WO2022127928A1 - 一种自动进样系统 - Google Patents

一种自动进样系统 Download PDF

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Publication number
WO2022127928A1
WO2022127928A1 PCT/CN2021/139400 CN2021139400W WO2022127928A1 WO 2022127928 A1 WO2022127928 A1 WO 2022127928A1 CN 2021139400 W CN2021139400 W CN 2021139400W WO 2022127928 A1 WO2022127928 A1 WO 2022127928A1
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WIPO (PCT)
Prior art keywords
module
channel switching
inert gas
liquid storage
pipeline
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Application number
PCT/CN2021/139400
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English (en)
French (fr)
Inventor
叶新山
姚文龙
熊德彩
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北京大学
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Publication date
Application filed by 北京大学 filed Critical 北京大学
Priority to US18/268,313 priority Critical patent/US20240036069A1/en
Priority to EP21905850.0A priority patent/EP4220182A4/en
Priority to JP2023535355A priority patent/JP2023553132A/ja
Publication of WO2022127928A1 publication Critical patent/WO2022127928A1/zh

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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
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/24—Automatic injection systems
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N35/10—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices
    • G01N35/1065—Multiple transfer devices
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277—Apparatus
    • B01J2219/00351—Means for dispensing and evacuation of reagents
    • B01J2219/00353—Pumps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277—Apparatus
    • B01J2219/00351—Means for dispensing and evacuation of reagents
    • B01J2219/00389—Feeding through valves
    • B01J2219/00409—Solenoids in combination with valves
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00274—Sequential or parallel reactions; Apparatus and devices for combinatorial chemistry or for making arrays; Chemical library technology
    • B01J2219/00277—Apparatus
    • B01J2219/00351—Means for dispensing and evacuation of reagents
    • B01J2219/00418—Means for dispensing and evacuation of reagents using pressure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/02—Feed or outlet devices; Feed or outlet control devices for feeding measured, i.e. prescribed quantities of reagents
    • 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
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/16—Injection
    • G01N30/20—Injection using a sampling valve

Definitions

  • the invention relates to the technical field of experiments, in particular to an automatic sampling system.
  • Pipeline transfer injection At present, there are peptide solid-phase synthesizers, oligosaccharide solid-phase synthesizers and automatic solid-phase extraction instruments on the market. Its advantages are that the system is airtight, safe, free from external interference and systemic; its disadvantages are long research and development cycles and high design and development costs for a single finished product. There are two ways to design it: 1.
  • the components are purchased and assembled, which can be flexibly adjusted and modified to facilitate the integration of programs (syringe pump unit, multi-channel switching valve, light source, low temperature circulation, magnetic stirring, etc., and online monitoring), but also requires Redesign requires a long period of time and requires talents from all walks of life, and there are many factors that affect the operation results after assembly. 2. Transformation and upgrading from commercial similar products, that is, appropriate transformation of mature automation products, short cycle and no need for too much manpower, can ensure normal work, but because mature products have mature software control systems developed by their own patents, program integration is troublesome , without source code, may need to redesign the integrated board. 2.
  • Automatic pipetting and sampling At present, there are mature automatic pipetting workstations for sale on the market (prices range from 100,000 to 400,000), which can be purchased directly and modified slightly. Its advantages are that it is simple, fast, and can directly solidify manual operations on the instrument; the disadvantage is that all operations need to be replaced by robotic arms, with high failure rate and large space. It is also a mature product, and the program integration is inconvenient.
  • the purpose of the present invention is to provide an automatic sampling system to ensure the stability and accuracy of automatic sampling during the experiment.
  • the present invention provides the following scheme:
  • An automatic sampling system comprising: an inert gas delivery module, a sampling channel switching module, a quantitative module, a disposal module, a liquid storage module and a host computer;
  • Both the liquid storage module and the sampling channel switching module are connected to the inert gas delivery module through pipelines; the quantitative module is respectively connected to the sampling channel switching module and the disposal module through pipelines; The liquid module is connected with the sampling channel switching module through a pipeline;
  • the inert gas delivery module, the sampling channel switching module and the quantitative module are all electrically connected to the upper position;
  • the inert gas delivery module is used to deliver the internally stored inert gas to the liquid storage module and the sampling channel switching module through pipelines respectively; the sampling channel switching module is used to extract the stored inert gas in the liquid storage module.
  • the upper computer is used to control the opening and closing of the inert gas delivery module and the quantitative module, and is used to control the sampling channel switching module to perform channel switching.
  • the inert gas delivery module includes: an inert gas storage, a pressure regulating filter and a first solenoid valve unit;
  • the inert gas storage is connected to the liquid storage module and the sampling channel switching module respectively through pipelines; the pressure regulating filter and the first solenoid valve unit are arranged between the inert gas storage and the liquid storage module. on the connecting pipeline, or on the connecting pipeline between the inert gas storage and the sampling channel switching module.
  • the liquid storage module includes N liquid storage bottles;
  • Each of the liquid storage bottles is connected with the inert gas delivery module through a pipeline; the bottom of the liquid storage bottle is conical or arc-shaped.
  • the liquid storage bottle comprises: a first channel opening, a second channel opening, a third channel opening and a bottle cap;
  • the first channel port is used for connecting with the sampling channel switching module through a pipeline;
  • the second channel port is used for connecting with the inert gas delivery module through a pipeline;
  • the third channel port is used for discharging the storage tank. gas or liquid in a liquid bottle;
  • the bottle cap is threadedly connected with the bottle mouth of the liquid storage bottle.
