305795 U CN 213305795U
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Abstract
The utility model provides a heating control device of a hydride generator, which comprises a T-shaped reaction tube and a heating temperature control component; the heating temperature control assembly comprises a clamping heat conduction device, a temperature measurement sensor and a heat dissipation device connected with the clamping heat conduction device. The utility model can realize controllable heating and cooling of the T-shaped reaction tube, thereby enabling the temperature in the T-shaped reaction tube to be matched with the ideal atomization temperature of the element to be detected in the detection process; and, increase the heated area through centre gripping heat conduction device, improve the degree of consistency of being heated, improved the repeatability that leads to data stability and test value, brought the convenience for using the hydride generator to carry out elemental analysis.
Description
Technical Field
The utility model belongs to the technical field of the hydride generator, especially, relate to a hydride generator heating control device.
Background
Hydride generators are used for analysis of some elements which are easy to generate hydrides and difficult to directly atomize. The principle is that covalent hydride is formed by a sample to be analyzed under the action of a strong reducing agent, the covalent hydride is introduced into a reaction tube, and the hydride is decomposed into gaseous atoms by controlling conditions (such as temperature) so as to realize atomic absorption measurement. The hydride generator based on flame heating enables a light path to pass through the reaction tube by adjusting the position of the bracket, and the atomic absorption cell is heated by flame to decompose and measure hydride.
However, this assay has two drawbacks: firstly, an atomization mode of heating a quartz tube by utilizing flame generated by burning combustible gas (such as acetylene) has the atomization temperature which is always and only in a higher state (1700-; secondly, when the flame generated by the combustible gas heats the quartz tube through the combustion seam, the lower end part of the quartz tube can only be heated, and the heating area can not cover the whole tube body, so that the lower end of the quartz tube is in a high-temperature state based on the flame, and the upper end of the quartz tube can not contact the flame, so that the upper temperature and the lower temperature are inconsistent, the heating is not uniform, the atomization rate of hydride is influenced, even a valence state effect is generated, and the measurement result is influenced.
In conclusion, in the experimental process of the existing hydride generator based on flame heating, on one hand, the atomization reaction in the quartz tube is unstable due to the overhigh heating temperature; on the other hand, the quartz tube has a limited flame heating area, which causes uneven heating, and thus the accuracy and stability of the measured data are greatly affected based on the two defects.
SUMMERY OF THE UTILITY MODEL
Aiming at the defects in the prior art, the hydride generator heating control device provided by the utility model can realize controllable heating and cooling of the T-shaped reaction tube on one hand; on the other hand, the heat conducting device is clamped to coat the projection reaction tube, so that the heating area is enlarged, the heating uniformity is improved, the stability of data detection and the repeatability of test values are improved, and convenience is brought to element analysis by using the hydride generator.
In order to achieve the above purpose, the technical scheme of the utility model is that: the hydride generator heating control device is applied to a hydride generator based on flame heating, and comprises: the T-shaped reaction tube and the heating temperature control assembly; the heating temperature control assembly comprises a clamping heat conduction device, a temperature measurement sensor and a heat dissipation device connected with the clamping heat conduction device; the T-shaped reaction tube comprises a projection reaction tube and a sample inlet tube vertically connected with the projection reaction tube; the clamping heat conduction device can be detachably connected with the T-shaped reaction tube and can clamp and coat the projection reaction tube of the T-shaped reaction tube; the temperature sensor is arranged on the clamping heat conduction device and can be contacted with the projection reaction tube when the T-shaped reaction tube is clamped and fixed; the heat dissipation device comprises a heat dissipation body connected with the clamping heat conduction device and a refrigeration assembly arranged on the heat dissipation body.
Preferably, the heat dissipation body comprises a plurality of heat dissipation single sheets; the heat dissipation single sheets are arranged in parallel, and the heat dissipation single sheets are vertical to the surface of one side, facing the heat dissipation single sheets, of the clamping heat conduction device; the refrigerating assembly comprises a plurality of refrigerating units arranged on the radiating single sheet of the radiating body; the refrigerating unit comprises a base radiating fin connected with the radiating single sheet and a refrigerating fan arranged on the base radiating fin. Preferably, the heating temperature control assembly further comprises: the clamping heat conduction device is provided with a heater and a temperature control device, the heater is arranged on the clamping heat conduction device and used for heating the T-shaped reaction tube, and the temperature control device is electrically connected with the heater and the temperature measurement sensor.
Preferably, the clamping heat conducting device comprises a base plate and a clamping plate; the base plate is elastically hinged with the clamping plate through a pin shaft; the clamping plate comprises a clamping part and a pressing part connected with the clamping part on the basis of the pin shaft; an included angle between the pressing part and the clamping part, which is far away from one end of the base plate, is less than 180 degrees; an accommodating cavity for accommodating the projection reaction tube is enclosed between the clamping part and the base plate, and clamping force for clamping the clamping part and the base plate in opposite directions is generated through the elasticity of the pin shaft; when the pressing part approaches to the base plate, the clamping part at the other end of the clamping plate is far away from the corresponding base plate based on the pin shaft, so that the volume of the accommodating cavity is increased, and the T-shaped reaction tube can conveniently enter the accommodating cavity; when the pressing part is far away from the base plate, the clamping part at the other end of the clamping plate is close to the corresponding base plate based on the pin shaft, so that the volume of the accommodating cavity is reduced, and the T-shaped reaction tube can be clamped and fixed by the clamping part and the base plate in the accommodating cavity; the clamping plate and the base plate can be in opposite direction based on the elasticity of the pin shaft, so that the T-shaped reaction tube is clamped and fixed.
Preferably, a first arc-shaped heating groove matched with the shape of the projection reaction tube is arranged on the base plate; a second arc-shaped heating groove corresponding to the first arc-shaped heating groove is formed in one side, facing the base plate, of the clamping part; the first arc-shaped heating groove and the second arc-shaped heating groove can be encircled to form an accommodating cavity for accommodating the projection reaction tube; the first arc-shaped heating groove and the second arc-shaped heating groove are internally provided with the heater and the temperature measuring sensor which can be abutted against the projection reaction tube when the T-shaped reaction tube is clamped and fixed.
Preferably, the clamping part further comprises a plurality of heating units and elastic connecting pieces which correspond to the heating units and are used for connecting the heating units; an elastic connecting piece is arranged between every two heating units, and the plurality of heating units are sequentially connected through the elastic connecting pieces to form the second arc-shaped heating groove; a plurality of the heating unit passes through elastic connection spare, and pass through elastic connection spare forms outside-in's contractile force, makes the arc of second arc heating groove's cross-section can be to the indent of centre of a circle department, so that T type reaction tube throw the reaction tube and be getting into when the holding intracavity, based on centripetal contractile force between the heating unit, make every the heating unit can be along with the shape laminate in the outer wall of throwing the reaction tube, and the centre gripping is fixed throw the reaction tube.
Preferably, the heating unit comprises a heating body and a connecting plate block; a heater is arranged in the heating body and used for heating the T-shaped reaction tube; the section of the heating body is of a trapezoidal structure; wherein, the side length of the upper end of the trapezoid structure is larger than that of the lower end; the upper end of the heating body is connected with the connecting plate, and the lower end of the heating body is used for abutting against the outer wall of the projection reaction tube; the connecting plates of every two heating units are elastically connected through one elastic connecting piece.
Preferably, the elastic connecting piece comprises a supporting fixing part, a first elastic component and a second elastic component which are sequentially arranged from top to bottom in parallel; the two ends of the support fixing part, the first elastic component and the second elastic component in the horizontal direction are respectively connected with a connecting plate block of a heating unit; and the lengths of the support fixing part, the first elastic component and the second elastic component are sequentially decreased progressively, so that under the support fixing of the support fixing part and the contraction of the inward elastic contraction force of the first elastic component and the second elastic component, the distance between the heating bodies of the heating units at the two ends is reduced and the heating bodies are close to each other.
