CN102297795B - Computer-controlled automatic liquid micro-extraction device - Google Patents
Computer-controlled automatic liquid micro-extraction device Download PDFInfo
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- CN102297795B CN102297795B CN 201110205165 CN201110205165A CN102297795B CN 102297795 B CN102297795 B CN 102297795B CN 201110205165 CN201110205165 CN 201110205165 CN 201110205165 A CN201110205165 A CN 201110205165A CN 102297795 B CN102297795 B CN 102297795B
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Abstract
The invention provides a computer-controlled automatic liquid micro-extraction device. The device comprises a computer, an injection pump, a switch valve, a hollow fibre membrane, a stirring device, a peristaltic pump and an ultrasonic device. The switch valve is provided with at least four joints. The injection pump is connected with the first joint of the switch valve through a connection pipe. A receptor solution bottle and a sampling bottle are respectively connected with other joints of the switch valve through a connection pipe. The hollow fibre membrane is U-shaped. When the device is used, two ends of the hollow fibre membrane are respectively connected with other joints of the switch valve through the connection pipe; the U-shaped bottom of the hollow fibre membrane is inserted in a liquid sample bottle; the liquid sample bottle is placed on the stirring device; one end of a liquid absorption pipe is inserted in the liquid sample bottle; the other end of the liquid absorption pipe is connected with one end of the peristaltic pump; the other end of the peristaltic pump is connected with a solid sample bottle placed in the ultrasonic device; and the computer is connected with the injection pump and a micro-processor in the switch valve through a serial interface. The device has the advantages of high automation degree, simple and convenient operation and good repeatability and is easily and cooperatively used with a detection instrument.
Description
Technical field
The invention belongs to chemical analysis field, be specifically related to the computer-controlled automatic hollow fiber membrane liquid-phase micro extraction device of a kind of employing, be used for the sample pretreatment of the various organic micro-pollutants of complex environment sample.
Background technology
Along with the development of analytical chemistry research, more and more higher to the requirement of Sample Pretreatment Technique Used.Traditional Sample Pretreatment Technique Used is mainly liquid-liquid extraction, and complex operation is time-consuming, and needs to consume a large amount of virose organic solvents, is difficult to realize robotization.
Liquid-phase micro-extraction is a kind of novel Sample Pretreatment Technique Used.This technology has overcome many deficiencies of traditional liquid-liquid technique, only uses micro updating even receive the organic solvent of upgrading to extract, and has adapted to the requirement of the microminiaturized development of modern analysis science.Liquid-phase micro-extraction is used for the pre-service of various complex environment samples, treasury gets, concentrate, purify and be integrated, reduced the sample pretreatment step, have simple to operate, enrichment times is large, extraction efficiency is high, is convenient to realize the advantage of coupling, is a kind of simple and convenient, environmentally friendly green Sample Pretreatment Technique Used.The most liquid-phase micro-extraction is manual control, and the manually-operated amount is large, and reappearance is relatively poor.
Summary of the invention
The object of the invention is to provide a kind of computer-controlled automatic liquid micro-extraction device, and this plant automation degree is high, and easy and simple to handle, favorable reproducibility is easy to and the detecting instrument coupling.
A kind of computer-controlled automatic liquid micro-extraction device provided by the invention is characterized in that this device comprises computing machine, syringe pump, transfer valve, hollow-fibre membrane, stirring apparatus, peristaltic pump and Vltrasonic device; Transfer valve is with at least five interfaces, and syringe pump is connected with the first interface of transfer valve by connecting pipe, and acceptor phase solution bottle and sample injection bottle connect respectively second, third interface of transfer valve by connecting pipe, and hollow-fibre membrane is U-shaped; During use, the two ends of hollow-fibre membrane link to each other with the 4th, the 5th interface of transfer valve by connecting pipe respectively; The fluid sample bottle is inserted in the U-shaped bottom of hollow-fibre membrane, and the fluid sample bottle is placed on the stirring apparatus, and an end of pipette inserts in the fluid sample bottle, and the other end connects an end of peristaltic pump, and the peristaltic pump other end connects the solid sample bottle that is placed in the Vltrasonic device; The microprocessor that computing machine is connected with transfer valve by serial line interface and syringe pump is connected.