  • the sampling channel switching module includes: a first multi-channel switching valve and a second multi-channel switching valve;
  • the first multi-channel switching valve is connected with M number of the liquid storage bottles through pipelines; the second multi-channel switching valve is connected with N-M liquid storage bottles through pipelines.
  • the quantitative module includes: a syringe pump unit, a pressure sensor, a flow meter and a second solenoid valve unit;
  • the inlet of the syringe pump unit is connected to the sampling channel switching module through a pipeline; the outlet of the syringe pump unit is connected to the flowmeter through a pipeline; the flowmeter is connected to the disposal module through a pipeline;
  • the second solenoid valve unit is arranged on the connection pipeline between the flowmeter and the treatment module; the pressure sensor is arranged on the connection pipeline between the syringe pump unit and the flowmeter; the second solenoid valve The unit, the pressure sensor and the flowmeter are all connected with the upper machine electromechanically.
  • the disposal module includes: a novel reactor, a solution pipe and a waste liquid bottle;
  • the sample inlet of the novel reactor and the liquid inlet of the waste product are connected to the second solenoid valve unit through pipelines;
  • the solution pipe is connected to the exhaust port of the novel reactor through pipelines connect;
  • the second solenoid valve unit is used to close the connection pipeline between the flowmeter and the new reactor when the solution in the new reactor reaches a set amount, and open the flowmeter and the waste gas. connection line for the liquid bottle.
  • the novel reactor includes: a bottle mouth, a bottle body and a sampling mouth;
  • the bottle body sequentially includes a reaction inner tank, a temperature circulation layer and a vacuum layer from the inside to the outside; the tank bottom of the reaction inner tank is a circular arc structure;
  • the sampling port is communicated with the reaction inner tank.
  • the syringe pump unit includes: a first syringe pump and a second syringe pump;
  • the first syringe pump is connected with a channel in the first multi-channel switching valve through a pipeline; the second syringe pump is connected with a channel in the second multi-channel switching valve through a pipeline; the The range of the first syringe pump is smaller than the range of the second syringe pump.
  • the present invention discloses the following technical effects:
  • the invention provides an automatic sampling system, which includes an inert gas delivery module, a sampling channel switching module, a quantitative module, a disposal module, a liquid storage module and a host computer.
  • an inert gas delivery module By using the upper computer to control the sampling channel switching module and the quantitative module, the precise control of the injection volume can be achieved.
  • the sampling channel switching module and the inert gas delivery module can be used to transmit each reaction solution independently, thereby further improving the stability of the injection, thereby ensuring the accuracy of the experimental reaction.
  • Fig. 1 is the structural representation of the automatic sampling system provided by the present invention
  • Fig. 2 is the structural representation of the liquid storage bottle provided by the present invention.
  • Fig. 3 is the structural representation of the novel reactor provided by the present invention.
  • FIG. 4 is a schematic structural diagram of the automatic sampling system provided in the embodiment of the present invention for collecting the solution to be reacted in the first liquid storage bottle.
  • 1-Inert gas delivery module 11-Inert gas storage, 12-Pressure regulating filter, 13-First solenoid valve unit, 131-First two-way solenoid valve, 132-Second two-way solenoid valve, 133-Three-way Solenoid valve, 2-sampling channel switching module, 21-first multi-channel switching valve, 22-second multi-channel switching valve, 3-quantitative module, 31-syringe pump unit, 311-first syringe pump, 312-second Syringe pump, 32-pressure sensor, 33-flow meter, 34-second solenoid valve unit, 4-disposal module, 41-new reactor, 411-bottle port, 412-injection port, 413-exhaust port, 414 -Sampling port, 415-bottle body, 4151-reaction liner, 4152-temperature circulation layer, 4153-vacuum layer, 42-solution tube, 43-waste liquid bottle, 5-liquid storage module, 51-liquid storage bottle, 511 -
  • the purpose of the present invention is to provide an automatic sampling system to ensure the stability and accuracy of automatic sampling during the experiment.
  • the automatic sampling system includes: an inert gas delivery module 1, a sampling channel switching module 2, a quantitative module 3, a disposal module 4, a liquid storage module 5 and a host computer (not shown in the figure) ).
  • Both the liquid storage module 5 and the sampling channel switching module 2 are connected to the inert gas delivery module 1 through pipelines.
  • the quantitative module 3 is respectively connected with the sampling channel switching module 2 and the treatment module 4 through pipelines.
  • the liquid storage module 5 is connected to the sampling channel switching module 2 through pipelines.
  • the inert gas delivery module 1 , the sampling channel switching module 2 and the quantitative module 3 are all electrically connected to the upper position.
  • the inert gas delivery module 1 is used to deliver the internally stored inert gas to the liquid storage module 5 and the sampling channel switching module 2 through pipelines, respectively.
  • the sampling channel switching module 2 is used for extracting the solution to be reacted stored in the liquid storage module 5 and for switching the channel for extracting the solution to be reacted.
  • the quantitative module 3 is used to determine the amount of the solution to be reacted injected into the treatment module 4 .
  • the host computer is used to control the opening and closing of the inert gas delivery module 1 and the quantitative module 3, and is used to control the sampling channel switching module 2 to perform channel switching.
  • All other external devices can be controlled by the host computer through the communication protocol by the programmable logic controller (Programmable Logic Controller, PLC) for program control to meet the normal operation of the automation program.
  • PLC Programmable Logic Controller
  • the above-mentioned inert gas delivery module 1 includes: an inert gas storage 11 , a pressure regulating filter 12 and a first solenoid valve unit 13 .
