CN203123956U - Automatic derivatization reaction treatment equipment - Google Patents
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- CN203123956U CN203123956U CN 201320052394 CN201320052394U CN203123956U CN 203123956 U CN203123956 U CN 203123956U CN 201320052394 CN201320052394 CN 201320052394 CN 201320052394 U CN201320052394 U CN 201320052394U CN 203123956 U CN203123956 U CN 203123956U
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- 238000001212 derivatisation Methods 0.000 title claims abstract description 55
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- 238000012545 processing Methods 0.000 claims abstract description 11
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Abstract
本实用新型公开了一种自动衍生化反应处理设备，该设备包括N个衍生化反应单元，每个衍生化反应单元包括溶剂瓶、清洗瓶、样品瓶、反应瓶、第一控制阀、第二控制阀、第三控制阀、第一单向阀、第二单向阀、第三单向阀、第一定量泵、第二定量泵、第三定量泵、定容传感器、温度传感器、加热器、电磁搅拌器、计时器及控制模块；所述控制模块包括主控制器、阀控制器、温度控制器、搅拌控制器、时间控制器、定容传感器及泵控制器；阀控制器、温度控制器、时间控制器、定容传感器及泵控制器均与主控器相连；利用控制模块根据衍生化反应的反应过程实时控制各部件，使得整个反应过程自动完成；能够降低人工劳动强度，准确的控制衍生时间和衍生温度，使批量样品衍生化实验准确性更高，平行性更好。
The utility model discloses an automatic derivatization reaction processing equipment, which comprises N derivatization reaction units, and each derivatization reaction unit comprises a solvent bottle, a cleaning bottle, a sample bottle, a reaction bottle, a first control valve, a second Control valve, third control valve, first one-way valve, second one-way valve, third one-way valve, first quantitative pump, second quantitative pump, third quantitative pump, constant volume sensor, temperature sensor, heating device, electromagnetic stirrer, timer and control module; the control module includes a main controller, valve controller, temperature controller, stirring controller, time controller, constant volume sensor and pump controller; valve controller, temperature The controller, time controller, constant volume sensor and pump controller are all connected to the main controller; the control module is used to control the components in real time according to the reaction process of the derivatization reaction, so that the entire reaction process can be completed automatically; it can reduce the labor intensity and accurately The precise control of derivatization time and derivatization temperature makes the batch sample derivatization experiments more accurate and parallel.
Description
技术领域technical field
本实用新型涉及一种自动衍生化反应处理设备。The utility model relates to an automatic derivatization reaction processing equipment.
背景技术Background technique
衍生化是一种利用化学变换把化合物转化成类似化学结构的物质。一般来说，一个特定功能的化合物参与衍生反应，溶解度，沸点，熔点，聚集态或化学成分会产生偏离，由此产生的新的化学性质可用于量化或分离。样品衍生化的作用主要是把难于分析的物质转化为与其化学结构相似但易于分析的物质，便于量化和分离，如当检测物质无紫外吸收时，可以将其加上生色团，生成可被检测的物质。Derivatization is the use of chemical transformations to convert compounds into similar chemical structures. In general, a specific functional compound participates in a derivatization reaction, and the solubility, boiling point, melting point, aggregation state or chemical composition will be deviated, and the resulting new chemical properties can be used for quantification or isolation. The role of sample derivatization is mainly to convert difficult-to-analyze substances into substances with similar chemical structures but easy to analyze, which is convenient for quantification and separation. For example, when the detection substance has no ultraviolet absorption, it can be added with a chromophore to generate detected substance.
化学衍生法在仪器分析中被广泛应用。气相色谱中应用化学衍生反应是为了增加样品的挥发度或提高检测灵敏度，而高效液相色谱的化学衍生法是指在一定条件下利用某种试剂(通称化学衍生试剂或标记试剂)与样品组份进行化学反应，反应的产物有利于色谱检测或分离。一般化学衍生法主要有以下几个目的：提高样品检测的灵敏度；改善样品混合物的分离度；适合于进一步做结构鉴定，如质谱、红外或核磁共振等。进行化学衍生反应应该满足如下要求：对反应条件要求不苛刻，且能迅速、定量地进行；对样品中的某个组份只生成一种衍生物，反应副产物及过量的衍生试剂不干扰被测样品的分离和检测；化学衍生试剂方便易得，通用性好。Chemical derivatization is widely used in instrumental analysis. The application of chemical derivatization reaction in gas chromatography is to increase the volatility of the sample or improve the detection sensitivity, while the chemical derivatization method of high performance liquid chromatography refers to the use of certain reagents (commonly known as chemical derivatization reagents or labeling reagents) and sample groups under certain conditions. Parts undergo a chemical reaction, and the product of the reaction is beneficial to chromatographic detection or separation. The general chemical derivatization method mainly has the following purposes: to improve the sensitivity of sample detection; to improve the resolution of sample mixture; to be suitable for further structural identification, such as mass spectrometry, infrared or nuclear magnetic resonance, etc. The chemical derivatization reaction should meet the following requirements: the reaction conditions are not harsh, and can be carried out quickly and quantitatively; only one derivative is generated for a certain component in the sample, and the reaction by-products and excessive derivatization reagents do not interfere with the derivatization. Separation and detection of test samples; chemical derivatization reagents are convenient and easy to obtain, and have good versatility.