Preferably, the sampling tube of the T-shaped reaction tube comprises: the device comprises a common input pipeline connected with the projection reaction pipe, and a sample to be tested branch pipeline and a clean gas branch pipeline which are connected with one end of the common input pipeline, which is far away from the projection reaction pipe, so as to form a three-way structure of the common input pipeline, the sample to be tested branch pipeline and the clean gas branch pipeline; the sample to be measured branch pipeline is used for inputting sample gas to be measured into the projection reaction pipe through the common input pipeline; the cleaning gas branch pipe is used for inputting cleaning gas into the projection reaction pipe through the common input pipe.
Preferably, the sample inlet pipe further comprises a gas-following blocking assembly which is arranged in the common input pipeline and is connected with the sample branch pipeline to be detected and the clean gas branch pipeline; the gas-following plugging component comprises a rotary hinged shaft, and a clean gas cover and a sample cover which are hinged with the hinged shaft; the angle between the clean gas cover and the sample cover is fixed; integrally forming the clean gas cover and the sample cover into an L-shaped structure movable based on the hinge shaft; the sample cover is matched with the pipe diameter of the sample branch pipeline to be detected; the cleaning gas cover is matched with the pipe diameter of the cleaning gas branch pipeline; when gas is input into the common input pipeline from the sample branch pipeline to be detected, the sample cover is far away from the sample branch pipeline to be detected, and the clean gas cover covers the port of the clean gas branch pipeline facing one end of the common input pipeline; when the gas is input into the common input pipeline from the inside of the clean gas branch pipeline, the clean gas cover is far away from the clean gas branch pipeline, and the sample cover covers the port of the sample branch pipeline to be detected, which faces one end of the common input pipeline.
The utility model provides a heating control device of a hydride generator, which can realize controllable heating and cooling of a T-shaped reaction tube, thereby enabling the temperature in the T-shaped reaction tube to be matched with the ideal atomization temperature of an element to be detected in the detection process, and avoiding the occurrence of overhigh heating temperature and unstable atomization reaction in a quartz tube; and, thereby increase the heated area through centre gripping heat conduction device cladding projection reaction tube, improve the uniformity of being heated, improved the repeatability that leads to data stability and test value, brought the convenience for using the hydride generator to carry out elemental analysis.
Drawings
Fig. 1 is a schematic circuit diagram of a heating control device of a hydride generator according to the present application;
FIG. 2 is a schematic structural view of a T-shaped reaction tube and a clamping heat-conducting device before and after combination;
FIG. 3 is a schematic side view of the heat transfer device;
FIG. 4 is an exploded view of the clamping heat transfer device and the T-shaped reaction tube;
FIG. 5 is a schematic view of a refrigeration assembly;
FIG. 6 is a schematic diagram of a heat dissipation device structure and a hot and cold air flow transmission circuit;
FIG. 7 is a schematic view of a connection structure including a plurality of heating units in the first arc-shaped heating bath;
FIG. 8 is a schematic view of a connection structure between the heating unit and the elastic connection member, and a partially enlarged schematic view of the elastic connection member;
FIG. 9 is a schematic diagram of a T-shaped reaction tube including exhaust ports with different exhaust directions;
FIG. 10 is a schematic view of a sample introduction tube of a T-shaped reaction tube;
FIG. 11 is a schematic structural view of a displacement adjustment assembly;
fig. 12 is a schematic structural view of the gas-liquid separation module.
Reference numerals: t-shaped reaction tube-1, projection reaction tube-11, exhaust port-111, sample inlet tube-12, common input pipeline-121, sample branch pipeline-122 to be detected, clean gas branch pipeline-123, gas following blocking component-124, rotary hinge shaft-1241, clean gas cover-1242, sample cover-1243, heating temperature control component-2, clamping heat conduction device-21, base plate-211, first arc heating groove-2111, clamping plate-212, clamping part-2121, second arc heating groove-2121 a, heating unit-2121 a-1, heating body-2121 a-11, connecting plate-2121 a-12, elastic connecting piece-2121 a-2, support fixing part-2121 a-21, first elastic component-2121 a-22, and a gas supply pipe-121, A second elastic component-2121 a-23, a pressing part-122, a pin shaft-213, a containing cavity-214, a heater-22, a temperature measuring sensor-23, a temperature control device-24, a heat dissipation device-25, a heat dissipation body-251, a heat dissipation single sheet-2511, a refrigeration component-252, a base heat dissipation sheet-2521, a refrigeration fan-2522, a gas-liquid separation component-3, a shell-31, a cooling cavity-311, a waste liquid discharge port-312, a centrifugal device-32, a gas-liquid separation cavity-321, a first centrifugal shaft-322, a second centrifugal shaft-323, an initial gas inlet port-324, a gas outlet port-325, a rotating blade-326, a gas drying part-3251, an S-shaped pipeline-3251 a, a desiccant-3251 b, a, Liquid cooling component-33, condenser pipe-331, semiconductor refrigerating device-332, liquid storage part-333, cooling liquid circulating device-334 and circulating pipeline-335.
The objects, features and advantages of the present invention will be further described with reference to the accompanying drawings.
Detailed Description
Reference will now be made in detail to the embodiments of the present invention, wherein like or similar reference numerals refer to like or similar elements or elements having like or similar functions throughout. Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically limited otherwise. In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," and "fixed" are to be construed broadly and may, for example, be fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meaning of the above terms in the present invention can be understood according to specific situations by those skilled in the art. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1: referring to fig. 1 to 6, the present embodiment provides a heating control device for a hydride generator, which is applied to a hydride generator based on flame heating, and comprises: a T-shaped reaction tube 1 and a heating temperature control component 2; the heating temperature control assembly 2 comprises a clamping heat conduction device 21, a temperature measurement sensor 23 and a heat dissipation device 25 connected with the clamping heat conduction device 21; the T-shaped reaction tube 1 comprises a projection reaction tube 11 and a sample inlet tube 12 vertically connected with the projection reaction tube 11; the clamping heat conduction device 21 can be detachably connected with the T-shaped reaction tube 1 and can clamp and coat the projection reaction tube 11 of the T-shaped reaction tube 1; the temperature sensor 23 is arranged on the clamping heat conduction device 21 and can be contacted with the projection reaction tube 11 when the T-shaped reaction tube 1 is clamped and fixed; the heat sink 25 includes a heat sink body 251 connected to the clamping heat conduction device 21, and a cooling assembly 252 disposed on the heat sink body 251.
Existing laboratory flame heating based hydride generators may include: PerkinElmer MHS-15, Shimadzu HVG-1, Teledyne CETAC HGX-200, and Beijing Hanshi 630B all have the problems of poor detection stability and reproducibility caused by uneven flame heating and/or uncontrollable over-high temperature. If the flame heating of the hydride generator needs to be changed into other heating modes to improve the stability, the whole hydride generator needs to be replaced, and the experiment cost is greatly improved. In the embodiment, only one independent set of hydride generator heating control device is externally hung, so that the purpose of high-temperature heating temperature control is realized under the condition of not changing the original equipment.
The T-shaped reaction tube 1 is used for being connected with a pipeline, and reaction gas is input into the sample inlet tube 12 until the gas enters the projection reaction tube 11 for irradiation so as to realize the detection purpose. The clamping heat conduction device 21 is used for clamping and fixing the projection reaction tube 11, can clamp and coat the T-shaped reaction tube 1 to realize fixation, and is detachably connected with the T-shaped reaction tube 1. The clamping heat conduction device 21 is conveniently disassembled and assembled with the T-shaped reaction tube 1. When the clamping heat conduction device 21 is connected with the T-shaped reaction tube 1, the outer wall of the projection reaction tube 11 can be coated and clamped, so that the clamping heat conduction device can play a role in fixing and can improve the heating area. The area or size of the coated projection reaction tube 11 is based on achieving a better heat conduction effect, and other positions except for the two ends used for projecting detection light rays can be coated, so that a better temperature control effect is achieved. The clamping heat-conducting device 21 may be made of a material that is resistant to high temperature and can achieve a uniform heat-conducting effect. For example, but not limited to, ceramics, magnesium aluminum compounds, mica, corundum, silicon, graphite, titanium alloys, diamond, and the like, as well as combinations of materials with or without other materials. The holding heat conduction device 21 may heat the holding heat conduction device 21 itself at a high temperature by using flame, or may have a heating function itself. After the T-shaped reaction tube 1 is clamped and coated and fixed through the clamping heat conduction device 21 during detection, heat is uniformly conducted through the coating contact part, compared with the existing heating mode, the heating area for heat conduction is increased, and the heating uniformity is improved. The heat sink 25 is connected to the clamping heat conductor 21. The heat dissipating body 251 may be an array of a plurality of heat dissipating fins arranged according to a certain configuration structure, and the heat dissipating body 251 may be disposed at an upper end of the clamping heat conducting device 21. The upper end of heat dissipation body 251 is equipped with refrigeration subassembly 252 for refrigerate heat dissipation body 251, thereby improve cooling effect and efficiency, make the temperature can drop to required temperature rapidly on controllable basis. The heat dissipating body 251 may have a sheet shape, and a better heat dissipating effect is achieved by increasing a heat dissipating surface area thereof.
