CN103100363B - Automatic derivatization reaction processing equipment and method - Google Patents
Automatic derivatization reaction processing equipment and method Download PDFInfo
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- CN103100363B CN103100363B CN201310036043.0A CN201310036043A CN103100363B CN 103100363 B CN103100363 B CN 103100363B CN 201310036043 A CN201310036043 A CN 201310036043A CN 103100363 B CN103100363 B CN 103100363B
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Abstract
The invention discloses automatic derivatization reaction processing equipment and a method. The equipment comprises N derivatization reaction units, wherein 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, a third control valve, a first one-way valve, a second one-way valve, a third one-way valve, a first constant displacement pump, a second constant displacement pump, a third constant displacement pump, a constant volume sensor, a temperature sensor, a heater, an electromagnetic stirrer, a timer and a control module, wherein each control module comprises a master controller, a valve controller, a temperature controller, a stirring controller, a time controller, a constant volume sensor and a pump controller; and in each control module, the valve controller, the temperature controller, the time controller, the constant volume controller and the pump controller are all connected with the master controller. According to the method, the control module is used to control all parts in real time according to the reaction process of the derivatization reaction, so that the whole reaction process can be completed automatically; and the labor intensity of workers can be reduced, and the derivatization time and the derivatization temperature can be accurately controlled, so that the derivatization experiments for batches of samples are higher in accuracy and better in parallelism.
Description
Technical field
The present invention relates to a kind of automatic derivatization reaction treatment Apparatus and method for.
Background technology
Derivatization is a kind of material that utilizes chemical transformation compound to be changed into similar chemical constitution.In general, the compound of a specific function participates in derivatization reaction, solubility, and boiling point, fusing point, state of aggregation or chemical composition can produce and depart from, and consequent new chemical property can be used for quantizing or separating.The effect of analyte derivative is to be mainly similar to its chemical constitution a Substance Transformation that is difficult to analyze but to be easy to the material of analyzing, and is convenient to quantize and separate, and as when detection material is during without UV absorption, can be added chromophore, the material that generation can be detected.
Chemical derivatization is widely used in Instrumental Analysis.In gas-chromatography, applied chemistry derivatization reaction is the volatility in order to increase sample or improves detection sensitivity, and the chemical derivatization of high performance liquid chromatography refers to and utilizes certain reagent (being generally called chemically derived reagent or labelled reagent) and sample component to carry out chemical reaction under certain condition, the product of reaction is conducive to chromatogram and detects or separate.General chemical derivatization mainly contains following object: the sensitivity that improves sample detection; Improve the separating degree of sample mixture; Be suitable for further doing Structural Identification, as mass spectrum, infrared or nuclear magnetic resonance etc.Carry out chemically derived reaction and should meet following requirement: reaction condition is required not harsh, and can be rapidly, carry out quantitatively; Certain component in sample is only generated to a kind of derivative, and byproduct of reaction and excessive derivative reagent do not disturb the separation and detection of sample; Chemically derived reagent is conveniently easy to get, and versatility is good.
At present, the conventional derivative reaction utensil in laboratory has volumetric flask, water-bath etc., some problems below existing in the time carrying out the test of common derivatization: 1, the visual constant volume of volumetric flask can cause volumetric errors, or cause constant volume error because of volumetric flask quality problems; 2, water-bath is in the derivatization process of batch sample, and temperature control has certain deviation, and cannot realize 100 DEG C of above derivative reactions; 3, in batch sample derivatization process, because causing the derivatization process of each sample, artificial origin's (as operating time, timing error etc.) is not quite similar, there is experimental error; 4, derivative reaction is subject to the impact of operating personnel's level.
Therefore, for reducing the experimental error of derivative reaction, be badly in need of providing a kind of derivatization reaction Apparatus and method for of automation, can control accurately derivative time, derivative temperature, make batch sample derivatization experiment accuracy higher, collimation is better.
Summary of the invention
A kind of automatic derivatization reaction treatment of the present invention Apparatus and method for, its object is to provide the chemical derivatization reaction treatment Apparatus and method for of a kind of automation, sequencing, overcomes accuracy and the not high problem of operating efficiency of in prior art, manually carrying out analyzing and testing experiment.
