CN105973810A - Miniature liquid reaction device and use method thereof - Google Patents
Miniature liquid reaction device and use method thereof Download PDFInfo
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- CN105973810A CN105973810A CN201610408895.1A CN201610408895A CN105973810A CN 105973810 A CN105973810 A CN 105973810A CN 201610408895 A CN201610408895 A CN 201610408895A CN 105973810 A CN105973810 A CN 105973810A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/03—Cuvette constructions
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6402—Atomic fluorescence; Laser induced fluorescence
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/03—Cuvette constructions
- G01N2021/0325—Cells for testing reactions, e.g. containing reagents
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a miniature liquid reaction device. The miniature liquid reaction device comprises a main separation tube, a sample injection tube and reagent injection tubes. A reaction tube is connected to the main separation tube in a matched mode, a gas-liquid separator is formed at one end of the reaction tube and located in the main separation tube, and the sample injection tube and the reagent injection tubes are both connected with the reaction tube. The main separation tube is provided with a gas inlet, a gas outlet and a liquid outlet, and a bladeless fan is further arranged in the main separation tube and located between the gas-liquid separator and the gas inlet. By means of the miniature liquid reaction device, full reactions of micro samples and reagents can be guaranteed, the requirements for the stability and repeatability of test data can be met to the maximum, and meanwhile full and complete gas-liquid separation after reactions can be guaranteed.
Description
Technical field
The present invention relates to detect device field, particularly relate to a kind of minisize liquid reaction unit and using method thereof.
Background technology
Generation hydride atoms spectrum analysis is an emerging field of atomic spectroscopic analysis, and this method has survey
The most highly sensitive fixed, the advantage such as mutual interference is few, be widely used in environment, food, medical supplies, health and epidemic prevention and
The fields such as metallurgical geology.The method is to be reacted with reducing agent by sample solution, makes element to be measured in sample solution
Ion generate gaseous hydride (Hg is reduced to metallic vapour), the reaction of Element generation hydride to be measured is such as
Under:
Mn++KBH4+HCl+3H2O-------MHn+KCl+H3BO3+H2
Hydride generator can be with atomic absorption analyzer, atomic fluorescence spectrophotometer, ICP-AES, ICP-MS
Support the use in instrument, in some way the hydride gas that reaction produces is sent into atomizer or ICP
Plasmatorch is measured.This device can be used for measuring trace As in sample solution, Sb, Bi, Se, Te,
The mensuration of the elements such as Ge, Sn, Pb, Hg.
Micro liquid reaction unit of the prior art typically can support trace test solution and reagent conveniently and efficiently
Reaction, the such as micro multifunctional sample-feeding device of Patent No. 200420084256, its simple in construction,
And analysis time and reagent can be saved, and measure the kind of element and scope is the biggest.But this technical scheme
Yet suffer from two large problems.First the design of its reaction tube is it cannot be guaranteed that the reaction of each sample and reagent is filled the most very much
Divide and sample is had waste, cause test result unstable, repeatable poor, affect the use of test data;
Secondly this device is in collecting the gas process that reaction produces, and (waste liquid is inverse often to collect partial reaction waste liquid
Stream, nitrogen and argon by being passed through are brought into), not only to associated with detecting instrument damaged, simultaneously the most also can between
Ground connection affects measurement result.And above-mentioned two big technical problems, always such micro liquid reaction unit urgently solves
Technical problem certainly and improvement difficult point.
Summary of the invention
The present invention solves a kind of efficient minisize liquid reaction unit that the problems referred to above of the prior art propose,
Ensure that fully carrying out of every secondary response, meet the stable and repeatable of test data to greatest extent, with
Time ensure that substantially entirely gas-liquid separation after reaction.
In order to realize above-mentioned technical purpose, the technical solution used in the present invention is:
A kind of minisize liquid reaction unit, separates pipe, sample feeding pipe and reagent sample feeding pipe, above-mentioned master including main
Separating pipe and be connected with reaction tube, one end of above-mentioned reaction tube is formed with gas-liquid separator, above-mentioned gas-liquid separation
Device is inside main separation pipe, and sample feeding pipe is all connected with above-mentioned reaction tube with reagent sample feeding pipe, and above-mentioned master divides
From pipe, there is air inlet, gas outlet and liquid outlet, inside above-mentioned main separation pipe, be additionally provided with bladeless fan, above-mentioned nothing
Blade fan is between gas-liquid separator and air inlet.
In order to optimize technique scheme further, the technical measures that the present invention is taked also include:
Preferably, assembly of the invention also includes miniature atomising device, above-mentioned miniature atomising device be arranged at above-mentioned instead
Should the outer wall of pipe, the reaction tube outer wall being connected with above-mentioned miniature atomising device is equipped with micropore, above-mentioned sample feeding pipe
It is connected with miniature atomising device;Above-mentioned design can make sample be atomized fully before entering reaction tube.
Preferably, assembly of the invention also includes sample storage box, and sample storage box is the design of integral type, is divided into sample storage
Product box and storage test kit.