  • the inert gas storage 11 is respectively connected to the liquid storage module 5 and the sampling channel switching module 2 through pipelines.
  • the pressure regulating filter 12 and the first solenoid valve unit 13 are arranged on the connecting pipeline between the inert gas storage 11 and the liquid storage module 5, or are arranged on the inert gas storage 11 and the sampling channel switching module 2 on the connecting line.
  • the first solenoid valve unit includes: a first two-way solenoid valve 131 , a second two-way solenoid valve 132 and a three-way solenoid valve 133 .
  • the first two-way solenoid valve 131 and the three-way solenoid valve 133 are disposed on the connection pipeline between the inert gas storage 11 and the sampling channel switching module 2 .
  • the second two-way solenoid valve 132 is disposed on the connection pipeline between the inert gas storage 11 and the liquid storage module 5 .
  • the number of pressure regulating filters 12 is two, and the two pressure regulating filters are respectively disposed on the connecting pipeline between the inert gas storage 11 and the sampling channel switching module 2 and the inert gas storage 11 and the on the connecting pipeline of the liquid storage module 5 .
  • the above-mentioned liquid storage module 5 includes N liquid storage bottles 51 .
  • Each of the liquid storage bottles 51 is connected to the inert gas delivery module 1 through pipelines.
  • the bottom 512 of the liquid storage bottle 51 is conical or arc-shaped.
  • Each liquid storage bottle 51 includes: a first channel opening, a second channel opening, a third channel opening and a bottle cap 511 .
  • the first channel port is used for connecting with the sampling channel switching module 2 through a pipeline.
  • the second passage port is used to connect with the inert gas delivery module 1 through a pipeline.
  • the third channel port is used to discharge the gas or liquid in the liquid storage bottle 51 .
  • the bottle cap 511 is threadedly connected to the bottle mouth 411 of the liquid storage bottle 51 , as shown in FIG. 2 .
  • the slightly positive pressure of the inert gas fills each liquid storage bottle 51 to prevent the closed liquid storage bottle 51 from generating negative pressure due to the reduction of the liquid, thereby affecting the accuracy of the injection.
  • liquid storage bottles 51 There are preferably four kinds of liquid storage bottles 51 provided by the present invention: 10 mL pointed bottom liquid storage bottle, 20 mL pointed bottom liquid storage bottle, 500 mL round bottom liquid storage bottle and 125 mL two-neck liquid storage bottle.
  • the 10mL and 20mL pointed-bottom liquid storage bottles are mainly used to reserve block samples and reagent catalysts.
  • the pointed bottom is designed to allow the pipeline to reach the bottom of the bottle 512 to avoid the loss and waste of the storage liquid.
  • the internal thread design is convenient for custom-made PTFE
  • the bottle cap is 511.
  • the 500mL round-bottom liquid storage bottle is mainly used to store ultra-dry organic solvents
  • the 125mL two-neck bottle is mainly used to store organic solvents for diluting the reaction solution, and even waste liquid.
  • the injection port 412 on the side is mainly used for insertion and extraction of sampling needles during online monitoring.
  • All the liquid storage bottles 51 are made of transparent tube-sealed glass, which has the ability to withstand pressure.
  • the main purpose of not using brown or black is to facilitate the user of the instrument to observe the remaining amount of the storage liquid.
  • the design of the custom cap 511 matched with the custom reservoir bottle 51 has undergone repeated exploration, verification and modification.
  • the bottle cap 511 has three passages, which are respectively used for ventilation, liquid passage and air release.
  • the bottle cap 511 In order to ensure the stability of the concentration of the stock solution and the accuracy of automatic sample injection, the bottle cap 511 must be tightly sealed, convenient for on-off, corrosion-resistant and durable.
  • an on-off switch is embedded inside the bottle cap 511, and the bottom of the bottle cap 511 is thinned and connected with an inverted cone to ensure that the compaction seal does not require a sealing ring and the connection is tight, and the top of the bottle cap 511 is arranged in a triangular shape
  • the inverted cone connection ensures the tightness of the connecting pipeline to obtain the initial customized bottle cap 511 .
  • the above sampling channel switching module 2 includes: a first multi-channel switching valve 21 and a second multi-channel switching valve 22 .
  • the first multi-channel switching valve 21 is connected to the M liquid storage bottles 51 through pipelines.
  • the second multi-channel switching valve 22 is connected to N-M of the liquid storage bottles 51 through pipelines.
  • the two ten-channel switching valves can be connected in parallel or cross-connected to liquid storage bottles 51 of different specifications.
  • the 10th channel of the two switching valves is always connected to the inert gas
  • the 9th channel is connected to the commonly used ultra-dry solvent (such as dichloromethane)
  • the 8th channel is connected to the secondary ultra-dry solvent (such as acetonitrile or toluene, etc.)
  • other channels can be independent or cross-connected with different or the same stock solution without cross-contamination.
  • 1 and FIG. 4 are only for simple illustration, and the connection pipelines of all the liquid storage bottles 51 are not drawn. Those skilled in the art can obtain from the technical field provided by the present invention in combination with common knowledge in the field.
  • the specific pipeline connection structure diagram is only for simple illustration, and the connection pipelines of all the liquid storage bottles 51 are not drawn.
  • the injection volume of less than or close to 1mL is connected to the first multi-channel switching valve 21, and the injection volume greater than or close to 1mL is connected to the second multi-channel switching valve 22.
  • Each channel of the multi-channel switching valve also needs to be connected with each storage liquid
  • the substances in the bottle 51 are in one-to-one correspondence.
