CN117706026A - Reaction end point test system based on chemical reaction enthalpy change - Google Patents
Reaction end point test system based on chemical reaction enthalpy change Download PDFInfo
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- CN117706026A CN117706026A CN202311737120.5A CN202311737120A CN117706026A CN 117706026 A CN117706026 A CN 117706026A CN 202311737120 A CN202311737120 A CN 202311737120A CN 117706026 A CN117706026 A CN 117706026A
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 67
- 238000012360 testing method Methods 0.000 title claims abstract description 26
- 238000004448 titration Methods 0.000 claims abstract description 63
- 238000004891 communication Methods 0.000 claims description 20
- 238000005070 sampling Methods 0.000 claims description 16
- 238000001514 detection method Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 3
- 238000010998 test method Methods 0.000 claims description 3
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 13
- 238000003756 stirring Methods 0.000 abstract description 4
- 238000012544 monitoring process Methods 0.000 abstract description 2
- 238000010586 diagram Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000003918 potentiometric titration Methods 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000009529 body temperature measurement Methods 0.000 description 1
- 239000013013 elastic material Substances 0.000 description 1
- 230000006870 function Effects 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K13/00—Thermometers specially adapted for specific purposes
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- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Molecular Biology (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Automatic Analysis And Handling Materials Therefor (AREA)
Abstract
The invention relates to the technical field of chemical reaction tests, in particular to a reaction end point test system based on chemical reaction enthalpy change, which is characterized in that a chemical reaction reagent to be detected is placed in a container bottle, then the container bottle is sealed through a container cover, the reagent in the container bottle is introduced into a titration unit and enters a connecting pipe after the temperature is controlled, the reagent is output to a placing table through a burette terminal, the placing table is integrated with an ultrasonic stirring structure, so that the reagent can be stirred while being titrated after entering the placing table, the temperature is monitored through a temperature sensor, the data of the temperature sensor can be acquired by an acquisition board, the temperature data is converted into voltage data, the reaction process is continuously monitored, a temperature curve, a first derivative curve of the temperature and a second derivative curve of the temperature are finally obtained, and the inflection point of the second derivative corresponds to the end point of the temperature titration, so that the temperature monitoring can be more stable and accurate.
Description
Technical Field
The invention relates to the technical field of chemical reaction tests, in particular to a reaction end point test system based on chemical reaction enthalpy change.
Background
Titration analysis is one type of chemical analysis in which a standard reagent of known accurate concentration is added dropwise to a solution of a substance to be measured until the chemical reaction is completely stopped, whereby the content of the component to be measured is calculated.
The common titration method mainly relies on the change of the color of an indicator to indicate the titration end point, and if the solution to be measured is turbid, the end point is difficult to indicate. The conventional potentiometric titration method is to determine the end point of titration according to the change of the potential of an indication electrode, can be used for titrating colored or turbid solution, has higher sensitivity and accuracy, and has the defect that the potential of the electrode is limited to a certain extent at low concentration.
However, in the conventional titration method, the end point of titration is mainly indicated by means of the color change of the indicator, and if the solution to be tested is turbid, the end point is difficult to indicate. The conventional potentiometric titration method is to determine the end point of titration according to the change of the potential of an indication electrode, can be used for titrating colored or turbid solution, has higher sensitivity and accuracy, and has the defect that the potential of the electrode is limited to a certain extent at low concentration.
Disclosure of Invention
The invention aims to provide a reaction end point testing system based on chemical reaction enthalpy change, which aims to measure the concentration of a reagent to be tested by using a thermal effect of a titration reaction by adopting a temperature titration method, thereby improving the operation efficiency and accuracy.