目前，实验室常用的衍生化反应器具有容量瓶、水浴锅等，在进行普通的衍生化试验时存在以下一些问题：1、容量瓶的目视定容会造成体积误差，或者因容量瓶质量问题引起定容误差；2、水浴锅在批量样品的衍生过程中，温度控制会有一定的偏差，并且无法实现100℃以上的衍生化反应；3、在批量样品衍生过程中，由于人为原因（如操作时间、计时误差等）引起各个样品的衍生过程不尽相同，存在实验误差；4、衍生化反应易受操作人员水平的影响。At present, the derivatization reactors commonly used in the laboratory include volumetric flasks, water baths, etc., and there are some problems in the following general derivatization experiments: 1. The visual volumetric volume of the volumetric flask will cause volume errors, or the quality of the volumetric flask The problem caused constant volume error; 2. During the derivation process of batch samples, the temperature control of the water bath will have a certain deviation, and the derivatization reaction above 100°C cannot be realized; 3. During the derivation process of batch samples, due to human reasons ( Such as operating time, timing error, etc.) cause the derivation process of each sample to be different, and there are experimental errors; 4. The derivatization reaction is easily affected by the level of the operator.
因此，为降低衍生化反应的实验误差，急需提供一种自动化的衍生反应设备，能够准确的控制衍生时间、衍生温度，使批量样品衍生化实验准确性更高，平行性更好。Therefore, in order to reduce the experimental error of the derivatization reaction, it is urgent to provide an automated derivatization reaction equipment that can accurately control the derivatization time and derivatization temperature, so that the derivatization experiment of batch samples has higher accuracy and better parallelism.
实用新型内容Utility model content
本实用新型一种自动衍生化反应处理设备，其目的在于提供一种自动化、程序化的化学衍生化反应处理设备，克服现有技术中人工进行分析检测实验的准确性和工作效率不高的问题。The utility model is an automatic derivatization reaction processing equipment, and its purpose is to provide an automatic and programmed chemical derivation reaction processing equipment, which overcomes the problems of low accuracy and low work efficiency of manual analysis and detection experiments in the prior art .
一种自动衍生化反应处理设备，包括N个衍生化反应单元，衍生化反应单元并联连接，每个衍生化反应单元包括溶剂瓶、清洗瓶、样品瓶、反应瓶、第一控制阀、第二控制阀、第三控制阀、第一单向阀、第二单向阀、第三单向阀、第一定量泵、第二定量泵、第三定量泵、定容传感器、温度传感器、加热器、电磁搅拌器、计时器及控制模块；An automatic derivatization reaction processing equipment, including N derivatization reaction units, the derivatization reaction units are connected in parallel, and each derivatization reaction unit includes a solvent bottle, a cleaning bottle, a sample bottle, a reaction bottle, a first control valve, a second Control valve, third control valve, first one-way valve, second one-way valve, third one-way valve, first quantitative pump, second quantitative pump, third quantitative pump, constant volume sensor, temperature sensor, heating device, electromagnetic stirrer, timer and control module;
所述控制模块包括主控制器、阀控制器、温度控制器、搅拌控制器、时间控制器、定容传感器及泵控制器；阀控制器、温度控制器、时间控制器、定容传感器及泵控制器均与主控器相连；其中N为大于或等于1的整数；The control module includes a main controller, a valve controller, a temperature controller, a stirring controller, a time controller, a constant volume sensor and a pump controller; a valve controller, a temperature controller, a time controller, a constant volume sensor and a pump The controllers are all connected to the main controller; where N is an integer greater than or equal to 1;
其中，阀控制器用于控制第一控制阀、第二控制阀、第三控制阀、第一单向阀、第二单向阀及第三单向阀的阀控制器；Wherein, the valve controller is a valve controller used to control the first control valve, the second control valve, the third control valve, the first check valve, the second check valve and the third check valve;
温度控制器用于控制加热器；The temperature controller is used to control the heater;
搅拌控制器用于控制电磁搅拌器；The stirring controller is used to control the electromagnetic stirrer;
泵控制器用于控制第一定量泵、第二定量泵及第三定量泵的泵控制器；The pump controller is used to control the pump controller of the first quantitative pump, the second quantitative pump and the third quantitative pump;