  • the inert gas storage 11 is successively depressurized and filtered through the pressure reducing valve and the pressure regulating filter 12 , so as to provide positive pressure and clean the pipeline.
  • the above-mentioned quantitative module 3 includes: a syringe pump unit 31 , a pressure sensor 32 , a flow meter 33 and a second solenoid valve unit 34 .
  • the inlet of the syringe pump unit 31 is connected to the sampling channel switching module 2 through a pipeline.
  • the outlet of the syringe pump unit 31 is connected to the flow meter 33 through a pipeline.
  • the flow meter 33 is connected to the treatment module 4 through pipelines.
  • the second solenoid valve unit 34 is disposed on the connection pipeline between the flow meter 33 and the treatment module 4 .
  • the pressure sensor 32 is arranged on the connection pipeline between the syringe pump unit 31 and the flow meter 33 .
  • the second solenoid valve unit 34 , the pressure sensor 32 and the flow meter 33 are all electrically connected to the upper position.
  • the syringe pump unit 31 includes a first syringe pump 311 and a second syringe pump 312 .
  • the first syringe pump 311 is connected to a channel in the first multi-channel switching valve 21 through a pipeline.
  • the second syringe pump 312 is connected to a channel in the second multi-channel switching valve 22 through a pipeline.
  • the range of the first syringe pump 311 is smaller than the range of the second syringe pump 312 .
  • injection is performed by the pipeline connected to the small-range syringe pump (ie, the first injection pump 311 ).
  • the pipeline connected by the large-range syringe pump ie, the second syringe pump 312
  • the two pipelines are performed in parallel and then combined into one into the reactor.
  • the syringe on the syringe pump can be replaced, the minimum is 500uL, the maximum is 25mL, and the number of switching valves and syringe pumps can be increased modularly for expansion.
  • Each pipeline is a syringe pump to provide injection power.
  • Each pipeline has its own syringe pump and the high-precision flowmeter 33 behind it to cooperate, double control to ensure the accuracy of the injection, and the measurement of the flowmeter 33 is used as the final injection between the syringe pump and the flowmeter 33. sample size.
  • One reason for this setting is that the accuracy (1%) of the syringe pump itself is lower than the accuracy (2 ⁇ ) of the flow meter 33 itself.
  • the second is that the syringe pump cannot identify air bubbles or whether there is a reserve liquid, and the measurement difference between the gas and the liquid of the flow meter 33 is large, and the measurement change when the gas passes through can be fed back to the double self-correction of the flow meter 33 and the syringe pump. .
  • the above-mentioned disposal module 4 includes: a novel reactor 41 , a solution pipe 42 and a waste liquid bottle 43 .
  • the sample inlet 412 of the novel reactor 41 and the liquid inlet of the waste product are both connected to the second solenoid valve unit 34 through pipelines.
  • the solution pipe 42 is connected to the exhaust port 413 of the novel reactor 41 through a pipeline.
  • the second solenoid valve unit 34 is used to close the connection pipeline between the flowmeter 33 and the new reactor 41 and open the flowmeter when the solution in the new reactor 41 reaches a set amount. 33 and the connection pipeline of the waste liquid bottle 43 .
  • the solenoid valve next to the flowmeter 33 will immediately switch the excess solution to be reacted into the waste liquid bottle 43 to ensure the injection volume into the new reactor 41 precise.
  • an instruction on whether to perform pipeline cleaning can be programmed in the host computer as required, and the waste liquid from the pipeline cleaning also enters the waste liquid bottle 43 .
  • an oil bubbler Connected with the air outlet of the novel reactor 41 is an oil bubbler that can prevent back suction. The purpose of this is to ensure that the air pressure in the novel reactor 41 is normal and no foreign gas or water vapor will enter the reactor. In order to achieve the airtightness requirements of the entire automatic sampling system.
  • the novel reactor 41 adopted in the present invention includes: a bottle mouth 411, a bottle body 415 and a sampling mouth 414.
  • the injection port 412 and the bottle body 415 form a set angle.
  • the exhaust port 413 and the sample inlet 412 are symmetrically arranged with the center line of the bottle mouth 411 as the center.
  • the bottle body 415 sequentially includes a reaction liner 4151, a temperature circulation layer 4152 and a vacuum layer 4153 from the inside to the outside.
  • the bottom of the reaction liner 4151 is a circular arc structure.
  • Both the exhaust port 413 and the sampling port 414 communicate with the reaction inner tank 4151 .
  • the sampling port 414 is arranged at the bottom of the reaction inner tank 4151 .
  • the automatic sample injection system mainly includes: an inert gas storage 11, a pressure regulating filter 12, various solenoid valves, various customized liquid storage bottles 51, two ten-channel switching valves, two equipped with different Syringe pump, pressure sensor 32, high-precision flowmeter 33 and novel reactor 41 of the range syringe.
  • an inert gas storage 11 a pressure regulating filter 12
  • various solenoid valves various customized liquid storage bottles 51
  • two ten-channel switching valves two equipped with different Syringe pump
  • pressure sensor 32 high-precision flowmeter 33
  • novel reactor 41 of the range syringe The connection relationship of each component in the above modules is shown in Figure 1 and Figure 4 .

