CN1053296A - Integrated micro-pipe flow injection instrument and manufacturing process thereof - Google Patents

Integrated micro-pipe flow injection instrument and manufacturing process thereof Download PDF

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Publication number
CN1053296A
CN1053296A CN 90105013 CN90105013A CN1053296A CN 1053296 A CN1053296 A CN 1053296A CN 90105013 CN90105013 CN 90105013 CN 90105013 A CN90105013 A CN 90105013A CN 1053296 A CN1053296 A CN 1053296A
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pipe
sensor
flow injection
pvc
chemical sensor
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崔洪波
孙君燕
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Institute of Applied Ecology of CAS
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Institute of Applied Ecology of CAS
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Priority to CN 90105013 priority Critical patent/CN1053296A/en
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Abstract

A kind of integrated micro-pipe flow injection instrument is characterized in that various chemical sensors all adopt microminiaturization, pipeline structure, and the form with standard socket between each parts is connected by the main organic glass integrated package of being with the microtubule road.Because integrated micro-pipe system is made up of the plexiglass block that has pipeline of particular design, do not need plastic foil bonding on it, can use and ne-leakage for a long time.This analysis instrument not only volume is little, in light weight, and have fast measuring, sample trace, analysis cost is low, measurement range is wide, the precision advantages of higher.