Preferably, above-mentioned gas-liquid separator is hollow spherical shape, and has gas-liquid separation hole;Above-mentioned it is designed with
Help the quick effusion of reacting gas, do not affect the downward discharge of waste reaction solution simultaneously.
Preferably, the hollow of above-mentioned bladeless fan without the diameter of leaf part more than the diameter of gas-liquid separator;Without leaf
Not flabellum in the middle part of fan, it is possible to provide the passage that waste reaction solution declines, and the difference of diameter is so that upwards
Dry and maximized avoid the waste reaction solution corrosion to bladeless fan simultaneously.
Preferably, above-mentioned sample feeding pipe and reagent sample feeding pipe are capillary tube.
Preferably, above-mentioned sample feeding tube portion pipeline is positioned at inside reaction tube, and this section of tubing has micropore,
Sample liquids is discharged by micropore, so that reaction contact area maximizes.
Preferably, above-mentioned sample feeding pipe is 1-12, more preferably 10.
Preferably, above-mentioned gas outlet can be with multiple Instrument crosslinkings such as such as atomic absorption analyzers.
On the other hand, the present invention also provides for a kind of utilizing above-mentioned minisize liquid reaction unit to carry out reaction test
The using method of method, the i.e. present invention, comprises the following steps:
Step 1, uses sample feeding pipe collecting test sample, uses reagent sample feeding pipe to gather reducing agent, makes survey
Test agent and reducing agent fully react at reaction tube;
Step 2, opens air inlet, gas outlet and liquid outlet, and is passed through nitrogen or argon at air inlet, starts
Bladeless fan, is pushed out gas outlet by the gas that reaction produces;
Step 3, collects the gas that step 2 is pushed out, detection.
The present invention uses technique scheme, compared with prior art, has the following technical effect that the present invention's
A kind of minisize liquid reaction unit, on the basis of existing technology, has made the improvement of multiple initiative.First,
The reaction tube of the present invention adds bladeless fan so that when collecting reacting gas, the argon being passed through and nitrogen
It is close to reaction tube tube wall up, and the waste liquid reacted drops into leakage fluid dram just by the hollow space of bladeless fan
Outside discharger, it is therefore prevented that part waste liquid is blown into gas outlet or detection device by the single gas that is passed through, it will be apparent that subtract
Lack quartz ampoule and the infringement of detection analytical tool, also improved repeatability and the stability of detection;Secondly,
Before the reaction of reaction tube, sample and reagent are all through pretreatment (micropore is beaten and spread and be atomized) so that the two
The reaction of reaction tube maximizes, and does not only have the waste of reagent, and complete and abundant due to react, detection
Repeatability obtained improving further.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the minisize liquid reaction unit of the present invention;
Reference therein is: main separation pipe 1, sample feeding pipe 2, reagent sample feeding pipe 3, reaction tube 4,
Gas-liquid separator 5, air inlet 6, gas outlet 7, liquid outlet 8, bladeless fan 9, miniature atomising device 10,
Sample storage box 11.
Detailed description of the invention
The invention provides a kind of minisize liquid reaction unit, enter including main pipe, sample feeding pipe and the reagent of separating
Sample pipe, described main separation pipe is connected with reaction tube 4, and one end of described reaction tube 4 is formed with gas-liquid separation
Device 5, described gas-liquid separator 5 inside main separation pipe 1, sample feeding pipe 2 and reagent sample feeding pipe 3 all with
Described reaction tube 4 is connected, and described main separation pipe 1 has air inlet 6, gas outlet 7 and liquid outlet 8, institute
Stating main separation pipe 1 inside and be additionally provided with bladeless fan 9, described bladeless fan 9 is positioned at gas-liquid separator 5 and air inlet
Between mouth 6.
In a preferred embodiment, assembly of the invention also includes miniature atomising device 10, described miniature atomising
Device 10 is arranged at the outer wall of described reaction tube 4, reaction tube 4 outer wall being connected with described miniature atomising device 10
Being equipped with micropore, described sample feeding pipe 2 is connected with miniature atomising device 10.
In a preferred embodiment, assembly of the invention also includes sample storage box 11, and described sample storage box 11 is divided into
Storage sample box and storage test kit.
In a preferred embodiment, described gas-liquid separator 5 is hollow spherical shape, and has gas-liquid separation hole.
In a preferred embodiment, the hollow of described bladeless fan 9 is more than gas-liquid separator without the diameter of leaf part
The diameter of 5.
In a preferred embodiment, described sample feeding pipe 2 and reagent sample feeding pipe 3 are capillary tube.
In a preferred embodiment, it is internal that described sample feeding pipe 2 section of tubing is positioned at reaction tube 4, this part
Pipeline has micropore.
In a preferred embodiment, described sample feeding pipe 2 is 1-12.
In a preferred embodiment, described gas outlet 7 can be with multiple Instrument crosslinking, especially Atomic Absorption
Analyser.
Below by specific embodiment, the present invention is carried out detailed and concrete introduction, so that being better understood from this
Bright, but following embodiment is not limiting as the scope of the invention.