To achieve the above object, in a first aspect, the present invention provides a reaction endpoint test system based on chemical reaction enthalpy change, which comprises a container assembly, a titration assembly and a detection assembly, wherein the container assembly comprises a container cover and a container bottle, the container cover is arranged at the top of the container bottle, the titration assembly comprises a suction pipe, a valve, a titration unit, a connecting pipe and a titration tube terminal, the valve is arranged on the titration unit, the suction pipe is connected with the container cover and the valve, one end of the connecting pipe is communicated with the titration unit, the other end of the connecting pipe is communicated with the titration tube terminal, the detection assembly comprises a placing table, a temperature sensor and a collecting plate, the placing table is arranged at the bottom of the titration tube terminal, the temperature sensor is arranged at one side of the placing table, and the collecting plate is connected with the temperature sensor and the titration unit.
Wherein, the container assembly also includes a drying pipe, the drying pipe is communicated with the container cover and is positioned at one side of the container cover.
The drying pipe comprises a pipe body and a filter element, and the filter element is arranged in the pipe body.
The burette terminal comprises a supporting rod, a sliding block, a clamp and a burette, wherein the supporting rod is arranged on one side of the placing table, the sliding block is in sliding connection with the supporting rod and is positioned on one side of the supporting rod, the clamp is arranged on the sliding block, and the burette is arranged on the clamp.
The sliding block comprises a block body, two elastic clamping plates and a button, wherein the two elastic clamping plates are fixed on the block body, the supporting rod is arranged between the two elastic clamping plates, the button is in sliding connection with the block body and is positioned at the top of the two elastic clamping plates, and the bottom of the button is in a triangular section.
Wherein the number of the clamps is a plurality.
The acquisition board comprises an MCU module, an AD sampling module, a PC communication module, a titrator unit communication module, a system clock, a ferroelectric memory and a power conversion module, wherein the AD sampling module is connected with the MCU module, the PC communication module is connected with the MCU module, the titrator unit communication module is connected with the MCU module, the system clock is connected with the MCU module, the ferroelectric memory is connected with the MCU module, and the power conversion module is connected with the MCU module.
In a second aspect, the present invention also provides a reaction endpoint test method based on chemical reaction enthalpy change, including: the system is powered on to carry out self-checking on each module, and the sampling module is sampled and calibrated;
setting a titration strategy through a titrator unit communication module;
starting a titration unit according to a set titration strategy, extracting detection liquid from a container bottle, and titrating through a burette;
the AD sampling module acquires temperature data and outputs a result table.
In the titration process, whether the second derivative of the temperature change is 0 or not is judged through the temperature data, and the titration is stopped when the second derivative of the temperature change is 0.
According to the reaction end point testing system based on chemical reaction enthalpy change, chemical reaction reagents to be detected are placed in the container bottle, then the container bottle is sealed through the container cover, the titration unit consists of the micro pump and the temperature control device, so that the reagents in the container bottle can be introduced into the titration unit, the temperature is controlled and then enters the connecting pipe, then the connecting pipe is output to the placing table through the buret terminal, the placing table is integrated with the ultrasonic stirring structure, the reagents can be stirred while entering the placing table, the temperature is monitored through the temperature sensor, the acquisition plate can acquire data of the temperature sensor, the temperature data are converted into voltage data, the reaction process is continuously monitored, and finally a temperature curve, a first derivative curve of the temperature, a second derivative curve of the temperature and an inflection point of the second derivative curve of the temperature, namely the corresponding temperature titration end point, are obtained, so that the temperature monitoring is more stable and accurate.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a block diagram of a reaction endpoint testing system based on chemical reaction enthalpy change according to a first embodiment of the invention.
Fig. 2 is a right side structural view of a reaction endpoint testing system based on chemical reaction enthalpy change according to a first embodiment of the present invention.
Fig. 3 is an enlarged view of a portion of detail a of fig. 2.
Fig. 4 is a block diagram of a collection board of a first embodiment of the present invention.
Fig. 5 is a flow chart of a reaction endpoint testing method based on chemical reaction enthalpy change according to a second embodiment of the invention.