Remarkable advantage of the present invention is embodied in:
(1) hollow-fibre membrane of the present invention's employing has porous membranes, thereby organic solvent and extract are kept apart, make in the hole of extraction process on polymeric membrane and carry out, thereby effectively prevent organic solvent emulsifying, guarantee the stable of organic solvent, reduced required consumption of organic solvent.Because the surface pore of polymeric membrane is many, provide very large contact area again, thereby improved extraction efficiency, save extraction time, strengthen simultaneously the stability of organic solvent liquid, had higher enrichment times, and can play to a certain extent the effect that purifies and avoid matrix to disturb.
But the sample direct injection analysis need not purification separation after the extraction, is easy to realize the purification enrichment of sample, improves sensitivity for analysis.The hollow-fibre membrane relative low price, cross pollution is avoided in disposable use.
(2) this device has adopted the high precision syringe pump to flow driver part as liquid, can draw in proportion arbitrarily volume and analyze.Thereby accuracy and the Systems balanth of liquid-phase micro-extraction have been improved.Syringe pump inside has microprocessor, and has and be easy to mutual external serial interface.By serial communication protocol, carry out communication through serial line interface and computing machine, can finish the feedback of steering order and syringe state.
(3) transfer valve selected of this device has six paths, has satisfied the needs that the liquid flow path of liquid-phase micro-extraction system switches.Transfer valve inside has microprocessor, and have and be easy to mutual external serial interface, pass through serial communication protocol, carry out communication through serial line interface and syringe pump, can finish and switch each liquid flow path of liquid-phase micro-extraction system and select different liquid stream modes, realize the stable control of transfer valve.
(4) syringe pump all has the interface that links to each other with the standard connecting pipe with transfer valve in this device, can realize good connection, guarantees impermeability.Hollow-fibre membrane links to each other with connecting pipe and can realize loading and unloading, and sample bottle is provided with stirring apparatus and can improves extraction efficiency.
(5) computer control software of this device integrated with satisfied the hardware of two kinds of serial communication protocols and the repertoire of data collecting card communication, therefore can pass through easily serial line interface at native system, the communication of realization and syringe pump and transfer valve, finish the control to syringe pump and transfer valve, thereby guarantee each result's accuracy and repeatability, reduced personal error.This control software can the powerful intelligent control function of computer, to extraction process carry out dynamically, the automatic control of static and any liquid stream mode, the accuracy of raising sample extraction.
Description of drawings
Fig. 1 is the structural representation of a kind of embodiment of computer-controlled automatic liquid micro-extraction device, and wherein 1 is computing machine; 2 is syringe pump; 3 is transfer valve; 4 is acceptor phase solution bottle; 5 is hollow-fibre membrane; 6 is stirring apparatus; 7 is the fluid sample bottle; 8 is sample injection bottle; 9 is waste liquid bottle; 10 is the cleaning fluid bottle; 11 is peristaltic pump; 12 is the solid sample bottle; 13 is Vltrasonic device.
Fig. 2 is computer control subprogram process flow diagram.
Embodiment
Below by by embodiment the present invention being described in further detail, but following examples only are illustrative, and protection scope of the present invention is not subjected to the restriction of these embodiment.
As shown in Figure 1, apparatus of the present invention comprise computing machine 1, syringe pump 2, transfer valve 3, hollow-fibre membrane 5, stirring apparatus 6, peristaltic pump 11 and Vltrasonic device 13.