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Abstract

一种自动进样系统，包括：惰性气体输送模块（1）、取样通道切换模块（2）、定量模块（3）、处置模块（4）、储液模块（5）和上位机。通过上位机对取样通道切换模块（2）、定量模块（3）进行控制，实现进样量的精确控制。并且，采用取样通道切换模块（2）和惰性气体输送模块（1），能够分别独立的传送各反应液，进而进一步提高进样的稳定性和准确性，进而保证实验反应的精确性。

Description

一种自动进样系统
本申请要求于2020年12月19日提交中国专利局、申请号为202011508993.5、发明名称为“一种自动进样系统”的中国专利申请的优先权，其全部内容通过引用结合在本申请中。
技术领域
本发明涉及实验技术领域，特别是涉及一种自动进样系统。
背景技术
现有保证精确进样主要有两种方式：一、管路转移进样：目前市场上有多肽固相合成仪和寡糖固相合成仪及自动固相萃取仪等。它的优点是体系密闭、安全、外界无干扰与系统性强；缺点是研发周期长、单个成品的设计与研制成本高。它的设计的途径有两个：1、组件购买组装，可灵活调整和修改，便于集成程序(注射泵单元、多通道切换阀、光源、低温循环、磁力搅拌等及在线监测)，但亦需要重新设计，周期长，需要各方面人才，且组装后运行结果存在较多影响因素。2、从商业化的相似产品改造升级，即适当改造成熟自动化产品，周期短且不需要太多的人力，可保证正常工作，但由于成熟产品有自己专利研发的成熟软件控制系统，程序集成麻烦，没有源代码，可能需要重新设计集成板。二、自动移液进样：目前市面上有成熟的自动移液工作站出售(价格在10-40万)，可直接进行购买稍加改造即可。它的优点是简单、快速、可直接将手动操作固化到仪器上；缺点是所有操作需要机械臂代替，故障率高、空间大，同样是成熟产品，程序集成不便。
因此，提供一种能够保证进样稳定性和精确性的自动进样系统是本领域亟待解决的一个技术难题。
发明内容
本发明的目的是提供一种自动进样系统，以保证实验过程中自动进样的稳定性和准确性。
为实现上述目的，本发明提供了如下方案：
一种自动进样系统，包括：惰性气体输送模块、取样通道切换模块、定量模块、处置模块、储液模块和上位机；
所述储液模块和所述取样通道切换模块均通过管路与所述惰性气体输送模块连接；所述定量模块通过管路分别与所述取样通道切换模块和所述处置模块连接；所述储液模块通过管路与所述取样通道切换模块连接；
所述惰性气体输送模块、所述取样通道切换模块和所述定量模块均与所述上位机电连接；
所述惰性气体输送模块用于将内部存储的惰性气体分别通过管路输送给所述储液模块和所述取样通道切换模块；所述取样通道切换模块用于提取所述储液模块中存储的待反应溶液，并用于切换提取所述待反应溶液的通道；所述定量模块用于确定注入所述处置模块中的待反应溶液量；
所述上位机用于控制所述惰性气体输送模块和所述定量模块的开启和关闭，并用于控制所述取样通道切换模块进行通道切换。
优选地，所述惰性气体输送模块包括：惰性气体存储器、调压过滤器和第一电磁阀单元；
所述惰性气体存储器通过管路分别与所述储液模块和所述取样通道切换模块连接；所述调压过滤器和第一电磁阀单元设置在所述惰性气体存储器与所述储液模块的连接管路上，或设置在所述惰性气体存储器与所述取样通道切换模块的连接管路上。
优选地，所述储液模块包括N个储液瓶；
每一所述储液瓶均与所述惰性气体输送模块通过管路连接；所述储液瓶的瓶底为锥形或弧形。
优选地，所述储液瓶包括：第一通道口、第二通道口、第三通道口和瓶盖；
所述第一通道口用于通过管路与所述取样通道切换模块连接；所述第二通道口用于通过管路与所述惰性气体输送模块连接；第三通道口用于排出所述储液瓶中的气体或液体；
所述瓶盖与所述储液瓶的瓶口螺纹连接。
优选地，所述取样通道切换模块包括：第一多通道切换阀和第二多通道切换阀；
所述第一多通道切换阀通过管路与M个所述储液瓶连接；所述第二多通道切换阀通过管路与N-M个所述储液瓶连接。
优选地，所述定量模块包括：注射泵单元、压力传感器、流量计和第二电磁阀单元；
所述注射泵单元的入口通过管路与所述取样通道切换模块连接；所述注射泵单元的出口通过管路与所述流量计连接；所述流量计通过管路与所述处置模块连接；所述第二电磁阀单元设置在所述流量计与所述处置模块的连接管路上；所述压力传感器设置在所述注射泵单元与所述流量计的连接管路上；所述第二电磁阀单元、所述压力传感器和所述流量计均与所述上位机电连接。
优选地，所述处置模块包括：新型反应器、溶液管和废液瓶；
所述新型反应器的进样口和所述废液品的进液口均通过管路与所述第二电磁阀单元连接；所述溶液管通过管路与所述新型反应器的排气口连接；
所述第二电磁阀单元用于当所述新型反应器中溶液达到设定量时，关闭所述流量计与所述新型反应器间的连接管路，并开启所述流量计与所述废液瓶的连接管路。
优选地，所述新型反应器包括：瓶口、瓶身和取样口；
所述进样口与所述瓶身间呈设定角度；所述排气口和所述进样口以所述瓶口的中心线为中心对称设置；
所述瓶身由内及外依次包括反应内胆、温度循环层和真空层；所述反应内胆的胆底为圆弧形结构；
所述取样口与所述反应内胆连通。