The temperature sensor 23 is arranged in the clamping heat conduction device 21, can be in contact with the projection reaction tube 11, and can acquire the current temperature of the T-shaped reaction tube 1 during detection. By comparing the collected current temperature with the preset temperature interval, when the current temperature is higher than the preset temperature interval, the refrigeration assembly 252 of the heat dissipation device 25 can be started to rapidly refrigerate the heat dissipation body 251, and the heat conducted by the heat conduction device 21 of the heat dissipation body 251 is rapidly cooled; when the current temperature enters the preset temperature range, the operation of the cooling component 252 of the heat dissipation device 25 may be stopped, and cooling may be stopped, so that the temperature is detected under the current detection condition.
The cooling assembly 252 may be an array of a plurality of coolers to cool the heat dissipating body 251. The refrigeration mode can be air cooling or liquid cooling. The liquid cooling can be cooling by adopting a cooling liquid circulation mode, and the cooling liquid can adopt liquid nitrogen, water and other liquids. In the experiment process, the heating temperature is higher, so the boiling point of the cooling liquid is required to be higher, and in addition, the distance between the circulating pipeline of the cooling liquid and the clamping heat conduction device 21 is more than a certain distance, otherwise the cooling liquid is easy to volatilize and is cooled and fails.
In the embodiment, after the clamping heat conduction device 21 clamps and fixes the T-shaped reaction tube 1, the clamping heat conduction device 21 can be heated, and as the clamping heat conduction device 21 clamps and covers the T-shaped reaction tube 1, heat is uniformly conducted to the projection reaction tube 11 by the clamping heat conduction device 21, so that the heating area of the projection reaction tube 11 is increased, and the heating efficiency and the heating uniformity are improved; the temperature measuring sensor 23 is used for monitoring the surface temperature of the T-shaped reaction tube 1, and when the temperature needs to be adjusted, the clamping heat conduction device 21 is cooled by the heat dissipation body 251 and the refrigeration component 252 of the heat dissipation device 25 together, so that the temperature rising, heating, cooling and refrigeration processes of the T-shaped reaction tube 1 are controllable. In a word, the embodiment can realize controllable heating of the T-shaped reaction tube 1, and the temperature in the T-shaped reaction tube 1 can be matched with the ideal atomization temperature of the element to be detected in the detection process; the clamping heat conduction device 21 is used for coating the projection reaction tube 11, so that the heating area is enlarged, the heating uniformity is improved, and the data stability and the repeatability of a test value are improved.
In addition, after the hydride generator heating control device finishes detection every time, the outer surface of the T-shaped reaction tube 1 can reach thousands of degrees, if the T-shaped reaction tube 1 needs to be replaced or taken out for cleaning, the T-shaped reaction tube needs to be stood for a long time for natural cooling, the experiment time is prolonged, and the experiment efficiency is reduced. This embodiment passes through heat abstractor 25, can automatic or manual start refrigeration subassembly 252, and the heat of passing through heat dissipation body 251 with T type reaction tube 1 rapidly conducts and carries out rapid cooling through refrigeration subassembly 252, can shorten the cooling time greatly, raises the efficiency, provides convenience for the experiment.
Further, the heat dissipation body 251 includes a plurality of heat dissipation single sheets 2511; the heat dissipation single sheets 2511 are arranged in parallel, and the heat dissipation single sheets 2511 are vertical to the surface of one side, facing the heat dissipation single sheets 2511, of the clamping heat conduction device 21; the cooling assembly 252 includes a plurality of cooling units disposed on a single cooling fin 2511 of the cooling body 251; the cooling unit includes a base heat radiation fin 2521 connected to the heat radiation single chip 2511, and a cooling fan 2522 provided on the base heat radiation fin 2521.
The heat dissipating body 251 includes a plurality of heat dissipating single sheets 2511 arranged in parallel, and the heat dissipating single sheets 2511 are sheet-shaped heat dissipating fins perpendicular to the surface connected between the clamping heat conducting devices 21, thereby increasing the heat conducting area and improving the heat dissipating effect. The surface of the material can be a plane or a curved surface, and the shape of the material except a parallel sheet can also be a spiral shape with certain rules and space intervals, and the like.
In this embodiment, each heat dissipating single piece 2511 of the heat dissipating body 251 may have an inverted trapezoid shape; this trapezoidal includes a minor face and a long limit, the minor face is connected with centre gripping heat conduction device 21, the one end of keeping away from centre gripping heat conduction device 21 is located on long limit, the realization utilizes finite space to come out the heat through minor face one end conduction, and with heat transfer to long limit one end, make the heat be fan-shaped minor face by centre gripping heat conduction device 21's junction, outside (long limit direction) sectorial radial conduction, thereby the heat is the outside conduction of scattering state and increases heat-conduction efficiency, improve refrigeration or cooling effect. Preferably, 4 radiating single fins 2511 are arranged side by side, and one or more refrigerating units are erected on the upper ends of every two radiating single fins 2511. An airflow space is arranged between two adjacent single heat dissipation sheets 2511, and cold airflow input or output by the refrigeration unit passes through the airflow space quickly, so that heat in the single heat dissipation sheets 2511 is brought out by cold airflow through the airflow space quickly through the airflow space, and quick cooling is realized.
In this embodiment, the cooling module 252 includes a plurality of cooling units arranged in an array, each cooling unit includes a cooling fan 2522 and a base heat sink 2521 at a lower end of the cooling fan 2522. The base radiating fins 2521 are connected with the radiating single sheets 2511 at the lower end and used for contacting and conducting heat on the radiating single sheets 2511, the refrigerating unit at the upper end transmits cold airflow to the base radiating fins 2521, and the airflow passes through the base radiating fins 2521 and enters the space between the radiating single sheets 2511 corresponding to the lower end of the refrigerating unit, so that the heat between the base radiating fins 2521 and the radiating single sheets 2511 is rapidly carried out by the airflow to achieve the rapid refrigerating effect. 4 groups of refrigerating units are arranged between every two radiating single sheets 2511 to realize rapid refrigeration of the radiating single sheets 2511.
Example 2: referring to fig. 1 and fig. 7 to 8, based on the above embodiment 1, this embodiment provides a heating control device for a hydride generator, wherein the heating temperature control assembly 2 further includes: a heater 22 arranged on the clamping heat-conducting device 21 and used for heating the T-shaped reaction tube 1, and a temperature control device 24 electrically connected with the heater 22 and the temperature measurement sensor 23.
The heater 22 and the temperature sensor 23 are embedded in the clamping heat conduction device 21, and after the T-shaped reaction tube 1 is combined with the clamping heat conduction device 21, both the heater 22 and the temperature sensor 23 can contact with the outer side surface of the T-shaped reaction tube 1 through the clamping heat conduction device 21. The temperature control device 24 is electrically connected with the temperature sensor 23 and the heater 22, the current temperature of the outer surface of the T-shaped reaction tube 1 is obtained through the temperature sensor 23, and the temperature returns to the temperature control device 24. The heater 22 may be a heating wire disposed in the clamping heat conduction device 21, the heating wire is electrically connected to the temperature control device 24, and the heating wire is covered with an insulating layer and distributed in the clamping heat conduction device 21, so that the clamping heat conduction device 21 can heat up uniformly.