In this example, the replacement valve is six-way valve, with seven interfaces (middle an interface, on every side six interfaces).On the syringe pump 2 with two-port valve, an interface of two-port valve is used for draw solution or air, another interface is connected by the first interface of connecting pipe with transfer valve 3, four interfaces of other of transfer valve are connected with acceptor phase solution bottle 4, sample injection bottle 8, waste liquid bottle 9 and cleaning fluid bottle 10 by connecting pipe respectively, and hollow-fibre membrane 5 is U-shaped; During use, the two ends of hollow-fibre membrane 5 connect respectively other two interfaces of transfer valve by connecting pipe, wherein fluid sample bottle 7 is inserted in the U-shaped bottom of hollow-fibre membrane 5, fluid sample bottle 7 is placed on the stirring apparatus 6, one end of pipette inserts in the fluid sample bottle 7, the other end connects an end of peristaltic pump 11, and the peristaltic pump other end connects the solid sample bottle 12 that is placed in the Vltrasonic device 13.
Wherein, the topworks inside such as syringe pump and transfer valve have microprocessor, and self can by linking to each other with the serial line interface of computing machine, receive and carry out instruction with the serial communication function.
In the above-mentioned example, waste liquid bottle 9 or/and cleaning fluid bottle 10 also can arrange, transfer valve just can be wanted two interfaces (namely adopt with the four-way valve of five interfaces or with the five-way valve of six interfaces and get final product) less, can also increase as required and establish other liquid bottle, correspondingly select corresponding transfer valve.
Computing machine in this device is general personal computer; Syringe pump can be selected different precision as required with peristaltic pump; Transfer valve can be selected different kinds (four-way valve, five-way valve, six-way valve etc.) according to the needs of pipeline number; Computer control software can be selected as required; Hollow-fibre membrane can be selected variety classes (Kynoar, polyacrylonitrile, polysulfones, Polyvinylchloride, polypropylene, tygon etc.) according to determination object; Stirring apparatus can be magnetic stirring apparatus; Vltrasonic device can be ultrasonic cleaner; Acceptor phase solution bottle and sample extraction bottle can need to adopt the materials such as glass, plastics per sample.
This device can be realized the pre-service to complex environment liquid and solid sample, and its use procedure is:
(1) hollow-fibre membrane is cut into suitable length, dries after cleaning with solvent supersonic.It is for subsequent use to link to each other with connecting pipe.
(2) mounted hollow-fibre membrane is put into organic solvent and soaked, make organic solvent be full of the space of hollow-fibre membrane, blot the hollow-fibre membrane surface with filter paper.
(3) fluid sample: the hollow-fibre membrane that will blot the surface all immerses in the sample, by the syringe pump in the computer control micro-extraction device of liquid phase, transfer valve, acceptor phase solution is injected hollow-fibre membrane, the flow velocity of control acceptor phase, the residence time and liquid stream mode; And rotating speed and the temperature of regulating stirring apparatus are carried out liquid-phase micro-extraction.
Solid sample: will be in the solid sample add a certain amount of aqueous solution, mixing covers tightly to be put into the groove type ultrasonic device behind the lid and extracts, after extraction finishes, by the computer control peristaltic pump with in the complete filling liquid sample bottle of the semi-solid sample in the extraction flask.The fluid sample bottle is placed under the hollow-fibre membrane, make hollow-fibre membrane all immerse in the sample, by the syringe pump in the computer control micro-extraction device of liquid phase, transfer valve, acceptor phase solution is injected hollow-fibre membrane, the flow velocity of control acceptor phase, the residence time and liquid stream mode; And rotating speed and the temperature of regulating stirring apparatus are carried out liquid-phase micro-extraction.
(4) after extraction finishes, by computer control the acceptor phase solution in the hollow-fibre membrane is all injected sample injection bottle, treat Instrument measuring;
(5) quantitatively suck cleaning solution, promote liquid stream and clean sampling valve and pipeline, in order to next time extraction.
Further specify the using method of this device below in conjunction with embodiment.