Container assembly 101, titration assembly 102, detection assembly 103, container lid 104, container bottle 105, suction tube 106, valve 107, titration unit 108, connection tube 109, burette terminal 110, placement table 111, temperature sensor 112, collection plate 113, drying tube 114, tube body 115, filter cartridge 116, support rod 117, slide block 118, clamp 119, titration head 120, block 121, elastic clamp 122, button 123, MCU module 124, AD sampling module 125, PC communication module 126, titrator unit communication module 127, system clock 128, ferroelectric memory 129, power conversion module 130.
Detailed Description
Embodiments of the present invention are described in detail below, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to like or similar elements or elements having like or similar functions throughout. The embodiments described below by referring to the drawings are illustrative and intended to explain the present invention and should not be construed as limiting the invention.
In the description of the present invention, it should be understood that the terms "length," "width," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like indicate orientations or positional relationships based on the orientation or positional relationships shown in the drawings, merely to facilitate describing the present invention and simplify the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and therefore should not be construed as limiting the present invention. Furthermore, in the description of the present invention, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
First embodiment
Referring to fig. 1 to 4, fig. 1 is a block diagram of a reaction endpoint testing system based on chemical reaction enthalpy change according to a first embodiment of the present invention. Fig. 2 is a right side structural view of a reaction endpoint testing system based on chemical reaction enthalpy change according to a first embodiment of the present invention. Fig. 3 is an enlarged view of a portion of detail a of fig. 2. Fig. 4 is a block diagram of a collection board of a first embodiment of the present invention. The invention provides a reaction endpoint testing system based on chemical reaction enthalpy change, which comprises a container assembly 101, a titration assembly 102 and a detection assembly 103, wherein the container assembly 101 comprises a container cover 104 and a container bottle 105, the container cover 104 is arranged at the top of the container bottle 105, the titration assembly 102 comprises a suction pipe 106, a valve 107, a titration unit 108, a connecting pipe 109 and a burette terminal 110, the valve 107 is arranged on the titration unit 108, the suction pipe 106 is connected with the container cover 104 and the valve 107, one end of the connecting pipe 109 is communicated with the titration unit 108, the other end of the connecting pipe 109 is communicated with the burette terminal 110, the detection assembly 103 comprises a placing table 111, a temperature sensor 112 and a collecting plate 113, the placing table 111 is arranged at the bottom of the burette terminal 110, the temperature sensor 112 is arranged at one side of the placing table 111, and the collecting plate 113 is connected with the temperature sensor 112 and the titration unit 108.
In this embodiment, a chemical reaction reagent to be detected is placed in the container bottle 105, then the container bottle 105 is sealed by the container cover 104, the titration unit 108 is composed of a micro pump and a temperature control device, so that the reagent in the container bottle 105 can be introduced into the titration unit 108 and controlled in temperature, then enters into the connecting pipe 109, and then is output to the placing table 111 through the buret terminal 110, the placing table 111 is integrated with an ultrasonic stirring structure, so that the reagent can be stirred while being titrated after entering into the placing table 111, and the temperature is monitored by the temperature sensor 112, the collecting plate 113 can acquire the data of the temperature sensor 112, so that the temperature data is converted into voltage data to continuously monitor the reaction process, and finally, a temperature curve, a first derivative curve of the temperature, an inflection point of the second derivative curve, namely, an end point of the corresponding temperature titration are obtained, so that the temperature can be more stable and accurate.
The container assembly 101 further includes a drying tube 114, the drying tube 114 being in communication with the container cover 104 and located on one side of the container cover 104. In order to balance the atmospheric pressure and avoid the introduction of impurities into the container bottle 105, the drying duct 114 is further provided on the container bottle 105 so that the drying duct 114 can dry and filter the incoming air.
Specifically, the drying duct 114 includes a duct body 115 and a filter element 116, and the filter element 116 is disposed in the duct body 115. The filter element 116 can filter impurities in the air entering the tube 115 so as to avoid affecting the reagent in the container bottle 105.