The temperature control device 24 may include a processor, a storage device, a temperature control circuit, a control device, a display device, etc. connected by a data bus; the storage device is stored with an operating system, a temperature control program, a data management program and the like; the temperature measuring sensor 23 and the heater 22 are electrically connected with the processor through a data bus. The temperature measuring sensor 23 collects the current external surface temperature T1 of the T-shaped reaction tube 1, the temperature T1 returns to the processor, the processor converts data and displays the data in real time through the display device, the control device is used for adjusting the adjusted instruction according to the value of T1, the processor adjusts the heater 22 based on the temperature control circuit, and the heater 22 is directly controlled to heat the working temperature T2 of the T-shaped reaction tube 1.
In the embodiment, after the T-shaped reaction tube 1 is detachably clamped and fixed by the clamping heat conduction device 21, the temperature of the T-shaped reaction tube 1 is monitored by the temperature measurement sensor 23 in the heating temperature control assembly 2, and controllable temperature rise and reduction can be carried out by the heater 22 under the regulation and control of the temperature control device 24, so that the T-shaped reaction tube 1 is heated by replacing the original flame heating mode, and the high-temperature heating controllable adjustment of the T-shaped reaction tube 1 is realized by the built-in independent heating control device, so that the temperature in the reaction tube can be matched with the optimal test temperature of an element to be tested in the detection process, the stability of data and the accuracy of a test value are improved, and convenience is brought to element analysis by using a hydride generator; moreover, the replacement of the original equipment of the whole device is avoided, a flame combustion head is not needed, and only the independent atom absorption pool heating control device is required to be externally hung on the basis of the original hydride generator based on flame heating, so that the cost is reduced, the resource waste is avoided, and the aim of directly applying the hydride generator based on flame heating is fulfilled.
The clamping heat conduction device 21 includes a base plate 211 and a clamping plate 212; the base plate 211 and the clamping plate 212 are elastically hinged by a pin shaft 213. The clamping plate 212 includes a clamping portion 2121 and a pressing portion 2122 connected to the clamping portion 2121 based on the pin shaft 213; the included angle between the pressing portion 2122 and the clamping portion 2121 far from the end of the base plate 211 is less than 180 °.
As described above, base plate 211 and clamp plate 212 are hinged to each other by pin shaft 213, and pin shaft 213 causes the elasticity of opposing clamping forces between base plate 211 and clamp plate 212. The position of the pin shaft 213 is about the middle position of the base plate 211, and the clamping plate 212 can be formed into a V shape with a certain angle, that is, the middle part is connected with the base plate 211 through the pin shaft 213, and two ends have a certain angle relative to the tilting of the base plate 211. For example, the angle between the nip portion 2121 and the pressing portion 2122 (the angle in the direction away from the base plate 211) is 120 °, the nip portion 2121 abuts against the base plate 211 before the pressing portion 2122 is not pressed, and the pressing portion 2122 forms an angle of 60 ° with the base plate 211.
The clamping part 2121 and the base plate 211 enclose a receiving cavity 214 for receiving the projection reactor 11, and the elasticity of the pin shaft 213 provides a clamping force between the clamping part 2121 and the base plate 211.
When the pressing portion 2122 approaches to the base plate 211, the clamping portion 2121 at the other end of the clamping plate 212 is separated from the corresponding base plate 211 based on the pin shaft 213, so that the volume of the accommodating cavity 214 is increased, and the T-shaped reaction tube 1 can conveniently enter the accommodating cavity 214; when the pressing portion 2122 is far away from the base plate 211, the clamping portion 2121 at the other end of the clamping plate 212 is close to the corresponding base plate 211 based on the pin shaft 213, so that the volume of the accommodating cavity 214 is reduced, and the T-shaped reaction tube 1 can be clamped and fixed by the clamping portion 2121 and the base plate 211 in the accommodating cavity 214; the clamping plate 212 and the base plate 211 can elastically meet each other based on the pin shaft 213 so as to clamp and fix the T-shaped reaction tube 1.
As the pin shaft 213 elastically connects the base plate 211 and the clamping plate 212, when the pressing portion 2122 is pressed to approach the base plate 211, the clamping portion 2121 is far from the base plate 211, the volume of the accommodating chamber 214 is increased, and the T-shaped reaction tube 1 can be installed; at this time, the pin shaft 213 has a pressure to press the clamping portion 2121 of the clamp plate 212 against the base plate 211, and when the pressing portion 2122 is stopped being pressed, the pressing portion 2122 is pressed against the T-shaped reaction tube 1 on the base plate 211 by the elastic pressure, thereby clamping and fixing the T-shaped reaction tube 1.
As described above, the pin shaft 213 serves to achieve the connection and elastic hinge between the base plate 211 and the clamping plate 212. Wherein, the pin shaft 213 can be provided with an elastic clamp spring, when the base plate 211 and the pressing part 2122 of the clamping plate 212 are pressed, the clamp spring is deformed, and after the pressing is stopped, the clamp spring restores the original shape based on the memory property to clamp the projection reaction tube 11 of the T-shaped reaction tube 1 therein. In addition, the elastic hinge implementation of the pin shaft 213 may be in other manners, which are not described in detail herein.
In the existing hydride generator, in order to guarantee the stability to the T-shaped reaction tube 1 dismounting mode is more tedious, its heating device and fixing device are two different parts respectively, thus bring inconvenience for T-shaped reaction tube 1 dismounting. In this embodiment, the built-in heater of centre gripping heat-transfer device 21, its body has heating function and fixed connection's function concurrently, and fixed connection is realized through the elasticity centre gripping, only need press base plate 211 and splint 212 to make according to the portion 2122 and be close to base plate 211, just can pack into or take out T type reaction tube 1, and elastic pressure through between base plate 211 and the splint 212 makes T type reaction tube 1 be fixed in wherein, thereby the convenience of the installation of T type reaction tube 1 and the stability in the testing process have been improved, the degree of accuracy of experimental data has been improved on the one hand, and on the other hand carries out the convenience that the in-process has improved the dismouting in the experiment, for the going on of experiment provides convenience.
A first arc-shaped heating groove 2111 matched with the shape of the projection reaction tube 11 is arranged on the base plate 211; a second arc-shaped heating groove 2121a corresponding to the first arc-shaped heating groove 2111 is formed in one side of the clamping part 2121 facing the base plate 211; the first arc-shaped heating groove 2111 and the second arc-shaped heating groove 2121a can form an accommodating cavity 214 for accommodating the projection reaction tube 11; the first arc heating groove 2111 and the second arc heating groove 2121a are respectively provided with a heater 22 and a temperature sensor 23 which can abut against the projection reaction tube 11 when the T-shaped reaction tube 1 is clamped and fixed.
The temperature sensors 23 can be arranged in a plurality of numbers, and the temperature sensors 23 at a plurality of different positions can simultaneously acquire the temperatures of different parts of the outer wall of the projection reaction tube 11, so that the current heating uniformity of the projection reaction tube 11 can be further confirmed. For example, 1 temperature sensor 23 is arranged at every 1 cm, the preset temperature difference range between every two temperature sensors 23 is set to be X less than or equal to 0.3 ℃, if the preset temperature difference calculated by the temperatures acquired by some two temperature sensors 23 exceeds 0.3 ℃, the heating temperature is determined to be uneven, the experiment is stopped, and the fault part is checked.
Above, the susceptor plate 211 is provided with a first arc-shaped heating groove 2111, which is shaped as an arc-shaped groove, the projection reaction tube 11 is tubular with a circular cross section, the length direction of the first arc-shaped heating groove 2111 of the susceptor plate 211 is adapted, and the arc shape of the first arc-shaped heating groove 2111 can be adapted to the projection reaction tube 11. Second arc adds heat channel 2121a and first arc adds heat channel 2111 corresponding and can symmetrical setting, so that enclose into an accommodation chamber 214 between two arc adds the heat channel, the shape of this accommodation chamber 214 can be cylindricly, with the shape of the appearance looks adaptation of projection reaction tube 11, so that can laminate the lateral wall of projection reaction tube 11 as far as possible after reaction tube 11 is thrown in the centre gripping, on the one hand can improve heating efficiency, make the heating more even, on the other hand can detect the temperature more accurately, in addition also can make the centre gripping to projection reaction tube 11 follow the shape more, can realize improving the stability of centre gripping.