Description

Integrated micro-pipe flow injection instrument and manufacturing process thereof
The invention belongs to the technical field of solution Continuous Flow Analysis, integrated flow injection analyzer of a kind of microminiaturization and manufacturing process thereof promptly are provided.
Flowing injecting analysis technology is that early seventies is by the Denmark chemist, J. the continuous analytical technology of a kind of solution (seeing United States Patent (USP) 4022575) founded of the Ru Qika (Ruzicka) and the E.H. Chinese gloomy (Hansen), it has that analysis speed is fast, precision is high, equipment and operating process are simple, save reagent and a series of advantage such as sample, wide adaptability, thereby is used widely.Nineteen eighty-three J, Ru Qika are bonded in the basic PH sensor of Polyvinylchloride (abbreviating PVC usually as) in the sensor socket of the microchannel system of being made up of plexiglass block that has semicircle pipeline and plastic foil again, so that flowing injecting analysis technology further is tending towards microminiaturized.Yet, owing to exist:
(1) plastic foil is peeled off and seepage solution by electrolyte solution etches such as acid, alkali for a long time easily;
(2) sensor manufacturing technology difficulty is big;
(3) the sensor kind is few and can not change;
(4) poor stability of instrument;
(5) serviceable life short etc., a series of weak points, thereby its range of application is subjected to bigger restriction.
The objective of the invention is promptly provides a kind of integrated microtubule flow injection analyzer and a series of microtubules road chemical sensor that is exclusively used on this analyser in order to develop microminiaturized and integrated flowing injecting analysis technology.
Integrated microtubule flow injection analyzer provided by the present invention is made up of parts such as chemical sensor, valve, sampling ring, static suppressor, pulse suppressors, it is characterized in that:
(1) various chemical sensors all adopt microminiaturization, pipeline structure;
(2) parts are connected with the organic glass integrated package on band microtubule road with the form of standard socket;
(3) between valve and sensor, be connected to stainless-steel tube and make static suppressor;
(4) between pump and valve, be connected to coil and make pulse suppressor.
The microtubule road chemical sensor that uses that matches with integrated microtubule flow injection analyzer provided by the present invention comprises: tubulose Ag/AgCl sensor, PVC base valinomycin potassium sensor; PVC base 3-n-octyl amine PH sensor, all-polymer parent tube shape ammonia gas sensor and glass capillary sodium sensor, they are formed by internal reference electrode, internal-filling liquid, sensitive membrane, runner pipe, it is characterized in that all kinds of chemical sensors all are designed to mini-type tubular circulation type structure of whole solid state, and (1) each chemical sensor forms cuboid outward, and two bottom sides has the groove (or tenon) that the tenon groove (or groove) with corresponding site on the main organic glass integrated package is meshed; (2) electrode is divided into two kinds of indicator electrode and contrast electrodes, and the runner pipe with integrated little three-way pipe structure links between the two; (3) little three-way pipe is made by the PVC material.
Because the system of the integrated micro-pipe among the present invention is made up of the plexiglass block that has pipeline of particular design, do not need plastic foil bonding on it, simple in structure firm, can use for a long time and do not have a solution phenomenon of osmosis.When design, consider the dynamic conditions of fluid, both made compact conformation as far as possible, eliminate pipeline vibration, move influence, reduce dispersion degree, improve sampling rate, keep liquid stream stable current potential.Integrated micro-pipe flow injection instrument provided by the present invention, the influence that can avoid sensor sensing film surface alternation of wetting and drying, thermograde changes and wash the film surface state variation that causes keeps stability and the reappearance measured; In addition, owing between valve and sensor, be connected to stainless-steel tube, when having eliminated the pump rotation, the influence that produces static; At pump and valve coil is arranged indirectly, eliminated the influence that produces pulse when pump rotates.Link to each other with waste liquid with little three-way pipe between indicator electrode and contrast electrode, not only finished the ionic conduction in the solution but also can eliminate the influence of the liquid junction potential of contrast electrode.The utility model has been given full play to the measuring ability of flow injection solution-treated function and chemical sensor, has solved the potential drifting problem, has simplified amount liquid, moves liquid, a series of experimental arrangements such as dilution, constant volume, stirring and detection.Compare with existing flow injection analyzer, integrated micro-pipe flow injection instrument provided by the present invention has that volume is little, sound construction, easy to assembly, simple to operate, measure fast (≈ 200 samples/hour) accurately (± 0.1mV), sample and reagent consumption few (80 microlitre), with low cost, a series of advantage such as applicability is wide, can be applicable to environmental protection, agricultural, industry, clinical examination, be particularly suitable for process control and continuous monitoring.
The structure of its most preferred embodiment of integrated micro-pipe flow injection instrument provided by the present invention as shown in Figure 1, Fig. 2 then is its flow injection process flow diagram; And its chemical sensor is respectively as Fig. 3-shown in Figure 7, and wherein Fig. 3 is PVC base valinomycin potassium sensor construction figure, and Fig. 4 be the basic 3-n-octyl amine of PVC PH sensor construction figure; Fig. 5 is tubulose Ag/AgCl sensor construction figure; Fig. 6 is an all-polymer base ammonia gas sensor structural drawing; Fig. 7 is glass capillary sodium sensor construction figure.In Fig. 1-7, (V) valve; (C) current-carrying; (B) damping fluid; (I) indicator electrode; (R) contrast electrode; (L) coil; (S) sampling ring; (G) stainless-steel tube; (W) waste liquid; (P) peristaltic pump; (1) Ag/Agcl internal reference electrode; (2) internal-filling liquid; (3) sensitive membrane; (4) runner pipe; (5) organic glass body; (6) ventilated membrane; (7) pvc pipe aperture.
Embodiment below in conjunction with Fig. 1-7 pair integrated micro-pipe flow injection instrument provided by the present invention makes briefly bright.Earlier the main organic glass integrated package of flow injection analyzer is gone up pore as pipeline with the drilling machine brill, and hold groove or tenon standard interface successfully as chemical sensor at the position of settling chemical sensor.When making microtubule road chemical sensor, make earlier tubulose Ag/AgCl sensor as follows, get one of long 12 millimeters, wide 3.5 millimeters, thick 0.03 millimeter silver foil, polishing back is that 1.2 millimeters stainless pin is rolled into tubulose with silver foil by means of diameter, uses thin filamentary silver (1) to weld and draw lead in the middle, and insert in the runner pipes (4) at two ends, use epoxy sealing, the tetrahydrofuran solution of Dropwise 5 %PVC is 5~6 again, and outside formation PVC film and runner pipe are connected as a single entity.Then respectively with 5% ammoniacal liquor, 5%NaClO 2Phosphate buffer (PH6.5), 0.1NHCl solution be current-carrying, by peristaltic pump (pump speed 2.0 ml/min), above-mentioned solution is pumped into the silver pipe successively, time was respectively 1,3,24 hour, be installed in then in the prior plexiglass block (5) that has bored pore (or having groove), will be up and down two plexiglass blocks compress.The manufacturing of other chemical sensor and install similarly with it all is that pvc pipe that the first centre that prepared beforehand is good has sensitive membrane (3) is installed in the organic glass hole and (sees Fig. 3-7), and is good with epoxy sealing, injects internal-filling liquid (K in the internal pore of hole +Electrode be silver chloride saturated 10 -2MKCl, Na +Electrode be silver chloride saturated 10 -2MNaCl, PH electrode are 1.0M citric acid-2.7MNaOH-0.01MNaCl, and the NH3 electrode is 0.1MNH 4Cl), insert the Ag/AgCl silk, seal as contrast electrode.Perhaps will have the pvc pipe of ventilated membrane (6) and the pvc pipe of middle (7) with holes and insert middle having in the pvc pipe of 3-n-octyl amine PH sensitive membrane simultaneously, and make PH sensitive membrane and ventilated membrane be close to the suitable ammonia sensitive electrode of making.At last above-mentioned each parts are placed the prior main plexiglass block that has bored pore or held groove successfully, two body plexiglass blocks compress up and down, and process the tenon (or groove) that the groove (or tenon) with the main organic glass integrated package of flow injection analyzer matches in the little plexiglass block bottom of chemical sensor, each chemical sensor is coupled together with main organic glass integrated package with tenon (or groove), and will have 80 microlitre sampling ring (S), the miniature valve that diameter is 1.7 centimetres (V), stainless-steel tube (G) and coil (L) are fixed on the main organic glass integrated package that has pore and standard socket, and then integrated micro-pipe flow injection instrument is promptly assembled and finished.Stainless-steel tube is answered ground connection during use.
Analyze potassium, sodium, chlorine with integrated micro-pipe flow injection instrument provided by the present invention, per hour can measure 80 samples totally 240 projects, and can print analysis result (the m moies/L of unit) immediately, each sample only needs 80 microlitres, compare with conventionals method of analysis such as flame photometries, have fast measuring, sample trace, low, the wide (K of measurement range of analysis cost +1.0-10.0m mo|es/L, Na +20-190m mo|es/L, Cl -20-190m mo|es/L), precision height (K +± 0.1m mo|es/L, Na +± 1.0m mo|es/L, Cl -± advantage such as 2.0mmo|es/L), the volume of instrument own little (300 * 300 * 350mm), (complete machine adds the about 10kg of annex) in light weight, get rid of combustion gas, be suitable for large-scale popularization and use.