优选地，所述注射泵单元包括：第一注射泵和第二注射泵；
所述第一注射泵通过管路与所述第一多通道切换阀中的一通道连接；所述第二注射泵通过管路与所述第二多通道切换阀中的一通道连接；所述第一注射泵的量程小于所述第二注射泵的量程。
根据本发明提供的具体实施例，本发明公开了以下技术效果：
本发明提供了一种自动进样系统，包括：惰性气体输送模块、取样通道切换模块、定量模块、处置模块、储液模块和上位机。通过采用上位机对取样通道切换模块、定量模块进行控制，能够实现进样量的精确控制。并且，采用取样通道切换模块和惰性气体输送模块，能够分别独立的传送各反应液，进而进一步提高进样的稳定性，进而保证实验反应的精确性。
说明书附图
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。
图1为本发明提供的自动进样系统的结构示意图；
图2为本发明提供的储液瓶的结构示意图；
图3为本发明提供的新型反应器的结构示意图；
图4为本发明实施例中提供的自动进样系统采集第一储液瓶中待反应溶液的结构原理图。
符号说明：
1-惰性气体输送模块，11-惰性气体存储器，12-调压过滤器，13-第一电磁阀单元，131-第一二通电磁阀，132-第二二通电磁阀，133-三通电磁阀，2-取样通道切换模块，21-第一多通道切换阀，22-第二多通道切换阀，3-定量模块，31-注射泵单元，311-第一注射泵，312-第二注射泵，32-压力传感器，33-流量计，34-第二电磁阀单元，4-处置模块，41-新型反应器，411-瓶口，412-进样口，413-排气口，414-取样口，415-瓶身，4151-反应内胆，4152-温度循环层，4153-真空层，42-溶液管，43-废液瓶，5-储液模块，51-储液瓶，511-瓶盖，512-瓶底。
具体实施方式
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
本发明的目的是提供一种自动进样系统，以保证实验过程中自动进样的稳定性和准确性。
为使本发明的上述目的、特征和优点能够更加明显易懂，下面结合附图和具体实施方式对本发明作进一步详细的说明。
如图1所示，本发明提供的自动进样系统，包括：惰性气体输送模块1、 取样通道切换模块2、定量模块3、处置模块4、储液模块5和上位机(图中未示出)。
所述储液模块5和所述取样通道切换模块2均通过管路与所述惰性气体输送模块1连接。所述定量模块3通过管路分别与所述取样通道切换模块2和所述处置模块4连接。所述储液模块5通过管路与所述取样通道切换模块2连接。
所述惰性气体输送模块1、所述取样通道切换模块2和所述定量模块3均与所述上位机电连接。
所述惰性气体输送模块1用于将内部存储的惰性气体分别通过管路输送给所述储液模块5和所述取样通道切换模块2。所述取样通道切换模块2用于提取所述储液模块5中存储的待反应溶液，并用于切换提取所述待反应溶液的通道。所述定量模块3用于确定注入所述处置模块4中的待反应溶液量。
所述上位机用于控制所述惰性气体输送模块1和所述定量模块3的开启和关闭，并用于控制所述取样通道切换模块2进行通道切换。
其他的外接设备都可以通过通讯协议由上位机控制可编程逻辑控制器(Programmable Logic Controller，PLC)进行程序控制以满足自动化程序的正常运行。
其中，上述惰性气体输送模块1包括：惰性气体存储器11、调压过滤器12和第一电磁阀单元13。
所述惰性气体存储器11通过管路分别与所述储液模块5和所述取样通道切换模块2连接。所述调压过滤器12和第一电磁阀单元13设置在所述惰性气体存储器11与所述储液模块5的连接管路上，或设置在所述惰性气体存储器11与所述取样通道切换模块2的连接管路上。
其中，第一电磁阀单元包括：第一二通电磁阀131、第二二通电磁阀132和三通电磁阀133。
第一二通电磁阀131和三通电磁阀133设置在所述惰性气体存储器11与所述取样通道切换模块2的连接管路上。第二二通电磁阀132设置在所述惰性气体存储器11与所述储液模块5的连接管路上。
优选地，调压过滤器12的个数为两个，两个调压过滤器分别设置在所述惰性气体存储器11与所述取样通道切换模块2的连接管路上和所述惰性气体 存储器11与所述储液模块5的连接管路上。
上述储液模块5包括N个储液瓶51。
每一所述储液瓶51均与所述惰性气体输送模块1通过管路连接。所述储液瓶51的瓶底512为锥形或弧形。
每一储液瓶51均包括：第一通道口、第二通道口、第三通道口和瓶盖511。
所述第一通道口用于通过管路与所述取样通道切换模块2连接。所述第二通道口用于通过管路与所述惰性气体输送模块1连接。第三通道口用于排出所述储液瓶51中的气体或液体。
所述瓶盖511与所述储液瓶51的瓶口411螺纹连接，如图2所示。
惰性气体微正压充满每一储液瓶51，以避免密闭的储液瓶51因液体的减少而产生负压，进而影响进样的准确度。
本发明提供的储液瓶51优选有四种：10mL尖底储液瓶，20mL尖底储液瓶，500mL圆底储液瓶和125mL两口储液瓶。10mL和20mL尖底储液瓶主要为储备砌块样品和试剂催化剂，尖底设计目的是让管路通到瓶底512避免储备液的损失和浪费，内螺纹设计方便配合定制的聚四氟乙烯瓶盖511。500mL圆底储液瓶主要为储备超干的有机溶剂，125mL两口瓶主要为储备稀释反应液的有机溶剂，甚至废液。侧面的进进样口412主要为在线监测时取样针的插入和拔出。所有的储液瓶51均为透明封管玻璃材质，具备耐压能力，未采用棕色或者黑色主要目的是便于仪器使用者观察储备液的剩余量。