Further, the clamping part 2121 further comprises a plurality of heating units 2121a-1, and elastic connecting pieces 2121a-2 corresponding to the heating units 2121a-1 and used for connecting the heating units 2121 a-1; an elastic connecting piece 2121a-2 is arranged between every two heating units 2121a-1, and the plurality of heating units 2121a-1 are sequentially connected through the elastic connecting pieces 2121a-2 to form a second arc-shaped heating groove 2121 a; the plurality of heating units 2121a-1 form an outward-inward contraction force through the elastic connecting members 2121a-2 and the elastic connecting members 2121a-2, so that the arcs of the cross sections of the second arc-shaped heating grooves 2121a can retract toward the center of the circle, and when the projection reaction tube 11 of the T-shaped reaction tube 1 enters the accommodating chamber 214, each heating unit 2121a-1 can be attached to the outer wall of the projection reaction tube 11 and clamp and fix the projection reaction tube 11 based on the centripetal contraction force between the heating units 2121 a-1.
In the heating process of the T-shaped reaction tube 1 in the hydride generator, the uniformity of heating affects the decomposition efficiency, speed, completeness and stability of the hydride, and the T-shaped reaction tube 1 can not completely fit the projection reaction tubes 11 with different sizes due to the different reaction requirements and detection means requirements of the T-shaped reaction tube 1 or products produced by different manufacturers with different sizes and models, and the diameters of the projection reaction tubes 11 have different sizes, so that the accommodating cavity 214 between the clamping part 2121 and the base plate 211 cannot completely fit the projection reaction tubes 11 with different sizes, and during clamping, the projection reaction tubes 11 may leave a part which cannot be attached (abutted) and a space, so that on one hand, the attachment area is insufficient, the heating efficiency is affected, on the other hand, the clamping cannot be carried out in a shape, and the clamping is unstable.
In another embodiment to solve the above problem, the clamping part 2121 is composed of a plurality of heating units 2121a-1 connected in sequence, an elastic connecting member 2121a-2 is provided between the heating units 2121a-1, the heating units 2121a-1 are connected in pairs by the elastic connecting member 2121a-2 to form a flexible connection consisting of a plurality of heating units 2121a-1, and the heating units 2121a-1 are connected to the heating units 2121a-1 at two ends on one hand, and can generate a shrinking force from outside to inside of the heating units 2121a-1 at two ends on the other hand, so that the first arc-shaped heating groove 2111 as a whole has a centripetal shrinking force from the arc periphery to the arc center, and thus after the projection reaction tube 11 of the T-shaped reaction tube 1 is placed in the accommodating cavity 214, the plurality of heating units 2121a-1 are adhered to the outer surface of the projection reaction tube 11 of the T-shaped reaction tube 1, the shape of the projection reaction tube 11 is matched and attached, so that the outer wall of the projection reaction tube 11 is wrapped and clamped in a shape following manner, on one hand, the attachment area is increased, and the heating efficiency is improved; on the other hand, the shape following clamping improves the stability of clamping and fixing the reaction tube.
Further, the heating unit 2121a-1 includes heating bodies 2121a-11 and connecting blocks 2121 a-12; a heater 22 is arranged in the heating body 2121a-11 and used for heating the T-shaped reaction tube 1; the section of the heating body 2121a-11 is of a trapezoidal structure; wherein, the side length of the upper end of the trapezoid structure is larger than that of the lower end; the upper ends of the heating bodies 2121a-11 are connected with the connecting plates 2121a-12, and the lower ends of the heating bodies 2121a-11 are used for abutting against the outer wall of the projection reaction tube 11; the connecting blocks 2121a-12 of each two heating units 2121a-1 are elastically connected by an elastic connection member 2121 a-2.
The heaters 2121a-11 are trapezoidal with large upper part and small lower part, the connecting plates 2121a-12 are arranged at the upper ends of the heaters 2121a-11, the width and length of the connecting plates can be the same as the upper length of the heaters 2121a-11, and the elastic connecting pieces 2121a-2 are connected to each connecting plate 2121a-12, so that the upper ends of the heaters 2121a-11 are fixed, the lower ends of the heaters are closed towards each other, and the clamping effect of centripetal (projecting the direction of the center of the cross section of the reaction tube 11) contraction is realized.
Further, the elastic connecting member 2121a-2 comprises a support fixing part 2121a-21, a first elastic element 2121a-22 and a second elastic element 2121a-23 arranged in parallel from top to bottom; the support fixing parts 2121a-21, the first elastic elements 2121a-22 and the second elastic elements 2121a-23 are coupled to the coupling blocks 2121a-12 of the heating unit 2121a-1 at both ends in the horizontal direction, respectively; and the lengths of the support fixtures 2121a-21, the first elastic elements 2121a-22 and the second elastic elements 2121a-23 are sequentially decreased such that the distance between the heating bodies 2121a-11 of the heating units 2121a-1 at both ends is decreased and approached under the support fixture of the support fixtures 2121a-21 and under the contraction of the inward elastic contraction force of the first elastic elements 2121a-22 and the second elastic elements 2121 a-23.
The resilient connecting element 2121a-2 includes a support fixture 2121a-21, a first resilient component 2121a-22 and a second resilient component 2121 a-23. Wherein the support fixing parts 2121a-21 have the longest length for supporting the connecting blocks 2121a-12 at both ends, and the first elastic elements 2121a-22 and the second elastic elements 2121a-23 at the lower ends may be spring members which are contracted toward the center. The connecting plate 2121a-12 has a certain height, and is sequentially connected with a support fixing part 2121a-21, a first elastic component 2121a-22 and a second elastic component 2121a-23 in the longitudinal direction, and under the support of the fixed length of the support fixing part 2121a-21, the two elastic components at the lower end respectively generate gradually increased elastic contraction force towards the center, so that the heating bodies 2121a-11 at the two ends of the elastic connecting part 2121a-2 are closed towards each other, and the overall contraction clamping effect is realized. As described above, the first resilient elements 2121a-22 and the second resilient elements 2121a-23 may be formed by a plurality of springs with different specifications, for example, the first resilient elements 2121a-22 may be two sets of springs, and the second resilient elements 2121a-23 may be 3 sets of springs.
Under the premise that the supporting and fixing part 2121a-21 supports and supports the heating units 2121a-1 at two ends, the first elastic component 2121a-22 and the second elastic component 2121a-23 which do not have different lengths and pull forces contract and pull back the end of the heating unit 2121a-1 far away from the supporting and fixing part 2121a-21, so that the contraction and centripetal approach between the heating units 2121a-1 are realized, and the effect of clamping the projection reaction tube 11 is generated, thereby better realizing the adaptation of the projection reaction tubes 11 with different sizes and diameters, improving the heat conduction efficiency and improving the stability.
Example 3: referring to fig. 9 to 10, based on the above embodiment 1 or 2, this embodiment provides a heating control device for a hydride generator, wherein the sample introduction tube 12 of the T-shaped reaction tube 1 includes: a common input pipeline 121 connected with the projection reaction tube 11, and a sample-to-be-detected branch pipeline 122 and a clean gas branch pipeline 123 both connected with one end of the common input pipeline 121, which is far away from the projection reaction tube 11, so as to form a three-way structure of the common input pipeline 121, the sample-to-be-detected branch pipeline 122 and the clean gas branch pipeline 123; the sample to be measured branch pipeline 122 is used for inputting a sample gas to be measured into the projection reaction tube 11 through the common input pipeline 121; the cleaning gas branch line 123 is used to supply cleaning gas into the projection reaction tubes 11 through the common supply line 121.
In the measurement of some elements which are easy to remain in the quartz tube, impurities are easy to generate or remain on the inner wall in the experiment, so that the memory effect is caused, and the next experimental data is influenced. To solve the above problem, in the present embodiment, the sample inlet 12 is provided with a bifurcated structure, i.e. a three-way structure formed by the common input pipeline 121, the sample-to-be-measured branch pipeline 122 and the clean gas branch pipeline 123, so as to be bifurcated into the sample-to-be-measured branch pipeline 122 and the clean gas branch pipeline 123. After each experiment, clean gas is input into the pipeline through the clean gas branch pipeline 123, and the clean gas can be dry compressed air and input into the reaction tube through an air compressor, an air pump and the like, so that the effect of rapidly removing residual impurities in the projection reaction tube 11 is achieved.
