CN114527225A - Wide-range rapid constant-temperature chromatographic column box - Google Patents
Wide-range rapid constant-temperature chromatographic column box Download PDFInfo
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- CN114527225A CN114527225A CN202210169007.0A CN202210169007A CN114527225A CN 114527225 A CN114527225 A CN 114527225A CN 202210169007 A CN202210169007 A CN 202210169007A CN 114527225 A CN114527225 A CN 114527225A
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- chromatographic column
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/50—Conditioning of the sorbent material or stationary liquid
- G01N30/52—Physical parameters
- G01N30/54—Temperature
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Abstract
The invention discloses a wide-range fast constant-temperature chromatographic column box which comprises semiconductor wafers, radiating fins, a metal block body for fixing a chromatographic column, an over-temperature protector, a fan, a temperature sensor, a main board and a DC power supply, wherein the semiconductor wafers are uniformly distributed on the metal block body for fixing the chromatographic column and are embedded in connecting groove holes of the metal block body for fixing the chromatographic column, the radiating fins are positioned on one side of the semiconductor wafers on the metal block body for fixing the chromatographic column and are locked and fixed on the metal block body for fixing the chromatographic column through screws, and the fan is fixed on one side of the metal block body for fixing the chromatographic column. The column box adopts the H-bridge drive circuit to control the semiconductor wafer, improves the temperature stabilizing speed on the basis of accurate and stable temperature control, widens the temperature control range, greatly improves the working efficiency of the liquid chromatographic analysis system due to the rapid temperature stabilization, and widens the temperature control range, so that the application range of the liquid chromatographic analysis system is wider.
Description
Technical Field
The invention relates to the technical field of liquid chromatographic analysis equipment, in particular to a wide-range rapid constant-temperature chromatographic column box.
Background
In a liquid chromatographic analysis system, because the chromatographic column thermostat can accurately and stably control the service temperature of a chromatographic column, the chromatographic column thermostat has a non-negligible effect on improving the column efficiency of the chromatographic column, improving the separation degree of chromatographic peaks, shortening the retention time, reducing back pressure and ensuring the repeatability of sample analysis results, so that the column thermostat is an important matching device of a liquid chromatograph.
At present, column thermostats in the market mostly use silicon controlled rectifiers to drive heating rods to heat, the time for heating and temperature stabilization is not ideal, only heating does not have a refrigeration function, and samples needing low-temperature analysis cannot meet the requirements.
Disclosure of Invention
The invention aims to provide a wide-range fast constant-temperature chromatographic column box, which aims to solve the problems that 1. silicon controlled rectifier drives a heating rod to heat, and the heating and temperature stabilizing time cannot achieve the optimal effect; 2. the controllable silicon drives the heating rod, and only heating does not have a refrigerating function, and the problems of functionality and practicability are lacked.
In order to achieve the purpose, the invention provides the following technical scheme:
a wide-range fast constant-temperature chromatographic column box comprises a semiconductor wafer, a heat sink, a metal block for fixing a chromatographic column, an over-temperature protector, a fan, a temperature sensor, a main board and a DC power supply, the semiconductor wafers are uniformly distributed on the metal block body of the fixed chromatographic column and are embedded in the connecting groove holes of the metal block body of the fixed chromatographic column, the radiating fin is positioned on one side of the semiconductor chip on the metal block body of the fixed chromatographic column and is locked and fixed on the metal block body of the fixed chromatographic column through screws, a fan is fixed on one side of the metal block body for fixing the chromatographic column, an over-temperature protector is fixed on the top of the metal block body for fixing the chromatographic column, the temperature sensor is arranged in a metal block body of the fixed chromatographic column, the temperature sensor and the DC power supply are connected with the mainboard through wires, and the mainboard is provided with a communication port, an H-bridge driving circuit and an MCU.
In a preferred embodiment of the present invention, the semiconductor dice are provided in four groups, each of the semiconductor dice is formed of a thermocouple pair composed of an N-type semiconductor and a P-type semiconductor, and the semiconductor dice are connected in series to a lead wire and connected to an H-bridge driving circuit.