其中，第一控制阀和第二控制阀均为三通控制阀，第三控制阀为二通控制阀；Wherein, the first control valve and the second control valve are three-way control valves, and the third control valve is a two-way control valve;
所述溶剂瓶、第一单向阀、第一定量泵、第一控制阀及反应瓶依次通过管路连接；The solvent bottle, the first one-way valve, the first quantitative pump, the first control valve and the reaction bottle are sequentially connected through pipelines;
所述清洗瓶和样品瓶均与第二控制阀相连，第二控制阀、第二单向阀、第二定量泵及反应瓶依次通过管路连接；Both the cleaning bottle and the sample bottle are connected to the second control valve, and the second control valve, the second one-way valve, the second quantitative pump and the reaction bottle are sequentially connected through pipelines;
所述反应瓶、第三单向阀、第三定量泵及检测装置依次通过管路连接；The reaction bottle, the third one-way valve, the third quantitative pump and the detection device are sequentially connected through pipelines;
所述反应瓶还通过管路与第三控制阀相连；The reaction bottle is also connected to the third control valve through a pipeline;
所述反应瓶上设有定容传感器及温度传感器，加热器及电磁搅拌器均设于反应瓶底部。The reaction bottle is provided with a constant volume sensor and a temperature sensor, and a heater and an electromagnetic stirrer are arranged at the bottom of the reaction bottle.
所述溶剂瓶数量为M个，M为大于或等于1的整数，当M大于或等于2时，溶剂瓶之间通过第一混合阀连通，第一混合阀与第一单向阀相连。The number of solvent bottles is M, and M is an integer greater than or equal to 1. When M is greater than or equal to 2, the solvent bottles are connected through the first mixing valve, and the first mixing valve is connected with the first one-way valve.
所述的清洗瓶数量为P个，P为整数大于或等于1的，当P大于或等于2时，清洗瓶之间通过第二混合阀连通，第二混合阀与第二控制阀相连。The number of cleaning bottles is P, and P is an integer greater than or equal to 1. When P is greater than or equal to 2, the cleaning bottles are connected through the second mixing valve, and the second mixing valve is connected with the second control valve.
所述管路为PEEK管。The pipeline is a PEEK tube.
有益效果Beneficial effect
本实用新型提供了一种自动衍生化反应处理设备，该设备包括N个衍生化反应单元，衍生化反应单元并联连接，每个衍生化反应单元包括溶剂瓶、清洗瓶、样品瓶、反应瓶、第一控制阀、第二控制阀、第三控制阀、第一单向阀、第二单向阀、第三单向阀、第一定量泵、第二定量泵、第三定量泵、定容传感器、温度传感器、加热器、电磁搅拌器、计时器及控制模块；所述控制模块包括主控制器、阀控制器、温度控制器、搅拌控制器、时间控制器、定容传感器及泵控制器；阀控制器、温度控制器、时间控制器、定容传感器及泵控制器均与主控器相连；其中N为大于或等于1的整数；其中，阀控制器用于控制第一控制阀、第二控制阀、第三控制阀、第一单向阀、第二单向阀及第三单向阀的阀控制器；温度控制器用于控制加热器；搅拌控制器用于控制电磁搅拌器；泵控制器用于控制第一定量泵、第二定量泵及第三定量泵的泵控制器；该装置结构简单，容易实现，适宜批量化进行衍生化反应；利用控制模块根据衍生化反应的反应过程实时控制各部件，使得整个反应过程自动完成；利用定量泵，使得衍生化反应过程中能够定量抽取溶液，减小批量生产中反应过程中的误差；采用定容传感器提高定容精度；采用自动衍生化反应前处理设备及方法，能够降低人工劳动强度，准确的控制衍生时间和衍生温度，使批量样品衍生化实验准确性更高，平行性更好。The utility model provides an automatic derivatization reaction processing equipment, which comprises N derivatization reaction units connected in parallel, and each derivatization reaction unit includes a solvent bottle, a cleaning bottle, a sample bottle, a reaction bottle, The first control valve, the second control valve, the third control valve, the first one-way valve, the second one-way valve, the third one-way valve, the first quantitative pump, the second quantitative pump, the third quantitative pump, the constant Capacitance sensor, temperature sensor, heater, electromagnetic stirrer, timer and control module; the control module includes main controller, valve controller, temperature controller, stirring controller, time controller, constant volume sensor and pump control controller; valve controller, temperature controller, time controller, constant volume sensor and pump controller are all connected to the main controller; wherein N is an integer greater than or equal to 1; wherein, the valve controller is used to control the first control valve, The valve controllers of the second control valve, the third control valve, the first one-way valve, the second one-way valve and the third one-way