从图4所示的自动进样的整体结构原理图中可以看出，在合成仪的研发过程中，除了最核心的反应器和光源及自动化进样与上位机软件的密切配合，还有起辅助和基础作用的定制配件设计，主要是各种储液瓶51和相应的瓶盖511。
与定制储液瓶51匹配的定制瓶盖511设计经历了反复的探索、验证和修改。前文提到瓶盖511有三个通道，分别为了通气、通液和放气。为了保证储备液的浓度稳定和自动进样的准确性，必须要求瓶盖511密封严格，方便通断，耐腐蚀和耐用。通过增加四氟瓶盖511的长度，在瓶盖511内部镶嵌通断开关，瓶盖511底部变细和倒锥连接，保证压实密封无需密封圈且连接紧密，瓶盖511上方通过三角型布置倒锥连接保证连接管路的密封性得到初始定制瓶盖 511。经过反复测试发现，该初始瓶盖511内部镶嵌的通断开关处有漏液现象，故又在通断开关处增加普通的弹性密封垫圈，此垫圈在瓶盖511外部，无需要求耐腐蚀功能，即得到如图2所示的四氟三通道压实性瓶盖511。
上述取样通道切换模块2包括：第一多通道切换阀21和第二多通道切换阀22。
所述第一多通道切换阀21通过管路与M个所述储液瓶51连接。所述第二多通道切换阀22通过管路与N-M个所述储液瓶51连接。
两个十通道切换阀可以平行或者交叉连接不同规格的储液瓶51。为方便使用，将两个切换阀的第10通道一直连接惰性气体，第9通道连接常用的超干溶剂(比如二氯甲烷)，第8通道连接次用的超干溶剂(比如乙腈或者甲苯等)，其他的各个通道可以分别独立或者交叉连接不同或相同的储备液，不会出现交叉污染的现象。图1和图4中各储液瓶51的连接方式只为简单示意，并未画出所有储液瓶51的连接管道，本领域技术人员可以依据本发明提供的技术领域结合本领域公知常识得到具体的管路连接结构图。
一般根据实验需要进样量小于或者接近1mL的连接第一多通道切换阀21，大于或者接近1mL的连接第二多通道切换阀22，多通道切换阀种的每个通道还需要和各个储液瓶51内的物质一一对应。而惰性气体存储器11则通过减压阀和调压过滤器12依次降压并过滤使用，起到提供正压和清洗管路的作用。
上述定量模块3包括：注射泵单元31、压力传感器32、流量计33和第二电磁阀单元34。
所述注射泵单元31的入口通过管路与所述取样通道切换模块2连接。所述注射泵单元31的出口通过管路与所述流量计33连接。所述流量计33通过管路与所述处置模块4连接。所述第二电磁阀单元34设置在所述流量计33与所述处置模块4的连接管路上。所述压力传感器32设置在所述注射泵单元31与所述流量计33的连接管路上。所述第二电磁阀单元34、所述压力传感器32和所述流量计33均与所述上位机电连接。
注射泵单元31包括：第一注射泵311和第二注射泵312。
所述第一注射泵311通过管路与所述第一多通道切换阀21中的一通道连 接。所述第二注射泵312通过管路与所述第二多通道切换阀22中的一通道连接。所述第一注射泵311的量程小于所述第二注射泵312的量程。
为保证进样的准确度，本发明提供的整个进样系统低于或者接近1mL的进样量时，由小量程注射泵(即第一注射泵311)连接的管路进样。高于或者接近1mL的进样量时，由大量程注射泵(即第二注射泵312)连接的管路进样，两条管路先平行进行后合二为一进入反应器中。注射泵上的注射器可以更换，最小500uL，最大25mL，且可以模块化增加切换阀和注射泵的数量进行拓展。每一条管路都是注射泵提供进样动力。每一条管路都有各自的注射泵和后面的高精度流量计33协同配合，双重控制以保证进样的准确性，且注射泵和流量计33之间以流量计33的计量作为最终的进样量。进行该设置的原因一是因注射泵本身的精确度(1％)低于流量计33本身的精确度(2‰)。二是注射泵无法识别气泡或者有无储备液，而流量计33在气体和液体之间的计量差别较大，有气体通过时计量变化大能反馈到流量计33和注射泵的双重自我修正中。
上述处置模块4包括：新型反应器41、溶液管42和废液瓶43。
所述新型反应器41的进样口412和所述废液品的进液口均通过管路与所述第二电磁阀单元34连接。所述溶液管42通过管路与所述新型反应器41的排气口413连接。
所述第二电磁阀单元34用于当所述新型反应器41中溶液达到设定量时，关闭所述流量计33与所述新型反应器41间的连接管路，并开启所述流量计33与所述废液瓶43的连接管路。
在高精度流量计33控制满足需要的进样量后，紧挨着流量计33的电磁阀会将多余的待反应溶液立即切换到废液瓶43中，保证进入新型反应器41的进样量准确。每次进样后可以根据需要在上位机中编写是否进行管路清洗指令，管路清洗的废液亦进入到废液瓶43中。与新型反应器41的出气口相连接的是可以防倒吸的油泡器，这样做的目的是为了保证新型反应器41内气压正常且不会有外来气体或水蒸气进入该反应器种，进而达到整个自动进样系统的密闭性要求。
如图3所示，本发明采用的新型反应器41包括：瓶口411、瓶身415和 取样口414。