Embodiment 1
High precision syringe pump VersaPump6 (V6) syringe (minimum extraction amount is 0.104 μ L, and precision is 0.06%) that adopts U.S. Kloehn company to be promoted by stepper motor; Transfer valve (six-way valve) the 50120 Intellect valve of U.S. Kloehn company; Serial line interface RS232; General purpose personal computer; The LabVIEW computer control software; Polypropylene hollow fiber membrane (external diameter 1000 μ m, internal diameter 600 μ m, tunica fibrosa void size 0.2 μ m); Vltrasonic device is ultrasonic cleaning machine; Acceptor phase solution bottle and fluid sample bottle all adopt 100mL vinyon bottle; The extraction sample is for containing perfluor organic acid water sample.Concrete grammar is as follows:
(1) at first hollow-fibre membrane is cut into 10cm, puts into the impurity that acetone ultrasonic cleaning 30min removes hollow-fibre membrane, after drying and volatilizing is removed acetone, link to each other for subsequent use with the teflon connecting pipe.
(2) mounted hollow-fibre membrane is put into n-octyl alcohol and soak 5min, make n-octyl alcohol be full of the space of hollow-fibre membrane.
(3) 100mL perfluor organic acid water sample is directly put into the fluid sample bottle, regulate water sample pH=2 with hydrochloric acid, the target extract is existed with neutral molecule, after the adding magnetic stir bar, place magnetic stirring apparatus pallet central authorities.
The extraction flask that (4) sample will be housed places under the hollow-fibre membrane, makes hollow-fibre membrane all immerse sample solution.Then by computer software LabVIEW control syringe pump and six-way valve, quantitatively draw 52 μ L ammonium acetate acceptor phase solution (pH=11), coutroi velocity (10 μ L/s), stays static time (20min), the ammonium acetate solution of drawing is injected hollow-fibre membrane fully, and the solution after will extracting pushes in the sample injection bottle.During extraction, start magnetic stirring apparatus, regulate the rotating speed (1300rpm) and temperature (20 ℃) of stirrer, carry out liquid-phase micro-extraction, the target extract at first is extracted in the n-octyl alcohol, then is stripped in the ammonium acetate solution.The control flow chart of computer software as shown in Figure 2.
(5) after extraction finishes, by computer software control syringe pump and six-way valve, the ammonium acetate solution in the hollow-fibre membrane is all injected sample injection bottle, treat Instrument measuring.
(6) quantitatively suck ammonium acetate solution as cleaning solution, promote liquid stream and clean sampling valve and pipeline, in order to next time extraction.
Utilize this device can detect that perfluor organic acid concentration range is in the water sample: 0.01-50 μ g/L; Recovery scope is 80.4-92.9%; The relative standard deviation scope is: 4.1-5.9%.
Adopt Pvdf Microporous Hollow Fiber Membrane (external diameter 800 μ m, internal diameter 600 μ m, tunica fibrosa void size 0.2 μ m); Acceptor phase solution bottle and fluid sample bottle all adopt 100mL vinyon bottle; The extraction sample is the chlorobenzene in the water sample.Concrete grammar is as follows:
(1) at first hollow-fibre membrane is cut into 15cm, puts into the impurity that ethanol ultrasonic cleaning 30min removes hollow-fibre membrane, after drying and volatilizing is removed ethanol, link to each other for subsequent use with the teflon connecting pipe.
(2) 100mL chlorobenzene water sample is directly put into the fluid sample bottle, after the adding magnetic stir bar, place magnetic stirring apparatus pallet central authorities.
The extraction flask that (3) sample will be housed places under the hollow-fibre membrane, makes hollow-fibre membrane all immerse sample solution.Then by computer software control syringe pump and six-way valve, quantitatively draw the n-octyl alcohol of 65 μ L, coutroi velocity (10 μ L/s), stays static time (20min), the n-octyl alcohol of drawing injected fully and by hollow-fibre membrane, and the solution after will extracting pushes in the sample injection bottle.Start magnetic stirring apparatus, regulate the rotating speed (400rpm) and temperature (20 ℃) of stirrer, carry out liquid-phase micro-extraction, the target extract is extracted in the n-octyl alcohol by the micropore of hollow-fibre membrane.The control flow chart of computer software as shown in Figure 2.