valve; the temperature controller is used to control the heater; the stirring controller is used to control the electromagnetic stirrer; the pump The controller is used to control the pump controller of the first quantitative pump, the second quantitative pump and the third quantitative pump; the device has a simple structure, is easy to implement, and is suitable for derivatization reactions in batches; Real-time control of each component enables the entire reaction process to be completed automatically; the quantitative pump is used to quantitatively extract the solution during the derivatization reaction, reducing the error in the reaction process in mass production; the constant volume sensor is used to improve the constant volume accuracy; the automatic derivatization is adopted The pretreatment equipment and method of the chemical reaction can reduce the labor intensity, accurately control the derivatization time and temperature, and make the batch sample derivatization experiment more accurate and parallel.
附图说明Description of drawings
图1为本实用新型的电气控制结构图；Fig. 1 is the electrical control structural diagram of the utility model;
图2为本实用新型的工作单元机械结构图；Fig. 2 is the mechanical structure diagram of the working unit of the present utility model;
图3为本实用新型的工作流程示意图。Fig. 3 is a schematic diagram of the workflow of the utility model.
具体实施方式Detailed ways
下面将结合附图对本实用新型做进一步说明，以6个工作单元为例。The utility model will be further described below in conjunction with the accompanying drawings, taking 6 working units as an example.
如图1和图2所示，一种自动衍生化反应处理设备，包括6个衍生化反应单元，每个衍生化反应单元包括溶剂瓶、清洗瓶、样品瓶、反应瓶、第一控制阀、第二控制阀、第三控制阀、第一单向阀、第二单向阀、第三单向阀、第一定量泵、第二定量泵、第三定量泵、定容传感器、温度传感器、加热器、电磁搅拌器、计时器及控制模块；所述控制模块包括主控制器，用于控制第一控制阀、第二控制阀、第三控制阀、第一单向阀、第二单向阀及第三单向阀的阀控制器，用于控制加热器的温度控制器，用于控制电磁搅拌器的搅拌控制器，时间控制器、定容传感器及控制第一定量泵、第二定量泵及第三定量泵的泵控制器；阀控制器、温度控制器、时间控制器、定容传感器及泵控制器均与主控器相连；As shown in Figure 1 and Figure 2, an automatic derivatization reaction processing equipment includes 6 derivatization reaction units, each derivatization reaction unit includes a solvent bottle, a cleaning bottle, a sample bottle, a reaction bottle, a first control valve, The second control valve, the third control valve, the first one-way valve, the second one-way valve, the third one-way valve, the first quantitative pump, the second quantitative pump, the third quantitative pump, constant volume sensor, temperature sensor , a heater, an electromagnetic stirrer, a timer and a control module; the control module includes a main controller for controlling the first control valve, the second control valve, the third control valve, the first check valve, the second check valve The valve controller of the one-way valve and the third one-way valve, the temperature controller used to control the heater, the stirring controller used to control the electromagnetic stirrer, the time controller, the constant volume sensor and the first quantitative pump, the second The pump controllers of the second quantitative pump and the third quantitative pump; valve controllers, temperature controllers, time controllers, constant volume sensors and pump controllers are all connected to the main controller;
其中，第一控制阀和第二控制阀为三通控制阀，第三控制阀为二通控制阀；Wherein, the first control valve and the second control valve are three-way control valves, and the third control valve is a two-way control valve;
所述溶剂瓶包括溶剂瓶A和溶剂瓶B，溶剂瓶A和溶剂瓶B均与第一混合阀相连，第一混合阀、第一单向阀、第一定量泵、第一控制阀与反应瓶依次通过管路相连；Described solvent bottle comprises solvent bottle A and solvent bottle B, and solvent bottle A and solvent bottle B are all connected with the first mixing valve, and the first mixing valve, the first one-way valve, the first quantitative pump, the first control valve and The reaction bottles are connected sequentially through pipelines;