As a preferred embodiment of the present invention, the H-bridge driving circuit is provided with a heating control terminal and a cooling control terminal, and the heating control terminal and the cooling control terminal are connected to pins of the MCU through a circuit.
In a preferred embodiment of the present invention, a heat sink is disposed on the fitting end surface of the semiconductor wafer, the heat sink is made of metal aluminum, the metal aluminum is fixed to the engaging surface of the connecting slot of the metal block for fixing the chromatographic column by screws, and the outer end surface of the semiconductor wafer is coated with heat-conductive silicone grease.
In a preferred embodiment of the present invention, the over-temperature protector is a normally closed self-recovery temperature-controlled switch, and the over-temperature protector is connected in series to the power supply line of the semiconductor chip.
As a preferred embodiment of the present invention, the fan is fixed to one side end of the metal block for fixing the chromatography column by screws, and a driving motor of the fan is connected to a pin of the MCU by a circuit.
In a preferred embodiment of the present invention, the temperature sensor is fixed in one side of the metal block body of the stationary chromatographic column by a heat conductive silica gel, and the temperature sensor is connected with the pin of the MCU by a wire.
Compared with the prior art, the invention has the beneficial effects that:
1. the column box adopts the H-bridge drive circuit to control the semiconductor wafer, improves the temperature stabilizing speed on the basis of accurate and stable temperature control, widens the temperature control range, greatly improves the working efficiency of the liquid chromatographic analysis system due to the rapid temperature stabilization, and widens the temperature control range, so that the application range of the liquid chromatographic analysis system is wider.
2. The semiconductor wafer of the column box utilizes the Peltier effect between the N-type semiconductor and the P-type semiconductor which are connected together, and realizes refrigeration and heating by carrying out energy exchange in motion through electron-hole.
Drawings
FIG. 1 is a schematic view of the overall structure of the column box of the present invention;
FIG. 2 is a schematic diagram of the heating/cooling of a semiconductor wafer according to the present invention;
FIG. 3 is a schematic diagram of an H-bridge driving circuit according to the present invention;
fig. 4 is a diagram of the overall working frame of the column box of the present invention.
In the figure: 1-semiconductor chip, 2-heat sink, 3-metal block for fixing chromatographic column, 4-over-temperature protector, 5-fan and 6-temperature sensor.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
Referring to fig. 1-4, the present invention provides a technical solution:
a wide-range fast constant-temperature chromatographic column box comprises a semiconductor wafer 1, a radiating fin 2, a metal block 3 for fixing a chromatographic column, an over-temperature protector 4, a fan 5, a temperature sensor 6, a mainboard and a DC power supply, wherein the semiconductor wafer 1 is uniformly distributed on the metal block 3 for fixing the chromatographic column and is embedded in a connecting groove hole of the metal block 3 for fixing the chromatographic column, the radiating fin 2 is positioned on one side of the semiconductor wafer 1 on the metal block 3 for fixing the chromatographic column, the radiating fin 2 is locked and fixed on the metal block 3 for fixing the chromatographic column through a screw, the fan 5 is fixed on one side of the metal block 3 for fixing the chromatographic column, the over-temperature protector 4 is fixed at the top of the metal block 3 for fixing the chromatographic column, the over-temperature protector 4 is a normally closed self-recovery temperature control switch, the over-temperature protector 4 is connected on a power supply lead of the semiconductor wafer 1 in series, the temperature sensor 6 is arranged in the metal block 3 for fixing the chromatographic column, the temperature sensor 6 and the DC power supply are connected with a mainboard through wires, and the mainboard is provided with a communication port, an H-bridge drive circuit and an MCU.
Four groups of semiconductor wafers 1 are arranged, each semiconductor wafer 1 is composed of a thermocouple pair composed of an N-type semiconductor and a P-type semiconductor, the semiconductor wafers 1 are connected in series on a lead and connected with an H-bridge driving circuit, a semiconductor refrigeration wafer utilizes the Peltier effect between the N-type semiconductor and the P-type semiconductor which are connected together, and realizes refrigeration and heating by energy exchange in the motion of electrons and holes, as shown in figure 2, the P-type semiconductor and the N-type semiconductor are connected in series to form a thermocouple pair loop, a direct current power supply is added at two ends of the loop, two ends of the thermocouple can respectively absorb heat and emit heat under the action of an external electric field, one surface of the semiconductor refrigeration wafer is attached to a load surface needing to be heated and refrigerated, and the heating and refrigerating purposes can be achieved by controlling the voltage directions at two ends of the loop.