(4) after extraction finishes, by computer software control syringe pump and six-way valve, the n-octyl alcohol in the hollow-fibre membrane is all injected sample injection bottle, treat Instrument measuring.
(5) quantitatively suck n-octyl alcohol, promote liquid stream and clean sampling valve and pipeline, in order to next time extraction.
The concentration range of utilizing this device can detect chlorobenzene in the water sample is: 0.1-40 μ g/L; Recovery scope is 80.9-95.7%; The relative standard deviation scope is: 3.2-16.8%.
Adopt LONGER peristaltic pump (model BT100-2J); Pvdf Microporous Hollow Fiber Membrane; The material of connecting pipe is teflon; Acceptor phase solvent bottle and liquid, solid sample bottle all adopt 100mL vinyon bottle; The extraction sample is the chlorobenzene in the pedotheque.Concrete grammar is as follows:
(1) at first hollow-fibre membrane is cut into 15cm, puts into the impurity that ethanol ultrasonic cleaning 30min removes hollow-fibre membrane, after drying and volatilizing is removed ethanol, link to each other for subsequent use with the teflon connecting pipe.
(2) the 10.0mL aqueous solution will be added in the 1.0g chlorobenzene pedotheque, mixing covers tightly to be put into groove type ultrasonic device (power 100W) behind the lid and extracts, the extraction 30min after, by peristaltic pump with in the complete filling liquid sample bottle of the semi-solid sample in the extraction flask.
The extraction flask that (3) sample will be housed places under the hollow-fibre membrane, makes hollow-fibre membrane all immerse sample solution.Then by computer software control syringe pump and six-way valve, quantitatively draw the n-octyl alcohol of 65 μ L, coutroi velocity (10 μ L/s), stays static time (20min), the n-octyl alcohol of drawing injected fully and by hollow-fibre membrane, and the solution after will extracting pushes in the sample injection bottle.Start magnetic stirring apparatus, regulate the rotating speed (400rpm) and temperature (30 ℃) of stirrer, carry out liquid-phase micro-extraction, the target extract is extracted in the n-octyl alcohol by the micropore of hollow-fibre membrane.The control flow chart of computer software as shown in Figure 2.
(4) after extraction finishes, by computer software control syringe pump and six-way valve, the n-octyl alcohol in the hollow-fibre membrane is all injected sample injection bottle, treat Instrument measuring.
(5) quantitatively suck n-octyl alcohol, promote liquid stream and clean sampling valve and pipeline, in order to next time extraction.
The concentration range of utilizing this device can detect chlorobenzene in the soil sample is: 0.01-1.5 μ g/g; Recovery scope is 72.1-90.7%; The relative standard deviation scope is: 4.2-10.8%.
The above is preferred embodiment of the present invention, but the present invention should not be confined to the disclosed content of this embodiment and accompanying drawing.So everyly do not break away from the equivalence of finishing under the spirit disclosed in this invention or revise, all fall into the scope of protection of the invention.