In order to achieve the effect of impurity removal and avoid the harm to operators caused by harmful gas generated by hydride reaction volatilizing outside the T-shaped reaction tube after measurement. In this embodiment, the two ends of the projection reaction tube 11 in the length direction are respectively provided with an exhaust port 111, the extending direction of the exhaust port 111 can be perpendicular to the length direction of the projection reaction tube 11, and is used for connecting with an air extraction device, the air extraction device can be a vacuum pump or the like or an exhaust ventilation device in a laboratory, and the exhaust ports 111 at the two ends can simultaneously remove impurities and gases in the projection reaction tube 11, so as to rapidly exhaust harmful gases. Therefore, harmful gas in the pipeline can be rapidly pumped out in the reaction process and the cleaning stage after the reaction is finished. On the one hand, the effect of rapid impurity removal is realized, residue is avoided, and on the other hand, harm of harmful gas to experimenters is avoided.
In another embodiment, the exhaust ports 111 at both ends may be arranged in parallel in the same direction, or may be arranged symmetrically one above the other. Preferably, the exhaust ports 111 in the upper and lower directions are symmetrically arranged and are matched with the clean gas branch pipeline 123 for inputting the clean gas, so that the input clean gas forms gas exhaust paths on two sides after entering the projection reaction tube 11, and compared with the exhaust ports 111 arranged in parallel in the same direction, the gas flow direction can be distributed over the whole tube body without dead angles, so that the residual gas in the pipeline can be rapidly and completely exhausted, the gas exhaust efficiency is improved, and the clean gas cleaning efficiency is improved.
Further, the sample inlet pipe 12 further includes a gas-following blocking assembly 124 disposed in the common input pipeline 121 and connected to both the sample-to-be-detected branch pipeline 122 and the clean gas branch pipeline 123; the accompanying gas block assembly 124 includes a rotation hinge shaft 1241, and a clean gas cover 1242 and a sample cover 1243 both hinged to the hinge shaft; the angle between the clean gas cap 1242 and the sample cap 1243 is fixed; the clean gas cover 1242 and the sample cover 1243 are integrally formed into an L-shaped structure movable based on the hinge shaft; moreover, the sample cover 1243 is adapted to the pipe diameter of the sample branch pipe 122 to be measured; the clean gas cover 1242 is adapted to the pipe diameter of the clean gas branch pipe 123; so that when gas is input from the sample branch pipe 122 to the common input pipe 121, the sample cover 1243 is away from the sample branch pipe 122, and the clean gas cover 1242 covers the port of the clean gas branch pipe 123 facing one end of the common input pipe 121; when gas is supplied from the clean gas branch pipe 123 to the common input pipe 121, the clean gas cover 1242 is away from the clean gas branch pipe 123, and the sample cover 1243 covers the port of the sample branch pipe 122 facing one end of the common input pipe 121.
Above-mentioned, when utilizing clean gas to inwards input edulcoration, perhaps gaseous in the tee bend except to throwing in the reaction tube 11, also can get into other pipelines in the reaction tube 11 that inputs into of reaction gas to throwing, cause gaseous revealing, influence reaction efficiency and the clean efficiency of edulcoration. In this embodiment, a gas-following blocking assembly 124 is provided, which is an L-shaped structure hinged at a tee joint position by rotating a hinge shaft 1241, an angle between a clean gas cover 1242 and a sample cover 1243 is fixed, that is, a fixed angle is formed between the two to form an L shape without change, when clean gas is input, the clean gas cover 1242 is pushed open, so that the sample cover 1243 at the other end of the L-shaped structure blocks a corresponding sample branch pipeline 122 to be tested, thereby ensuring that the clean gas does not enter the sample branch pipeline 122 to be tested; when the input of the cleaning gas is stopped and the input of the reaction gas to be measured is started, the sample cover 1243 is opened, and the cleaning gas cover 1242 closes the corresponding cleaning gas branch line 123, thereby ensuring that the reaction gas to be measured does not enter the cleaning gas branch line 123. This embodiment is through based on the articulated reciprocal activity along with gas shutoff subassembly 124 in the pipeline of rotation articulated shaft 1241, realized that clean gas and the reaction gas that awaits measuring input alone in the pipeline, through rushing into of air current, open current required pipeline to close the pipeline that the other end need not admit air, avoided the gaseous problem of revealing of probably appearing, and then influenced reaction efficiency and the clear efficiency of edulcoration, this embodiment has improved clean efficiency, security and convenience have been improved.
Example 4: based on the above embodiments 1, 2 or 3, as shown in fig. 12, this embodiment provides a hydride generator heating control device, further including a gas-liquid separation assembly 3. The gas-liquid separation assembly 3 includes a housing 31, a centrifugal device 32, and a liquid cooling assembly 33; the centrifugal device 32 is sleeved in the shell 31, a gas-liquid separation cavity 321 is arranged in the centrifugal device 32, and a cooling cavity 311 for containing circulating cooling liquid is arranged between the centrifugal device 32 and the shell 31; the liquid cooling module 33 comprises a condenser pipe arranged in the gas-liquid separation cavity 321, a semiconductor refrigerating device 332, a liquid storage part 333, a cooling liquid circulating device 334 and a circulating pipeline 335; the condensation pipe is communicated with the cooling cavity 311, the cooling cavity 311 is communicated with the liquid storage part 333 through a circulating pipeline 335, the liquid storage part 333 is attached and connected with the semiconductor refrigerating device 332, and the cooling liquid circulating device 334 is connected with the circulating pipeline 335 and used for enabling cooling liquid to circulate; the condensation pipe, the cooling cavity 311, the circulation pipeline 335 and the liquid storage part 333 form a circulation closed loop, circulating cooling liquid is arranged in the circulation closed loop, the cooling liquid carries heat out of the gas-liquid separation cavity 321 from inside to outside based on the condensation pipe and the cooling cavity 311 in the circulation process, enters the liquid storage part 333 through the circulation pipeline 335 to be cooled based on the semiconductor refrigerating device 332, and then is returned to the cooling cavity 311 and the condensation pipe through the circulation pipeline 335. The coolant circulation device 334 may be a circulation pump.
A first centrifugal shaft 322 connected with the casing 31 is arranged at the upper end of the centrifugal device 32, and a gas output port 325 extending from the casing 31 to the outside for outputting gas after gas-liquid separation is arranged in the first centrifugal shaft 322; a second centrifugal shaft 323 connected with the housing 31 is arranged at the lower end of the centrifugal device 32, an initial gas inlet port 324 for inputting initial sample gas to be tested into the gas-liquid separation cavity 321 is arranged in the second centrifugal shaft 323, and a plurality of nozzles extending into the gas-liquid separation cavity 321 and spraying gas towards different directions can be arranged at the front end of the second centrifugal shaft 323; a waste liquid outlet 312 is also arranged, and the waste liquid outlet 312 can be provided with a selective one-way membrane; the recirculation line 335 is connected to the cooling chamber 311 via the second centrifugal shaft 323.
When the centrifugal device 32 rotates at a high speed relative to the housing 31 through the first centrifugal shaft 322 and the second centrifugal shaft 323, the initial gas inlet port 324 inputs the initial sample gas to be tested from the outside, the initial sample gas to be tested is sprayed upwards from the lower end to the inner walls of the condensation tube and the centrifugal device 32, the hot liquid vapor therein is rapidly refrigerated and condensed to form liquid drops, the liquid drops on the condensation tube are gathered on the inner wall of the centrifugal device 32 under the high-speed rotation of the centrifugal device 32 and flow out from the waste liquid outlet 312 to the lower end due to the gravity, and the gas after gas-liquid separation is output from the gas outlet port 325. In another embodiment, the inner wall of the centrifugal device 32 is provided with a plurality of rotating blades 326 for forming an ascending gas flow in the gas-liquid separation chamber 321 when the gas to be measured rotates, so that after the initial gas to be measured is condensed and centrifuged, the liquid component is condensed on the inner wall or the condensing pipe of the gas-liquid separation chamber 321 and is gathered to the lower waste liquid outlet 312 along with the gravity, and the gas rotates and rises after the gas-liquid separation to realize the three-dimensional separation in different directions.