A kind of automatic derivatization reaction treatment equipment, comprise N derivative reaction unit, derivative reaction unit is connected in parallel, and each derivative reaction unit comprises solvent bottle, washer bottle, sample bottle, reaction bulb, the first control valve, the second control valve, the 3rd control valve, the first check valve, the second check valve, the 3rd check valve, the first constant displacement pump, the second constant displacement pump, the 3rd constant displacement pump, constant volume sensor, temperature sensor, heater, magnetic stirrer, timer and control module;
Described control module comprises master controller, valve control, temperature controller, mixing control device, time controller, constant volume sensor and pump controller; Valve control, temperature controller, time controller, constant volume sensor and pump controller are all connected with main controller; Wherein N is more than or equal to 1 integer;
Wherein, valve control is for controlling the valve control of the first control valve, the second control valve, the 3rd control valve, the first check valve, the second check valve and the 3rd check valve;
Temperature controller is for control heater;
Mixing control device is used for controlling magnetic stirrer;
Pump controller is for controlling the pump controller of the first constant displacement pump, the second constant displacement pump and the 3rd constant displacement pump;
Wherein, the first control valve and the second control valve are three-way control valve, and the 3rd control valve is two-way control valve;
Described solvent bottle, the first check valve, the first constant displacement pump, the first control valve and reaction bulb connect by pipeline successively;
Described washer bottle is all connected with the second control valve with sample bottle, and the second control valve, the second check valve, the second constant displacement pump and reaction bulb connect by pipeline successively;
Described reaction bulb, the 3rd check valve, the 3rd constant displacement pump and checkout gear connect by pipeline successively;
Described reaction bulb is also connected with the 3rd control valve by pipeline;
Described reaction bulb is provided with constant volume sensor and temperature sensor, and heater and magnetic stirrer are all located at reaction bulb bottom.
Described solvent bottle quantity is M, and M is more than or equal to 1 integer, in the time that M is more than or equal to 2, between solvent bottle, is communicated with by the first mixing valve, and the first mixing valve is connected with the first check valve.
Described washer bottle quantity is P, and P is that integer is more than or equal to 1, in the time that P is more than or equal to 2, between washer bottle, is communicated with by the second mixing valve, and the second mixing valve is connected with the second control valve.
Described pipeline is PEEK pipe.
A kind of automatic derivatization reaction treatment method, the method for the equipment based on above-mentioned comprises the following steps:
Step 1: open the first check valve, start the first constant displacement pump, with the solvent bottle of derivative liquid rinse in solvent bottle and the pipeline between the first constant displacement pump;
Step 2: start the second constant displacement pump, the pipeline between the second control valve gating sample bottle and the second check valve, extracts quantitative sample solution to reaction bulb, and the first constant displacement pump extracts quantitative derivative solution and cut out the first control valve to reaction bulb;
Step 3: utilize temperature sensor control heater to make solution temperature in reaction bulb rise to design temperature, then start timer timing to setting-up time, mixing control device starts magnetic stirrer work;
Step 4: to being derivative reaction while completing, timer, heater and agitator quit work until the setting-up time of timer, allows the solution after derivative be cooled to room temperature;
Step 5: start constant volume sensor, reaction solution in reaction bulb is settled to set volume, residue reaction solution is discharged by the first control valve, if reaction solution volume is less than set volume in reaction bulb, open the first control valve, start derivative liquid to the reaction bulb of the first constant displacement pump extraction and be settled to set volume, start agitator mixing time T;
Step 6: start the 3rd constant displacement pump, the solution after quantitative extraction is derivative is to checkout gear;
Step 7: pipeline cleaning, open the 3rd control valve, will remain solution after derivatization reaction and discharge, the second control valve gating detergent line, the second constant displacement pump extracts after cleaning solution cleans the pipeline between the second control valve to the three control valves and cuts out the 3rd control valve.
Described solvent bottle quantity is M, M is more than or equal to 1 integer, in the time that M is more than or equal to 2, and the solvent ratios being extracted by the each solvent bottle of mixing valve control, all solvent bottles are first communicated with the entrance of mixing valve, and the outlet of mixing valve is connected with the first check valve again.