Burette terminal 110 includes bracing piece 117, slider 118, clamp 119 and burette 120, bracing piece 117 sets up one side of placing the platform 111, slider 118 with bracing piece 117 sliding connection, and be located one side of bracing piece 117, clamp 119 sets up on slider 118, burette 120 sets up on clamp 119. The sliding block 118 may slide on the supporting rod 117, so that the height of the clamp 119 may be conveniently adjusted to adjust the position of the titration head 120, so that the titration effect is better.
The sliding block 118 comprises a block 121, two elastic clamping plates 122 and a button 123, wherein the two elastic clamping plates 122 are fixed on the block 121, the supporting rod 117 is arranged between the two elastic clamping plates 122, the button 123 is slidably connected with the block 121 and is positioned at the top of the two elastic clamping plates 122, and the bottom of the button 123 is of a triangular section. The elastic clamping plates 122 are made of an elastic material, so that the positions of the blocks 121 can be fixed by the cooperation of the two elastic clamping plates 122, and when the blocks 121 need to be moved, the buttons 123 can be pressed, so that the bottoms of the buttons 123 are inserted between the two elastic clamping plates 122 to prop the two elastic clamping plates 122 apart, thereby conveniently moving the blocks 121.
The number of the clamps 119 is plural. By providing a plurality of such clamps 119, a plurality of burettes can be placed, making use more convenient.
The acquisition board 113 includes MCU module 124, AD sampling module 125, PC communication module 126, titrator unit communication module 127, system clock 128, ferroelectric memory 129 and power conversion module 130, AD sampling module 125 with MCU module 124 is connected, PC communication module 126 with MCU module 124 is connected, titrator unit communication module 127 with MCU module 124 is connected, system clock 128 with MCU module 124 is connected, ferroelectric memory 129 with MCU module 124 is connected, power conversion module 130 with MCU module 124 is connected.
In this embodiment, the MCU employs PIC32MZ1024EFE064, the acquisition board 113 employs ADS125524 bit analog-to-digital converter, the 2 serial port communication MCU module 124 employs AT24C256C chip based on MAX232ESE, the ferroelectric memory 129 employs three voltage conversion MCU modules 124, wherein 12V to 5V employs LM2576SX-5.0 chip, 5V to 3.3V employs AMS1117-3.3 chip (for CPU power supply), and 5V to 2.5V employs ADR421BRZ.
Second embodiment
Referring to fig. 5, fig. 5 is a flowchart illustrating a method for testing a reaction endpoint based on chemical reaction enthalpy change according to a second embodiment of the present invention. On the basis of the first embodiment, the invention also provides a reaction endpoint testing method based on chemical reaction enthalpy change, which comprises the following steps:
s101, the system is powered on to carry out self-checking on each MCU module 124, and an AD sampling module 125 is sampled and calibrated;
and (3) system power-on self-checking: including serial port scanning, ferroelectric memory 129 self-test, AD sampling, timer, voltage detection, etc. And includes factory AD sampling calibration (zero and full scale).
S102, setting a titration strategy through a titrator unit communication module 127;
titration method setting:
setup: including the name of the method, the titrant component, the temperature stirring speed, the titration speed, the sampling interval, the maximum titration capacity, etc.
Inputs: temperature measurement head number, filter coefficients, etc.
Endpoints: terminal number, termination condition judgment.
Results: save and output formats.
S103, starting a titration unit 108 according to a set titration strategy, extracting detection liquid from a container bottle, and titrating through a burette;
and judging whether the second derivative of the temperature change is 0 or not according to the set dropping quantity and the set dropping speed, stopping the titration when the second derivative of the temperature change is 0, and finishing one period. And polling in turn. In the titration process, whether the second derivative of the temperature change is 0 or not is judged through the temperature data, and the titration is stopped when the second derivative of the temperature change is 0.
The S104AD sampling module 125 acquires temperature data and outputs a result table.