The H-bridge driving circuit is provided with a heating control end and a refrigerating control end, the heating control end and the refrigerating control end are connected with pins of the MCU through circuits, the H-bridge driving circuit realizes the control of the semiconductor refrigerating sheet by adjusting circuit parameters, as shown in figure 3, HOT and COOL in the figure are respectively a heating end and a refrigerating end, the PWM function of a PWM converter on a pin of the single chip Microcomputer (MCU) is utilized to control the on-off of Q1, Q2, Q5 and Q6 four MOSFETs, thereby controlling the positive and negative of voltage between Peltier A and Peltier B, reversing the current flowing through the semiconductor sheet, realizing the heating and refrigerating functions of the semiconductor sheet, and regulating the current flowing through the semiconductor sheet by utilizing the PWM function and a PID algorithm to realize accurate temperature control.
The heat radiator is mainly used for cooling the semiconductor wafer 1 and rapidly dissipating heat on one side of the semiconductor wafer 1, so that the temperature difference between two sides of the semiconductor wafer 1 is not too large, P, N semiconductors are protected, the heat-conducting silicone grease takes organic silicone as a main raw material, and materials with excellent heat resistance and heat conductivity are added for heat conduction and heat dissipation of the semiconductor wafer 1.
The over-temperature protector 4 is a normally closed self-recovery temperature control switch, the over-temperature protector 4 is connected in series on a power supply lead of the semiconductor wafer 1, when the temperature exceeds the highest temperature of the column box, the over-temperature protector 4 is automatically disconnected, namely, the power supply of the semiconductor wafer 1 is disconnected, and when the temperature is lower than the highest temperature of the column box, the over-temperature protector 4 is closed, namely, the power supply of the semiconductor wafer 1 is recovered, so that the semiconductor wafer can be protected from being damaged, and the chromatographic column can be protected from being burnt out by high temperature.
Fan 5 passes through the one side end of the metal block 3 of screw fixation chromatographic column, and fan 5's driving motor passes through the circuit and is connected with MCU's pin, and the fan mainly prevents work when the low temperature state, produces the comdenstion water, through MCU to the judgement of temperature to the executive control who opens and stop it.
In the system, the MCU converses with the upper computer through a communication port to realize the reverse control of the upper computer on the column box, such as temperature setting, temperature display, PID self-setting, error alarm and the like, the MCU controls the H-bridge drive circuit through a PID algorithm to realize accurate temperature control, the MCU and the H-bridge drive circuit are supplied with power through a DC power supply (24V), a temperature sensor on the column box directly transmits a temperature signal monitored in real time to the MCU, the MCU accurately drives the on-off time of a hot end and a cold end of the H-bridge through comparing the set temperature and the real-time temperature to realize accurate temperature control, an over-temperature protector on the column box monitors the highest temperature which the column box can bear, and when the temperature is too high, the over-temperature protector can automatically cut off to cut off the power supply of the semiconductor wafer, when the temperature is lower than the highest temperature, the over-temperature protector can be automatically closed, and the power supply of the semiconductor wafer is recovered; when the temperature is lower, the MCU starts the fan to prevent the generation of condensed water when the MCU works in a low-temperature state.
Example two
The utility model provides a chromatographic column case, including the metal block of fixed chromatographic column, the heating rod, DC power and silicon controlled rectifier pressure regulating control circuit, the heating rod passes through the both sides of the metal block of screw fixation in fixed chromatographic column, the heating rod passes through power line and silicon controlled rectifier pressure regulating control circuit's circuit articulate, silicon controlled rectifier pressure regulating control circuit's communication port passing signal line is connected with the communication articulate of external host computer, this column case mainly drives the heating rod through silicon controlled rectifier pressure regulating control circuit, the mode of voltage size regulation and control to silicon controlled rectifier pressure regulating control circuit with the help of the host computer simultaneously, adjust the heating temperature of heating rod, thereby realize the regulation and control of temperature.