Claims (4)
1. a computer-controlled automatic liquid micro-extraction device is characterized in that, this device comprises computing machine (1), syringe pump (2), transfer valve (3), hollow-fibre membrane (5), stirring apparatus (6), peristaltic pump (11) and Vltrasonic device (13);
Transfer valve (3) is with at least five interfaces, syringe pump (2) is connected by the first interface of connecting pipe with transfer valve (3), acceptor phase solution bottle (4) and sample injection bottle (8) connect respectively second, third interface of transfer valve by connecting pipe, hollow-fibre membrane (5) is U-shaped; During use, the two ends of hollow-fibre membrane (5) link to each other with the 4th, the 5th interface of transfer valve (3) by connecting pipe respectively; Fluid sample bottle (7) is inserted in the U-shaped bottom of hollow-fibre membrane (5), fluid sample bottle (7) is placed on the stirring apparatus (6), one end of pipette inserts in the fluid sample bottle (7), the other end connects an end of peristaltic pump (11), and the peristaltic pump other end connects the solid sample bottle (12) that is placed in the Vltrasonic device (13); Computing machine (1) is connected 3 with syringe pump (2) with transfer valve by serial line interface) in microprocessor be connected;
Described computer-controlled automatic liquid micro-extraction device is used for the pre-service to complex environment liquid and solid sample, and its use procedure is:
(1) hollow-fibre membrane is cut into suitable length, dries after cleaning with solvent supersonic; It is for subsequent use to link to each other with connecting pipe;
(2) mounted hollow-fibre membrane is put into organic solvent and soaked, make organic solvent be full of the space of hollow-fibre membrane, blot the hollow-fibre membrane surface with filter paper;
(3) fluid sample: the hollow-fibre membrane that will blot the surface all immerses in the sample, by the syringe pump in the computer control micro-extraction device of liquid phase, transfer valve, acceptor phase solution is injected hollow-fibre membrane, the flow velocity of control acceptor phase, the residence time and liquid stream mode; And rotating speed and the temperature of regulating stirring apparatus are carried out liquid-phase micro-extraction;
Solid sample: will be in the solid sample add a certain amount of aqueous solution, mixing covers tightly to be put into the groove type ultrasonic device behind the lid and extracts, after extraction finishes, by the computer control peristaltic pump with in the complete filling liquid sample bottle of the semi-solid sample in the extraction flask; The fluid sample bottle is placed under the hollow-fibre membrane, make hollow-fibre membrane all immerse in the sample, by the syringe pump in the computer control micro-extraction device of liquid phase, transfer valve, acceptor phase solution is injected hollow-fibre membrane, the flow velocity of control acceptor phase, the residence time and liquid stream mode; And rotating speed and the temperature of regulating stirring apparatus are carried out liquid-phase micro-extraction;
(4) after extraction finishes, by computer control the acceptor phase solution in the hollow-fibre membrane is all injected sample injection bottle, treat Instrument measuring;
(5) quantitatively suck cleaning solution, promote liquid stream and clean sampling valve and pipeline, in order to next time extraction.
2. a kind of computer-controlled automatic liquid micro-extraction device according to claim 1 is characterized in that, this device also comprises waste liquid bottle (9), and transfer valve is with six interfaces, and waste liquid bottle (9) links to each other with the 6th interface of transfer valve by connecting pipe.
3. a kind of computer-controlled automatic liquid micro-extraction device according to claim 1 is characterized in that, this device also comprises cleaning fluid bottle (10), and transfer valve is with six interfaces, and cleaning fluid bottle (10) links to each other with the 6th interface of transfer valve by connecting pipe.
4. a kind of computer-controlled automatic liquid micro-extraction device according to claim 1, it is characterized in that, this device also comprises waste liquid bottle (9) and cleaning fluid bottle (10), transfer valve is with seven interfaces, and waste liquid bottle (9) links to each other with the 6th, the 7th interface of transfer valve by connecting pipe respectively with cleaning fluid bottle (10).
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| CN102974127B (en) * | 2012-11-23 | 2017-12-08 | 中国计量学院 | A kind of hollow-fibre membrane micro-extraction apparatus and its application |
| CN106018856B (en) * | 2016-08-09 | 2017-06-30 | 上海昂林科学仪器有限公司 | Anion surfactant automatic analysing apparatus |
| CN107478770B (en) * | 2017-06-19 | 2020-03-24 | 中国原子能科学研究院 | Extraction/back extraction dynamics research device based on rising single-liquid-drop method |
| CN109655326B (en) * | 2018-11-27 | 2021-09-28 | 中国科学院合肥物质科学研究院 | Soil leaching method |
| CN110124353A (en) * | 2019-05-23 | 2019-08-16 | 中仪科立河北科技有限公司 | A kind of Full Automatic Liquid liquid extracting and purifying device and method |
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