And when the dripping is stopped, synchronously outputting a Results report, and simultaneously, carrying out one-time pouring according to the set maximum titration capacity.
The above disclosure is only a preferred embodiment of the present invention, and it should be understood that the scope of the invention is not limited thereto, and those skilled in the art will appreciate that all or part of the procedures described above can be performed according to the equivalent changes of the claims, and still fall within the scope of the present invention.
Claims (9)
1. A reaction end point testing system based on chemical reaction enthalpy change is characterized in that,
including container subassembly, titration subassembly and detection component, container subassembly includes container lid and container bottle, the container lid sets up the top of container bottle, titration subassembly includes suction tube, valve, titration unit, connecting pipe and buret terminal, the valve sets up titration unit is last, the suction tube with the container lid with the valve is connected, the one end of connecting pipe with titration unit intercommunication, the other end of connecting pipe with buret terminal intercommunication, detection component is including placing platform, temperature sensor and collection board, place the platform setting and be in the bottom at buret terminal, temperature sensor sets up one side of placing the platform, the collection board with temperature sensor with titration unit connects.
2. A reaction endpoint test system based on chemical reaction enthalpy change according to claim 1,
the container assembly further includes a drying tube in communication with the container cover and located on one side of the container cover.
3. A reaction endpoint test system based on chemical reaction enthalpy change according to claim 2,
the drying pipe comprises a pipe body and a filter element, and the filter element is arranged in the pipe body.
4. A reaction endpoint test system based on chemical reaction enthalpy change according to claim 3,
the burette terminal comprises a supporting rod, a sliding block, a clamp and a burette, wherein the supporting rod is arranged on one side of the placing table, the sliding block is in sliding connection with the supporting rod and is positioned on one side of the supporting rod, the clamp is arranged on the sliding block, and the burette is arranged on the clamp.
5. A reaction endpoint test system based on chemical reaction enthalpy change according to claim 4,
the sliding block comprises a block body, two elastic clamping plates and a button, wherein the two elastic clamping plates are fixed on the block body, the supporting rod is arranged between the two elastic clamping plates, the button is in sliding connection with the block body and is positioned at the top of the two elastic clamping plates, and the bottom of the button is in a triangular section.
6. A reaction endpoint test system based on chemical reaction enthalpy change according to claim 5,
the number of the clamps is a plurality.
7. A reaction endpoint test system based on chemical reaction enthalpy change according to claim 6,
the acquisition board comprises an MCU module, an AD sampling module, a PC communication module, a titrator unit communication module, a system clock, a ferroelectric memory and a power conversion module, wherein the AD sampling module is connected with the MCU module, the PC communication module is connected with the MCU module, the titrator unit communication module is connected with the MCU module, the system clock is connected with the MCU module, the ferroelectric memory is connected with the MCU module, and the power conversion module is connected with the MCU module.
8. A reaction endpoint test method based on chemical reaction enthalpy change, which is applied to the reaction endpoint test system based on chemical reaction enthalpy change according to claim 7, is characterized in that,
comprising the following steps: the system is powered on to carry out self-checking on each module, and the sampling module is sampled and calibrated;
setting a titration strategy through a titrator unit communication module;
starting a titration unit according to a set titration strategy, extracting detection liquid from a container bottle, and titrating through a burette;
the AD sampling module acquires temperature data and outputs a result table.
9. A reaction endpoint test method based on chemical reaction enthalpy change according to claim 8, characterized in that,
in the titration process, whether the second derivative of the temperature change is 0 or not is judged through the temperature data, and the titration is stopped when the second derivative of the temperature change is 0.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311737120.5A CN117706026A (en) | 2023-12-15 | 2023-12-15 | Reaction end point test system based on chemical reaction enthalpy change |
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| CN202311737120.5A CN117706026A (en) | 2023-12-15 | 2023-12-15 | Reaction end point test system based on chemical reaction enthalpy change |
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