The following table shows the functions and various indexes of the chromatographic column box and the traditional chromatographic column box in comparison and analysis:
to above-mentioned two kinds of different post casees, through last respectively to safety, the function, the programming rate, accuse temperature time, accuse temperature range, accuse temperature characteristic and radiating efficiency carry out the analysis and reachs, this post case compares most obvious advantage with traditional post case is that this post case has cold/hot temperature control and safety protection function, control temperature time and control by temperature change scope will be superior to traditional post case simultaneously, under the condition of considering the cost, because the increase of this post case functional component and temperature control subassembly, therefore, the cost will be a little higher than traditional post case, but compare from comprehensive aspect, the price/performance ratio of this post case will be higher than traditional post case.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. The utility model provides a wide range quick homothermal chromatographic column case which characterized in that: the device comprises a semiconductor wafer (1), a radiating fin (2), a metal block body (3) for fixing a chromatographic column, an over-temperature protector (4), a fan (5), a temperature sensor (6), a mainboard and a DC power supply, wherein the semiconductor wafer (1) is uniformly distributed on the metal block body (3) for fixing the chromatographic column and is embedded in a connecting groove hole of the metal block body (3) for fixing the chromatographic column, the radiating fin (2) is positioned on one side of the semiconductor wafer (1) on the metal block body (3) for fixing the chromatographic column and is fixedly locked on the metal block body (3) for fixing the chromatographic column through screws, the fan (5) is fixed on one side of the metal block body (3) for fixing the chromatographic column, the over-temperature protector (4) is fixed at the top of the metal block body (3) for fixing the chromatographic column, and the temperature sensor (6) is arranged in the metal block body (3) for fixing the chromatographic column, the temperature sensor (6) and the DC power supply are connected with a mainboard through wires, and a communication port, an H-bridge driving circuit and an MCU are arranged on the mainboard.
2. A wide range rapid thermostatted chromatography column box as claimed in claim 1, characterized in that: the semiconductor wafer (1) is provided with four groups, the semiconductor wafer (1) is composed of thermocouple pairs consisting of an N-type semiconductor and a P-type semiconductor, and the semiconductor wafer (1) is connected in series on a lead and is connected with an H-bridge driving circuit.
3. A wide range rapid thermostatted chromatography column box as claimed in claim 1, characterized in that: and the H-bridge drive circuit is provided with a heating control end and a refrigerating control end, and the heating control end and the refrigerating control end are connected with pins of the MCU through circuits.
4. A wide range rapid thermostatted chromatography column box as claimed in claim 1, characterized in that: the embedded end face of the semiconductor wafer (1) is provided with a radiator, the radiator is made of metal aluminum, the metal aluminum is fixed on the connection face of the connection groove hole of the metal block (3) of the fixed chromatographic column through screws, and heat-conducting silicone grease is coated on the end face of the outer side of the semiconductor wafer (1).
5. A wide range rapid isothermal chromatography column cassette as claimed in claim 1, characterized in that: the over-temperature protector (4) is a normally closed self-recovery temperature control switch, and the over-temperature protector (4) is connected in series with a power supply lead of the semiconductor wafer (1).
6. A wide range rapid thermostatted chromatography column box as claimed in claim 1, characterized in that: the fan (5) is fixed at one side end of the metal block body (3) for fixing the chromatographic column through screws, and a driving motor of the fan (5) is connected with pins of the MCU through a circuit.