Claims (4)

1, a kind of integrated micro-pipe flow injection instrument of being made up of chemical sensor (I or R), miniature valve (V), sampling ring (S), static suppressor (G), each parts of pulse suppressor (L) is characterized in that:
A) various chemical sensors all adopt microminiaturization, pipeline structure;
B) form with standard socket is connected by the main organic glass integrated package of being with the microtubule road between each parts;
C) between miniature valve and chemical sensor, be connected to stainless-steel tube (G) and make static suppressor;
D) between peristaltic pump and miniature valve, be connected to coil (L) and make pulse suppressor.
2, a kind of for assembling the microtubule road chemical sensor that integrated micro-pipe flow injection instrument is used, comprising: tubulose Ag/AgCl sensor; The plain potassium sensor of PVC base valine, PVC base 3-octylame PH sensor; All-polymer parent tube shape ammonia gas sensor and glass capillary sodium sensor, they are formed by Ag/AgCl internal reference electrode (1), internal-filling liquid (2), sensitive membrane (3), runner pipe (4), plexiglass block (5) etc., it is characterized in that each chemical sensor all is designed to mini-type tubular circulation type structure of whole solid state; And:
A) each chemical sensor is a cuboid, and two bottom sides has the groove (or tenon) that the tenon (or groove) with corresponding site on the main organic glass integrated package is meshed;
B) electrode is divided into two kinds of indicator electrode (I) and contrast electrodes (R), adopts integrated little three-way pipe structure and stream pipe to link between them;
C) runner pipe is made with the PVC material.
3, a kind of manufacture method that is exclusively used in integrated micro-pipe flow injection instrument microtubule road chemical sensor is characterized in that it is made of following four procedures:
A) pore or groove in plexiglass block, have been bored;
B) centre that prepared beforehand is the good pvc pipe that has a sensitive membrane (3) is installed in the hole of plexiglass block, uses epoxy sealing;
C) in the internal pore of hole, inject internal-filling liquid (2), and insert the Ag/AgCl silk and seal as electrode;
D) plexiglass block with upper and lower two bodies compresses, and processes the tenon (or groove) that the groove (or tenon) with flow injection analyzer master organic glass integrated package matches in its underpart.
4, by the described chemical sensor manufacture method of claim 3, it is characterized in that said centre has the pvc pipe of sensitive membrane, be inserted with the pvc pipe of the pvc pipe of band ventilated membrane (6) or middle (7) with holes in the middle of also can being and post the pvc pipe of 3-n-octyl amine PH sensitive membrane.
CN 90105013 1990-01-09 1990-01-09 Integrated micro-pipe flow injection instrument and manufacturing process thereof Pending CN1053296A (en)

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CN 90105013 CN1053296A (en) 1990-01-09 1990-01-09 Integrated micro-pipe flow injection instrument and manufacturing process thereof

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Application Number Priority Date Filing Date Title
CN 90105013 CN1053296A (en) 1990-01-09 1990-01-09 Integrated micro-pipe flow injection instrument and manufacturing process thereof

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CN1053296A true CN1053296A (en) 1991-07-24

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100465638C (en) * 2006-09-15 2009-03-04 清华大学 Flow injection analysis based electrochemistry analyzer
CN101441178B (en) * 2005-07-15 2010-09-22 北京吉天仪器有限公司 Flow injection colorimetry cyanogen measuring instrument for measuring cyanide content
CN106541711A (en) * 2016-10-12 2017-03-29 华中科技大学 A kind of parallel synthesizer and synthetic method of air-sensitive film transferred based on microdroplet premix

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101441178B (en) * 2005-07-15 2010-09-22 北京吉天仪器有限公司 Flow injection colorimetry cyanogen measuring instrument for measuring cyanide content
CN100465638C (en) * 2006-09-15 2009-03-04 清华大学 Flow injection analysis based electrochemistry analyzer
CN106541711A (en) * 2016-10-12 2017-03-29 华中科技大学 A kind of parallel synthesizer and synthetic method of air-sensitive film transferred based on microdroplet premix

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