所述清洗瓶和样品瓶均通过管路依次与第二控制阀、第二单向阀及第二定量泵相连至反应瓶；其中，清洗瓶包括清洗瓶C和清洗瓶D，清洗瓶C和清洗瓶D均与第二混合阀相连，第二混合阀与第二控制阀相连；Both the cleaning bottle and the sample bottle are connected to the reaction bottle with the second control valve, the second one-way valve and the second quantitative pump in sequence through pipelines; wherein, the cleaning bottle includes cleaning bottle C and cleaning bottle D, cleaning bottle C and The cleaning bottles D are all connected to the second mixing valve, and the second mixing valve is connected to the second control valve;
所述反应瓶通过管路依次与第三单向阀及第三定量泵相连至检测装置；The reaction bottle is sequentially connected to the detection device through the pipeline with the third one-way valve and the third quantitative pump;
所述反应瓶还通过管路与第三控制阀相连；The reaction bottle is also connected to the third control valve through a pipeline;
所述反应瓶上设有定容传感器及温度传感器，加热器及电磁搅拌器均设于反应瓶底端。The reaction bottle is provided with a constant volume sensor and a temperature sensor, and a heater and an electromagnetic stirrer are arranged at the bottom of the reaction bottle.
基于上述设备的工作过程如下：The working process based on the above equipment is as follows:
步骤1：打开第一单向阀，启动第一定量泵，用溶剂瓶中的衍生液A或B或AB润洗一遍溶剂瓶与第一定量泵之间的管路；Step 1: Open the first one-way valve, start the first quantitative pump, and rinse the pipeline between the solvent bottle and the first quantitative pump with the derivative liquid A or B or AB in the solvent bottle;
步骤2：启动第二定量泵，第二控制阀选通样品瓶与第二单向阀之间的管路，抽取2ml样品溶液至反应瓶，第一定量泵抽取5ml衍生溶液至反应瓶后关闭第一控制阀；Step 2: Start the second quantitative pump, the second control valve gates the pipeline between the sample bottle and the second one-way valve, draw 2ml of sample solution to the reaction bottle, and the first quantitative pump draws 5ml of derivative solution to the reaction bottle closing the first control valve;
步骤3：利用温度传感器控制加热器使反应瓶中溶液温度升至设定温度，然后启动计时器计时至设定时间，搅拌控制器启动电磁搅拌器工作；Step 3: Use the temperature sensor to control the heater to raise the temperature of the solution in the reaction bottle to the set temperature, then start the timer to count to the set time, and the stirring controller starts the electromagnetic stirrer to work;
步骤4：待计时器的设定时间到即衍生化反应完成时，计时器、加热器和搅拌器停止工作，让衍生后的溶液冷却至室温；Step 4: When the set time of the timer is up, that is, when the derivatization reaction is completed, the timer, heater and stirrer are stopped, and the derivatized solution is allowed to cool to room temperature;
步骤5：启动定容传感器，将反应瓶中的反应溶液定容至设定容积10ml，剩余反应溶液通过第一控制阀排出，若反应瓶中反应溶液容积小于设定容积，则打开第一控制阀，通过第二定量泵抽取衍生液至反应瓶定容至10ml，启动搅拌器搅拌时间T，其中T为10秒；Step 5: Start the constant volume sensor, set the reaction solution in the reaction bottle to a set volume of 10ml, and the remaining reaction solution is discharged through the first control valve. If the volume of the reaction solution in the reaction bottle is less than the set volume, open the first control valve. Valve, extract the derivative liquid through the second quantitative pump to the reaction bottle and set the volume to 10ml, start the stirrer for stirring time T, wherein T is 10 seconds;
步骤6：启动第三定量泵，定量抽取2ml衍生后的溶液至检测装置中；Step 6: start the third quantitative pump, and quantitatively draw 2ml of the derivatized solution into the detection device;
步骤7：管道清洗，打开第三控制阀，将剩余衍生反应后溶液排出，第二控制阀选通清洗管路，第二定量泵抽取清洗溶液C或D或CD清洗第二控制阀至第三控制阀之间的管路后关闭第三控制阀。Step 7: Pipeline cleaning, open the third control valve, discharge the remaining derivatization reaction solution, the second control valve selects the cleaning pipeline, and the second quantitative pump pumps the cleaning solution C or D or CD to clean the second control valve to the third Close the third control valve after the pipeline between the control valves.
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