It should be noted that, when the existing hydride generator is used for reaction, a reducing agent needs to be injected into a sample to be measured, when the element content of the sample to be measured is high, the reaction process with the reducing agent is sometimes very violent, sometimes a large amount of liquid bubbles and liquid-containing hot vapor are generated, during the reaction continuing process, the gas, the liquid bubbles, the liquid-containing hot vapor and the reaction liquid of the sample to be measured are directly injected into the T-shaped reaction tube 1 through a pipeline by an input device such as a peristaltic pump, and the liquid substance is continuously heated by high temperature after entering, so that the T-shaped reaction tube 1 is polluted, and the T-shaped reaction tube 1 cannot be used and is difficult to clean, and the measured data also has no experimental significance. The gas-liquid separator of the existing hydride generator can not solve the problem of liquid hot steam, and the hot steam can still be conveyed out along with the hydride gas.
In order to solve the problem, the gas-liquid separation assembly 3 is arranged at the front end of the T-shaped reaction tube 1 in the embodiment, and is used for realizing gas-liquid separation before detection and preventing backflow and liquid substances from entering the T-shaped reaction tube 1 to cause interference. The initial sample gas to be measured is the gas directly input after the reaction, mainly gaseous hydride, wherein foam liquid, micro liquid drops and liquid vapor generated by high-temperature reaction may be entrained, the input initial sample gas to be measured is cooled by using a condensation tube in the centrifugal device 32 and the inner wall of the centrifugal device 32 in a circulating liquid cooling manner, so that the hot vapor generated by reaction heat release in the initial sample gas to be measured is condensed to the condensation tube or the centrifugal device 32 to form a liquid state, the foam liquid and the micro liquid drops in the initial sample gas are attached to the inner walls of the centrifugal tube and the centrifugal device 32 under the high-speed centrifugation of the centrifugal device 32 based on a centrifugal effect and flow to the waste liquid discharge port 312 based on gravity to be collected and flow out, and the dry gas can be output to the gas output port 325 (an updraft generated by the rotating blade 326). Thereby realizing the bidirectional flow division of the gas and the liquid. A motor and a transmission may be provided at the first centrifugal shaft 322 and/or the second centrifugal shaft 323 for driving the rotation of the centrifugal device 32. The waste liquid outlet 312 may be provided with a waste liquid storage device for collecting waste liquid and connected to a quantitative liquid discharge pipe, and the waste liquid in the waste liquid storage device can be discharged from the quantitative liquid discharge pipe after reaching a predetermined volume.
Referring to fig. 11, in order to avoid contamination in the T-shaped reaction tube 1 caused by unremoved residual liquid vapor in the input gas during the experiment and memory effect, a gas drying portion 3251 is disposed at the gas output port 325 in this embodiment, and the gas drying portion 3251 is formed by an S-shaped pipeline 3251a with a drying agent 3251b disposed therein, so that the input gas can pass through the drying agent 3251b in the S-shaped pipeline 3251a and then be output to the branch pipeline 122 to be measured. Through the S-shaped pipeline 3251a, a drying agent 3251b is arranged in the S-shaped pipeline 3251a, so that the effect of removing water vapor and drying is achieved after the output gas passes through the drying agent 3251b, and then further output is carried out, so that the purposes of further removing impurities and water are achieved. Wherein the desiccant 3251b may include, but is not limited to, calcium sulfate, calcium chloride, and the like. To improve the drying effect, the S-shaped pipes 3251a can be connected in series in multiple sets while ensuring the gas flow rate.
In addition, before the projection reaction tube 11 of the T-shaped reaction tube 1 is detected, the optical path of the apparatus needs to be adjusted so that the optical path of the apparatus completely passes through the projection reaction tube 11 (which passes through both ends of the projection reaction tube 11 in the length direction), and the optical path is stable in the whole detection process, otherwise, the data repeatability is poor, and even the signal cannot be detected. The existing adjusting method is that a T-shaped reaction tube 1 is fixed with a flame combustion head through a bracket, the position is manually adjusted to be aligned with light paths at two ends, and then the adjustment is continuously carried out through the change of the current absorption value until the maximum absorption energy value is reached.
In order to solve the above problem, in another embodiment of this embodiment, the hydride generator heating control device may further include a displacement adjustment assembly in addition to the above parts; wherein, move the adjustment subassembly and include horizontal slide rail, locate the vertical movable slide rail on the horizontal slide rail, the base plate 211 of centre gripping heat conduction device 21 is located on the vertical movable slide rail.
A vertically movable slide rail for adjusting the displacement of the clamping heat transfer device 21 in the vertical direction of the Y-axis; and, the vertically movable slide rail can move along the horizontal direction of the X-axis of the horizontal slide rail, thereby adjusting the displacement of the clamping heat-conducting device 21 in the horizontal direction of the X-axis. Correspondingly, the bottom end of the vertical movable sliding rail can be provided with an X-direction pulley and an X-direction transmission mechanism which can move along the horizontal sliding rail, and an X-direction driving motor which drives the X-direction transmission mechanism through the X-direction driving motor so as to drive the X-direction pulley, so that the whole vertical movable sliding rail can be driven to reciprocate along the X-direction of the horizontal sliding rail. Correspondingly, a Y-direction pulley, a Y-direction transmission mechanism and a Y-direction driving motor can be arranged at the joint of the clamping heat conduction device 21 and the vertical movable sliding rail, the Y-direction driving motor drives the Y-direction transmission mechanism to drive the Y-direction pulley, so that the clamping heat conduction device 21 can be driven to move back and forth along the Y direction vertical to the movable sliding rail. Correspondingly, the X-direction driving motor and the Y-direction driving motor are both connected with a central control device of the equipment, or the central control device is independently arranged, and the current absorption value of the T-shaped reaction tube 1 is obtained in real time or at regular time, so that the spatial position of the T-shaped reaction tube 1 is automatically adjusted until the maximum signal is reached. Further, the projection reactor 11 of the T-shaped reactor 1 can be automatically adjusted to the correct position by the following control method.
In the X and Y directions of the cross section of the T-shaped reaction tube 1, a projection area capable of projecting the T-shaped reaction tube 1 and obtaining signal data is set in advance, and the shape of the projection area may be a square or other shapes. In the projection area, a plurality of detection coordinate points are divided in advance, and the number of the detection coordinate points can basically cover every detection position in the projection area. Adjusting the X axis and the Y axis of the T-shaped reaction tube 1 to enable the central point of the cross section of the T-shaped reaction tube to obtain signal data at each detection coordinate point in the projection area; and sequencing all the signal data, selecting a maximum value, obtaining a detection coordinate corresponding to the maximum value, taking the detection coordinate as a space detection position, and stopping adjusting the displacement of the X axis and the Y axis. Through the moving adjusting assembly provided in the embodiment, the automation of the displacement adjustment of the projection reaction tube 11 is greatly improved, the experiment efficiency is improved, the repeatability of multiple experiments is improved, and errors are prevented.