Described washer bottle quantity is P, P is more than or equal to 1 integer, in the time that P is more than or equal to 2, and the cleaning fluid ratio being extracted by the each washer bottle of mixing valve control, all washer bottles are first communicated with the entrance of mixing valve, and the outlet of mixing valve is connected with the second control valve again.
Beneficial effect
The invention provides a kind of automatic derivatization reaction treatment Apparatus and method for, this equipment comprises N derivative reaction unit, derivative reaction unit is connected in parallel, and each derivative reaction unit comprises solvent bottle, washer bottle, sample bottle, reaction bulb, the first control valve, the second control valve, the 3rd control valve, the first check valve, the second check valve, the 3rd check valve, the first constant displacement pump, the second constant displacement pump, the 3rd constant displacement pump, constant volume sensor, temperature sensor, heater, magnetic stirrer, timer and control module; Described control module comprises master controller, valve control, temperature controller, mixing control device, time controller, constant volume sensor and pump controller; Valve control, temperature controller, time controller, constant volume sensor and pump controller are all connected with main controller; Wherein N is more than or equal to 1 integer; Wherein, valve control is for controlling the valve control of the first control valve, the second control valve, the 3rd control valve, the first check valve, the second check valve and the 3rd check valve; Temperature controller is for control heater; Mixing control device is used for controlling magnetic stirrer; Pump controller is for controlling the pump controller of the first constant displacement pump, the second constant displacement pump and the 3rd constant displacement pump; This apparatus structure is simple, easily realizes, and suitable batch is carried out derivative reaction; The method utilizes control module to control in real time each parts according to the course of reaction of derivative reaction, and whole course of reaction is completed automatically; Utilize constant displacement pump, make can quantitatively extract solution in derivative reaction process, reduce the error in course of reaction in batch production; Adopt constant volume sensor to improve constant volume precision; Adopt automatic derivatizationization reaction pre-processing device and method, can reduce hand labor intensity, control accurately derivative time and derivative temperature, make batch sample derivatization experiment accuracy higher, collimation is better.
Brief description of the drawings
Fig. 1 is electric control structure figure of the present invention;
Fig. 2 is working cell of the present invention mechanical construction drawing;
Fig. 3 is workflow schematic diagram of the present invention.
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention will be further described, taking 6 working cells as example.
As depicted in figs. 1 and 2, a kind of automatic derivatization reaction treatment equipment, comprise 6 derivative reaction unit, derivatization unit is connected in parallel, and each derivative reaction unit comprises solvent bottle, washer bottle, sample bottle, reaction bulb, the first control valve, the second control valve, the 3rd control valve, the first check valve, the second check valve, the 3rd check valve, the first constant displacement pump, the second constant displacement pump, the 3rd constant displacement pump, constant volume sensor, temperature sensor, heater, magnetic stirrer, timer and control module; Described control module comprises master controller, for controlling the valve control of the first control valve, the second control valve, the 3rd control valve, the first check valve, the second check valve and the 3rd check valve, for the temperature controller of control heater, for controlling the mixing control device of magnetic stirrer, the pump controller of time controller, constant volume sensor and control the first constant displacement pump, the second constant displacement pump and the 3rd constant displacement pump; Valve control, temperature controller, time controller, constant volume sensor and pump controller are all connected with main controller;
Wherein, the first control valve and the second control valve are three-way control valve, and the 3rd control valve is two-way control valve;
Described solvent bottle comprises solvent bottle A and solvent bottle B, and solvent bottle A is all connected with the first mixing valve with solvent bottle B, and the first mixing valve, the first check valve, the first constant displacement pump, the first control valve and reaction bulb connect by pipeline successively;
Described washer bottle and sample bottle are all connected to reaction bulb with the second control valve, the second check valve and the second constant displacement pump successively by pipeline; Wherein, washer bottle comprises washer bottle C and washer bottle D, and washer bottle C is all connected with the second mixing valve with washer bottle D, and the second mixing valve is connected with the second control valve;
Described reaction bulb is connected to checkout gear with the 3rd check valve and the 3rd constant displacement pump successively by pipeline;
Described reaction bulb is also connected with the 3rd control valve by pipeline;
Described reaction bulb is provided with constant volume sensor and temperature sensor, and heater and magnetic stirrer are all located at reaction bulb bottom.