所述进样口412与所述瓶身415间呈设定角度。所述排气口413和所述进样口412以所述瓶口411的中心线为中心对称设置。
所述瓶身415由内及外依次包括反应内胆4151、温度循环层4152和真空层4153。所述反应内胆4151的胆底为圆弧形结构。
所述排气口413和所述取样口414均与所述反应内胆4151连通。所述取样口414设置在所述反应内胆4151底部。
基于上述内容，本发明提供的自动进样系统主要包括：惰性气体存储器11、调压过滤器12、各种电磁阀、各种定制储液瓶51、两个十通道切换阀、两个配备不同量程注射器的注射泵、压力传感器32、高精度流量计33和新型反应器41。以上个模块中各部件的连接关系如图1和图4所示。
本说明书中各个实施例采用递进的方式描述，每个实施例重点说明的都是与其他实施例的不同之处，各个实施例之间相同相似部分互相参见即可。
本文中应用了具体个例对本发明的原理及实施方式进行了阐述，以上实施例的说明只是用于帮助理解本发明的方法及其核心思想；同时，对于本领域的一般技术人员，依据本发明的思想，在具体实施方式及应用范围上均会有改变之处。综上所述，本说明书内容不应理解为对本发明的限制。

Claims (9)

  1. 一种自动进样系统，其特征在于，包括：惰性气体输送模块、取样通道切换模块、定量模块、处置模块、储液模块和上位机；
    所述储液模块和所述取样通道切换模块均通过管路与所述惰性气体输送模块连接；所述定量模块通过管路分别与所述取样通道切换模块和所述处置模块连接；所述储液模块通过管路与所述取样通道切换模块连接；
    所述惰性气体输送模块、所述取样通道切换模块和所述定量模块均与所述上位机电连接；
    所述惰性气体输送模块用于将内部存储的惰性气体分别通过管路输送给所述储液模块和所述取样通道切换模块；所述取样通道切换模块用于提取所述储液模块中存储的待反应溶液，并用于切换提取所述待反应溶液的通道；所述定量模块用于确定注入所述处置模块中的待反应溶液量；
    所述上位机用于控制所述惰性气体输送模块和所述定量模块的开启和关闭，并用于控制所述取样通道切换模块进行通道切换。
  2. 根据权利要求1所述的自动进样系统，其特征在于，所述惰性气体输送模块包括：惰性气体存储器、调压过滤器和第一电磁阀单元；
    所述惰性气体存储器通过管路分别与所述储液模块和所述取样通道切换模块连接；所述调压过滤器和第一电磁阀单元设置在所述惰性气体存储器与所述储液模块的连接管路上，或设置在所述惰性气体存储器与所述取样通道切换模块的连接管路上。
  3. 根据权利要求1所述的自动进样系统，其特征在于，所述储液模块包括N个储液瓶；
    每一所述储液瓶均与所述惰性气体输送模块通过管路连接；所述储液瓶的瓶底为锥形或弧形。
  4. 根据权利要求3所述的自动进样系统，其特征在于，所述储液瓶包括：第一通道口、第二通道口、第三通道口和瓶盖；
    所述第一通道口用于通过管路与所述取样通道切换模块连接；所述第二通道口用于通过管路与所述惰性气体输送模块连接；第三通道口用于排出所述储液瓶中的气体或液体；
    所述瓶盖与所述储液瓶的瓶口螺纹连接。
  5. 根据权利要求3所述的自动进样系统，其特征在于，所述取样通道切换模块包括：第一多通道切换阀和第二多通道切换阀；
    所述第一多通道切换阀通过管路与M个所述储液瓶连接；所述第二多通道切换阀通过管路与N-M个所述储液瓶连接。
  6. 根据权利要求5所述的自动进样系统，其特征在于，所述定量模块包括：注射泵单元、压力传感器、流量计和第二电磁阀单元；
    所述注射泵单元的入口通过管路与所述取样通道切换模块连接；所述注射泵单元的出口通过管路与所述流量计连接；所述流量计通过管路与所述处置模块连接；所述第二电磁阀单元设置在所述流量计与所述处置模块的连接管路上；所述压力传感器设置在所述注射泵单元与所述流量计的连接管路上；所述第二电磁阀单元、所述压力传感器和所述流量计均与所述上位机电连接。
  7. 根据权利要求6所述的自动进样系统，其特征在于，所述处置模块包括：新型反应器、溶液管和废液瓶；
    所述新型反应器的进样口和所述废液品的进液口均通过管路与所述第二电磁阀单元连接；所述溶液管通过管路与所述新型反应器的排气口连接；
    所述第二电磁阀单元用于当所述新型反应器中溶液达到设定量时，关闭所述流量计与所述新型反应器间的连接管路，并开启所述流量计与所述废液瓶的连接管路。
  8. 根据权利要求7所述的自动进样系统，其特征在于，所述新型反应器包括：瓶口、瓶身和取样口；
    所述进样口与所述瓶身间呈设定角度；所述排气口和所述进样口以所述瓶口的中心线为中心对称设置；
    所述瓶身由内及外依次包括反应内胆、温度循环层和真空层；所述反应内胆的胆底为圆弧形结构；
    所述取样口与所述反应内胆连通。
  9. 根据权利要求6所述的自动进样系统，其特征在于，所述注射泵单元包括：第一注射泵和第二注射泵；
    所述第一注射泵通过管路与所述第一多通道切换阀中的一通道连接；所述第二注射泵通过管路与所述第二多通道切换阀中的一通道连接；所述第一注射 泵的量程小于所述第二注射泵的量程。
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