7. A wide range rapid thermostatted chromatography column box as claimed in claim 1, characterized in that: the temperature sensor (6) is fixed in one side of the metal block body (3) of the fixed chromatographic column through heat-conducting silica gel, and the temperature sensor (6) is connected with a pin of the MCU through a circuit.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210169007.0A CN114527225A (en) | 2022-02-23 | 2022-02-23 | Wide-range rapid constant-temperature chromatographic column box |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210169007.0A CN114527225A (en) | 2022-02-23 | 2022-02-23 | Wide-range rapid constant-temperature chromatographic column box |
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| Publication Number | Publication Date |
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| CN114527225A true CN114527225A (en) | 2022-05-24 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202210169007.0A Pending CN114527225A (en) | 2022-02-23 | 2022-02-23 | Wide-range rapid constant-temperature chromatographic column box |
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20090106029A (en) * | 2008-04-04 | 2009-10-08 | 포항공과대학교 산학협력단 | Temperature control device for liquid chromatography column and high performance liquid chromatography apparatus using the same |
| CN104034831A (en) * | 2014-06-08 | 2014-09-10 | 华东理工大学 | Super-long protein and polypeptide separation capillary liquid chromatography column system with automatic temperature control |
| CN204330698U (en) * | 2014-12-24 | 2015-05-13 | 江苏汉邦科技有限公司 | A kind of thermostat being applied to supercritical fluid chromatography system |
| CN205561330U (en) * | 2016-04-25 | 2016-09-07 | 青岛科技大学 | Quick constant temperature control box of small -size semiconductor high accuracy |
| CN206420838U (en) * | 2017-01-17 | 2017-08-18 | 广州市锦泉仪器科技有限公司 | The semiconductor that a kind of column oven for making liquid chromatograph cools |
| CN209803069U (en) * | 2019-04-16 | 2019-12-17 | 无锡赛那尔仪器设备制造有限公司 | Temperature control system for column oven of liquid chromatograph |
| CN211505359U (en) * | 2019-11-14 | 2020-09-15 | 无锡赛那尔仪器设备制造有限公司 | Column oven with circulating air duct |
| CN113567599A (en) * | 2021-07-22 | 2021-10-29 | 上海天美科学仪器有限公司 | Efficient and stable heat dissipation system for temperature-controllable device |
| CN113587531A (en) * | 2021-07-22 | 2021-11-02 | 上海天美科学仪器有限公司 | Mechanism for solving condensate water generated during refrigeration of temperature control device |
| CN215812599U (en) * | 2021-08-04 | 2022-02-11 | 兰州东立龙信息技术有限公司 | Capillary chromatographic column stationary liquid low-temperature coating device |
-
2022
- 2022-02-23 CN CN202210169007.0A patent/CN114527225A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20090106029A (en) * | 2008-04-04 | 2009-10-08 | 포항공과대학교 산학협력단 | Temperature control device for liquid chromatography column and high performance liquid chromatography apparatus using the same |
| CN104034831A (en) * | 2014-06-08 | 2014-09-10 | 华东理工大学 | Super-long protein and polypeptide separation capillary liquid chromatography column system with automatic temperature control |
| CN204330698U (en) * | 2014-12-24 | 2015-05-13 | 江苏汉邦科技有限公司 | A kind of thermostat being applied to supercritical fluid chromatography system |
| CN205561330U (en) * | 2016-04-25 | 2016-09-07 | 青岛科技大学 | Quick constant temperature control box of small -size semiconductor high accuracy |
| CN206420838U (en) * | 2017-01-17 | 2017-08-18 | 广州市锦泉仪器科技有限公司 | The semiconductor that a kind of column oven for making liquid chromatograph cools |
| CN209803069U (en) * | 2019-04-16 | 2019-12-17 | 无锡赛那尔仪器设备制造有限公司 | Temperature control system for column oven of liquid chromatograph |
| CN211505359U (en) * | 2019-11-14 | 2020-09-15 | 无锡赛那尔仪器设备制造有限公司 | Column oven with circulating air duct |
| CN113567599A (en) * | 2021-07-22 | 2021-10-29 | 上海天美科学仪器有限公司 | Efficient and stable heat dissipation system for temperature-controllable device |
| CN113587531A (en) * | 2021-07-22 | 2021-11-02 | 上海天美科学仪器有限公司 | Mechanism for solving condensate water generated during refrigeration of temperature control device |
| CN215812599U (en) * | 2021-08-04 | 2022-02-11 | 兰州东立龙信息技术有限公司 | Capillary chromatographic column stationary liquid low-temperature coating device |
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