And (3) alignment experiment: 1. experimental set-up group: group A: heating the T-shaped reaction tube by using Perkinelmer mhs-15 hydride based on flame heating; group B: the hydride generator heating control device in the embodiment 2 is hung inside and outside the hydride generator to heat the T-shaped reaction tube without adopting flame heating. 2. The method conditions are as follows: and (3) performing parallel tests on the arsenic reference substance solution with the concentration of 2ng/mL by utilizing the group A and the group B devices respectively, wherein the liquid is carried with 1.5% hydrochloric acid, the reducing agent is a 1% sodium hydroxide solution containing 3% sodium borohydride, the wavelength of the arsenic element electrodeless discharge lamp is 197.2nm, and the integration time is 25 s. The atomization mode is as follows: group A acetylene-air (2.5:10) flames heat the T-shaped reaction tube; the group B external hanging hydride generator heating control device is set at 900 ℃; each was assayed in parallel 10 times. 3. The experimental results are as follows: group A: 1-0.0098; 2-0.01093; 3-0.0122; 4-0.0084; 5-0.0103; 6-0.0106; 7-0.0112; 8-0.0120; 9-0.0113; 10-0.0100; STD-0.0011; RSD-10.52%. Group B is 1-0.0104; 2-0.0105; 3-0.0107; 4-0.0105; 5-0.0106; 6-0.0105; 7-0.0107; 8-0.0103; 9-0.0105; 10-0.0104; STD-0.0001; RSD-1.22%. The experimental results show that the RSD% of the group B is reduced by 79% compared with the group A, and the stability is obviously improved.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A hydride generator heating control device is applied to a hydride generator based on flame heating, and is characterized by comprising:
the T-shaped reaction tube and the heating temperature control assembly;
the heating temperature control assembly comprises a clamping heat conduction device, a temperature measurement sensor and a heat dissipation device connected with the clamping heat conduction device;
the T-shaped reaction tube comprises a projection reaction tube and a sample inlet tube vertically connected with the projection reaction tube;
the clamping heat conduction device can be detachably connected with the T-shaped reaction tube and can clamp and coat the projection reaction tube of the T-shaped reaction tube; the temperature sensor is arranged on the clamping heat conduction device and can be contacted with the projection reaction tube when the T-shaped reaction tube is clamped and fixed;
the heat dissipation device comprises a heat dissipation body connected with the clamping heat conduction device and a refrigeration assembly arranged on the heat dissipation body.
2. A hydride generator heating control device as claimed in claim 1, wherein the heat dissipating body comprises a plurality of heat dissipating monoliths;
the heat dissipation single sheets are arranged in parallel, and the heat dissipation single sheets are vertical to the surface of one side, facing the heat dissipation single sheets, of the clamping heat conduction device;
the refrigerating assembly comprises a plurality of refrigerating units arranged on the radiating single sheet of the radiating body;
the refrigerating unit comprises a base radiating fin connected with the radiating single sheet and a refrigerating fan arranged on the base radiating fin.
3. The hydride generator heating control device of claim 1, wherein the heating temperature control assembly further comprises: the clamping heat conduction device is provided with a heater and a temperature control device, the heater is arranged on the clamping heat conduction device and used for heating the T-shaped reaction tube, and the temperature control device is electrically connected with the heater and the temperature measurement sensor.
4. A hydride generator heating control device as claimed in claim 3, wherein the clamping heat conductor comprises a base plate and a clamping plate;
the base plate is elastically hinged with the clamping plate through a pin shaft;
the clamping plate comprises a clamping part and a pressing part connected with the clamping part on the basis of the pin shaft; an included angle between the pressing part and the clamping part, which is far away from one end of the base plate, is less than 180 degrees;
an accommodating cavity for accommodating the projection reaction tube is enclosed between the clamping part and the base plate, and clamping force for clamping the clamping part and the base plate in opposite directions is generated through the elasticity of the pin shaft;
when the pressing part approaches to the base plate, the clamping part at the other end of the clamping plate is far away from the corresponding base plate based on the pin shaft, so that the volume of the accommodating cavity is increased, and the T-shaped reaction tube can conveniently enter the accommodating cavity;
when the pressing part is far away from the base plate, the clamping part at the other end of the clamping plate is close to the corresponding base plate based on the pin shaft, so that the volume of the accommodating cavity is reduced, and the T-shaped reaction tube can be clamped and fixed by the clamping part and the base plate in the accommodating cavity;
the clamping plate and the base plate can be in opposite direction based on the elasticity of the pin shaft, so that the T-shaped reaction tube is clamped and fixed.
5. A hydride generator heating control device as claimed in claim 4, wherein the susceptor plate is provided with a first arc-shaped heating groove adapted to the shape of the projection reaction tube;
a second arc-shaped heating groove corresponding to the first arc-shaped heating groove is formed in one side, facing the base plate, of the clamping part; the first arc-shaped heating groove and the second arc-shaped heating groove can be encircled to form an accommodating cavity for accommodating the projection reaction tube;
the first arc-shaped heating groove and the second arc-shaped heating groove are internally provided with the heater and the temperature measuring sensor which can be abutted against the projection reaction tube when the T-shaped reaction tube is clamped and fixed.
6. A hydride generator heating control device as claimed in claim 5, wherein the nip further comprises a plurality of heating units, and elastic connecting members corresponding to the heating units for connecting the heating units;
an elastic connecting piece is arranged between every two heating units, and the plurality of heating units are sequentially connected through the elastic connecting pieces to form the second arc-shaped heating groove;
a plurality of the heating unit passes through elastic connection spare, and pass through elastic connection spare forms outside-in's contractile force, makes the arc of second arc heating groove's cross-section can be to the indent of centre of a circle department, so that T type reaction tube throw the reaction tube and be getting into when the holding intracavity, based on centripetal contractile force between the heating unit, make every the heating unit can be along with the shape laminate in the outer wall of throwing the reaction tube, and the centre gripping is fixed throw the reaction tube.
7. A hydride generator heating control device as claimed in claim 6, wherein the heating unit comprises a heating body and a connecting plate;
a heater is arranged in the heating body and used for heating the T-shaped reaction tube;
the section of the heating body is of a trapezoidal structure; wherein,
the side length of the upper end of the trapezoid structure is larger than that of the lower end; the upper end of the heating body is connected with the connecting plate, and the lower end of the heating body is used for abutting against the outer wall of the projection reaction tube;
the connecting plates of every two heating units are elastically connected through one elastic connecting piece.
8. The heating control device for a hydride generator as claimed in claim 7, wherein the elastic connecting member comprises a supporting fixing portion, a first elastic member and a second elastic member arranged in parallel from top to bottom;
the two ends of the support fixing part, the first elastic component and the second elastic component in the horizontal direction are respectively connected with a connecting plate block of a heating unit; and the lengths of the support fixing part, the first elastic component and the second elastic component are sequentially decreased progressively, so that under the support fixing of the support fixing part and the contraction of the inward elastic contraction force of the first elastic component and the second elastic component, the distance between the heating bodies of the heating units at the two ends is reduced and the heating bodies are close to each other.
9. A hydride generator heating control device according to claim 1,
the sampling tube of the T-shaped reaction tube comprises: the device comprises a common input pipeline connected with the projection reaction pipe, and a sample to be tested branch pipeline and a clean gas branch pipeline which are connected with one end of the common input pipeline, which is far away from the projection reaction pipe, so as to form a three-way structure of the common input pipeline, the sample to be tested branch pipeline and the clean gas branch pipeline;
the sample to be measured branch pipeline is used for inputting sample gas to be measured into the projection reaction pipe through the common input pipeline;
the cleaning gas branch pipe is used for inputting cleaning gas into the projection reaction pipe through the common input pipe.
10. The hydride generator heating control device according to claim 9, wherein the sample introduction pipe further comprises a gas block assembly disposed in the common input line and connected to both the sample-to-be-measured branch line and the clean gas branch line;
the gas-following plugging component comprises a rotary hinged shaft, and a clean gas cover and a sample cover which are hinged with the hinged shaft;
the angle between the clean gas cover and the sample cover is fixed; integrally forming the clean gas cover and the sample cover into an L-shaped structure movable based on the hinge shaft; and,
the sample cover is matched with the pipe diameter of the branch pipeline of the sample to be detected; the cleaning gas cover is matched with the pipe diameter of the cleaning gas branch pipeline;
when gas is input into the common input pipeline from the sample branch pipeline to be detected, the sample cover is far away from the sample branch pipeline to be detected, and the clean gas cover covers a port of the clean gas branch pipeline facing one end of the common input pipeline;
when the gas is input into the common input pipeline from the inside of the clean gas branch pipeline, the clean gas cover is far away from the clean gas branch pipeline, and the sample cover covers the port of the sample branch pipeline to be detected, which faces one end of the common input pipeline.
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CN111867167A (en) * | 2020-08-19 | 2020-10-30 | 辽宁省检验检测认证中心 | Hydride generator heating control device |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN111867167A (en) * | 2020-08-19 | 2020-10-30 | 辽宁省检验检测认证中心 | Hydride generator heating control device |
CN111867167B (en) * | 2020-08-19 | 2024-08-06 | 辽宁省检验检测认证中心 | Heating control device of hydride generator |
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