A kind of automatic derivatization reaction treatment method, the method based on the said equipment comprises the following steps:
Step 1: open the first check valve, start the first constant displacement pump, with the derivative liquid A in solvent bottle or the pipeline between B or solvent bottle of AB rinse and the first constant displacement pump;
Step 2: start the second constant displacement pump, the pipeline between the second control valve gating sample bottle and the second check valve, extracts 2ml sample solution to reaction bulb, and the first constant displacement pump extracts 5ml derivative solution and cut out the first control valve to reaction bulb;
Step 3: utilize temperature sensor control heater to make solution temperature in reaction bulb rise to design temperature, then start timer timing to setting-up time, mixing control device starts magnetic stirrer work;
Step 4: to being derivative reaction while completing, timer, heater and agitator quit work until the setting-up time of timer, allows the solution after derivative be cooled to room temperature;
Step 5: start constant volume sensor, reaction solution in reaction bulb is settled to set volume 10ml, residue reaction solution is discharged by the first control valve, if reaction solution volume is less than set volume in reaction bulb, open the first control valve, extract derivative liquid to reaction bulb by the second constant displacement pump and be settled to 10ml, start agitator mixing time T, wherein T is 10 seconds;
Step 6: start the 3rd constant displacement pump, quantitatively extract the solution of 2ml after derivative to checkout gear;
Step 7: pipeline cleaning, open the 3rd control valve, after remaining derivatization reaction, solution is discharged, the second control valve gating detergent line, and the second constant displacement pump extracts after cleaning solution C or D or CD clean the pipeline between the second control valve to the three control valves and cuts out the 3rd control valve.
Claims (3)
1. an automatic derivatization reaction treatment method, it is characterized in that, adopt a kind of automatic derivatization reaction treatment equipment, described automatic derivatization reaction treatment equipment comprises a kind of automatic derivatization reaction treatment equipment, comprise N derivative reaction unit, derivative reaction unit is connected in parallel, each derivative reaction unit comprises solvent bottle, washer bottle, sample bottle, reaction bulb, the first control valve, the second control valve, the 3rd control valve, the first check valve, the second check valve, the 3rd check valve, the first constant displacement pump, the second constant displacement pump, the 3rd constant displacement pump, constant volume sensor, temperature sensor, heater, magnetic stirrer, timer and control module,
Described control module comprises master controller, valve control, temperature controller, mixing control device, time controller, constant volume sensor and pump controller; Valve control, temperature controller, time controller, constant volume sensor and pump controller are all connected with main controller; Wherein N is more than or equal to 1 integer;
Wherein, valve control is for controlling the valve control of the first control valve, the second control valve, the 3rd control valve, the first check valve, the second check valve and the 3rd check valve;
Temperature controller is for control heater;
Mixing control device is used for controlling magnetic stirrer;
Pump controller is for controlling the pump controller of the first constant displacement pump, the second constant displacement pump and the 3rd constant displacement pump;
Wherein, the first control valve and the second control valve are three-way control valve, and the 3rd control valve is two-way control valve;
Described solvent bottle, the first check valve, the first constant displacement pump, the first control valve and reaction bulb connect by pipeline successively;
Described washer bottle is all connected with the second control valve with sample bottle, and the second control valve, the second check valve, the second constant displacement pump and reaction bulb connect by pipeline successively;
Described reaction bulb, the 3rd check valve, the 3rd constant displacement pump and checkout gear connect by pipeline successively;
Described reaction bulb is also connected with the 3rd control valve by pipeline;
Described reaction bulb is provided with constant volume sensor and temperature sensor, and heater and magnetic stirrer are all located at reaction bulb bottom;
Described solvent bottle quantity is M, and M is more than or equal to 1 integer, in the time that M is more than or equal to 2, between solvent bottle, is communicated with by the first mixing valve, and the first mixing valve is connected with the first check valve;
Described washer bottle quantity is P, and P is that integer is more than or equal to 1, in the time that P is more than or equal to 2, between washer bottle, is communicated with by the second mixing valve, and the second mixing valve is connected with the second control valve;
Described pipeline is PEEK pipe;
Treatment step is as follows:
Step 1: open the first check valve, start the first constant displacement pump, with the solvent bottle of derivative liquid rinse in solvent bottle and the pipeline between the first constant displacement pump;
Step 2: start the second constant displacement pump, the pipeline between the second control valve gating sample bottle and the second check valve, extracts quantitative sample solution to reaction bulb, and the first constant displacement pump extracts quantitative derivative solution and cut out the first control valve to reaction bulb;
Step 3: utilize temperature sensor control heater to make solution temperature in reaction bulb rise to design temperature, then start timer timing to setting-up time, mixing control device starts magnetic stirrer work;
Step 4: to being derivative reaction while completing, timer, heater and agitator quit work until the setting-up time of timer, allows the solution after derivative be cooled to room temperature;
Step 5: start constant volume sensor, reaction solution in reaction bulb is settled to set volume, residue reaction solution is discharged by the first control valve, if reaction solution volume is less than set volume in reaction bulb, open the first control valve, start derivative liquid to the reaction bulb of the first constant displacement pump extraction and be settled to set volume, start agitator mixing time T;
Step 6: start the 3rd constant displacement pump, the solution after quantitative extraction is derivative is to checkout gear;
Step 7: pipeline cleaning, open the 3rd control valve, will remain solution after derivatization reaction and discharge, the second control valve gating detergent line, the second constant displacement pump extracts after cleaning solution cleans the pipeline between the second control valve to the three control valves and cuts out the 3rd control valve.
2. automatic derivatization reaction treatment method according to claim 1, it is characterized in that, described solvent bottle quantity is M, M is more than or equal to 1 integer, in the time that M is more than or equal to 2, the solvent ratios being extracted by the each solvent bottle of mixing valve control, all solvent bottles are first communicated with the entrance of mixing valve, and the outlet of mixing valve is connected with the first check valve again.
3. automatic derivatization reaction treatment method according to claim 1 and 2, it is characterized in that, described washer bottle quantity is P, P is more than or equal to 1 integer, in the time that P is more than or equal to 2, the cleaning fluid ratio being extracted by the each washer bottle of mixing valve control, all washer bottles are first communicated with the entrance of mixing valve, and the outlet of mixing valve is connected with the second control valve again.
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| CN201310036043.0A CN103100363B (en) | 2013-01-30 | 2013-01-30 | Automatic derivatization reaction processing equipment and method |
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| CN103100363B true CN103100363B (en) | 2014-08-06 |
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| CN112791688A (en) * | 2021-02-02 | 2021-05-14 | 申联生物医药（上海）股份有限公司 | Full-automatic solid-phase organic synthesis modularization equipment |
| CN117030637A (en) * | 2023-06-14 | 2023-11-10 | 北京市计量检测科学研究院 | Solid sample detection device |
Citations (4)
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| JP2000189778A (en) * | 1998-12-31 | 2000-07-11 | Tetsuyoshi Nakamura | Supercritical water dioxins continuous decomposition device |
| US20080032416A1 (en) * | 2004-09-02 | 2008-02-07 | Park Han O | Miniaturized Apparatus For Real-Time Monitoring |
| CN202410645U (en) * | 2012-01-17 | 2012-09-05 | 浙江丰登化工股份有限公司 | Automatic pressure and temperature control device for hydrogenation reaction kettle |
| CN202516542U (en) * | 2012-03-06 | 2012-11-07 | 美药星（南京）制药有限公司 | PH and temperature automatic control system for reaction kettle |
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- 2013-01-30 CN CN201310036043.0A patent/CN103100363B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000189778A (en) * | 1998-12-31 | 2000-07-11 | Tetsuyoshi Nakamura | Supercritical water dioxins continuous decomposition device |
| US20080032416A1 (en) * | 2004-09-02 | 2008-02-07 | Park Han O | Miniaturized Apparatus For Real-Time Monitoring |
| CN202410645U (en) * | 2012-01-17 | 2012-09-05 | 浙江丰登化工股份有限公司 | Automatic pressure and temperature control device for hydrogenation reaction kettle |
| CN202516542U (en) * | 2012-03-06 | 2012-11-07 | 美药星（南京）制药有限公司 | PH and temperature automatic control system for reaction kettle |
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