This device of embodiment one is combined with Atomic Absorption Spectrometer, lead, the inspection of arsenic element content in Tibetan medicine prescribed preparation
Application in survey
Taking a small amount of Tibetan medicine sample to be measured, enter pretreatment by wet digesting mode, sample HCL then is carried out
Dissolve, with K3Fe (CN) 6 and KI, the lead in solution, arsenic oxidoreduction become Pb4+, As3+ respectively,
Sample solution is put in storage sample box, and places KBH4 in storage test kit.
Then sample feeding pipe 2 and reagent sample feeding pipe 3 are inserted in storage sample box and storage test kit respectively;This reality
Executing sample feeding pipe in example is capillary tube, and by capillarity, sample is arrived reaction tube, and discharged into by micropore
In reaction tube;During reducing agent is delivered to miniature atomising device 10 by reagent sample feeding pipe 3 simultaneously, start nebulizer,
Reducing agent discharges in reaction tube with atomised form;Reacted gas and liquid enter gas-liquid separator 5
In, by gas-liquid separation hole, waste liquid falls, and through the hollow space of bladeless fan 9, falls into liquid outlet 8,
Meanwhile, the bladeless fan 9 of startup utilizes the nitrogen or argon that air inlet 6 is passed through, by reacting gas from gas outlet
7 release, and enter the T-shaped quartz ampoule of atomic absorption analyzer, then utilize atomic absorption analyzer to detect.
This device of embodiment two and the combination of atomic fluorescence spectrophotometer, answering in the tribute detection of content of element of surface water
With
Taking a small amount of surface water to be measured, fully shaken up by water sample, 25.0mL is in 50mL conical flask in absorption,
Carry out clearing up pretreatment with potassium permanganate-digest by potassium persulfate, sample solution is put in storage sample box, and
And place NaBH in storage test kit4。
Then sample feeding pipe 2 and reagent sample feeding pipe 3 are inserted in storage sample box and storage test kit respectively;This reality
Executing sample feeding pipe in example is capillary tube, and by capillarity, sample is arrived reaction tube, and discharged into by micropore
In reaction tube;During reducing agent is delivered to miniature atomising device 10 by reagent sample feeding pipe 3 simultaneously, start nebulizer,
Reducing agent discharges in reaction tube with atomised form;Reacted gas and liquid enter gas-liquid separator 5
In, by gas-liquid separation hole, waste liquid falls, and through the hollow space of bladeless fan 9, falls into liquid outlet 8,
Meanwhile, the bladeless fan 9 of startup utilizes the nitrogen or argon that air inlet 6 is passed through, by reacting gas from gas outlet
7 release, and enter atomic fluorescence spectrophotometer and detect.
This device of embodiment three and the combination of atomic fluorescence spectrophotometer, the application in the lead element content detection of Folium Camelliae sinensis
Take tea sample 0.5g after crushed in 100mL conical flask, add nitric acid-perchloric acid mixed acid
10mL, shakes up immersion, stands overnight, and it is faint yellow or colourless for being placed on electric furnace heating and clearing up to Digestive system,
Add the continuation heating of 20mL water after the coldest and catch up with acid, remaining 0.5~1.0mL to digestion solution.Add after cooling
A small amount of water, and add hydrochloric acid 0.5mL, oxalic acid (10g/L) 0.5mL, the potassium ferricyanide (50g/L) 0.5mL,
Mixing, is put in the sample solution made in storage sample box, and places NaBH in storage test kit4。
Then sample feeding pipe 2 and reagent sample feeding pipe 3 are inserted in storage sample box and storage test kit respectively;This reality
Executing sample feeding pipe in example is capillary tube, and by capillarity, sample is arrived reaction tube, and discharged into by micropore
In reaction tube;During reducing agent is delivered to miniature atomising device 10 by reagent sample feeding pipe 3 simultaneously, start nebulizer,
Reducing agent discharges in reaction tube with atomised form;Reacted gas and liquid enter gas-liquid separator 5
In, by gas-liquid separation hole, waste liquid falls, and through the hollow space of bladeless fan 9, falls into liquid outlet 8,
Meanwhile, the bladeless fan 9 of startup utilizes the nitrogen or argon that air inlet 6 is passed through, by reacting gas from gas outlet
7 release, and enter atomic fluorescence spectrophotometer and detect.
In the above embodiments detection, it is showed no waste liquid adverse current and is brought into the situation of gas outlet or quartz ampoule, simultaneously
Sample utilizes fully, and reaction is good completely, and the repeatability of experiment is high.The minisize liquid reaction dress of the visible present invention
Put and prevent the single gas that is passed through that part waste liquid is blown into gas outlet or detection device, it will be apparent that decrease quartz
Pipe and the infringement of detection analytical tool, also improve repeatability and the stability of detection;And can make sample and
Reagent maximizes in the reaction of reaction tube, does not only have the waste of reagent, and complete and abundant due to react,
The repeatability of detection has obtained improving further.
Being described in detail the specific embodiment of the present invention above, but it is intended only as example, the present invention is also
It is not restricted to particular embodiments described above.To those skilled in the art, any the present invention is carried out
Equivalent modifications and substitute the most all among scope of the invention.Therefore, without departing from the spirit of the present invention and model
Enclose lower made impartial conversion and amendment, all should contain within the scope of the invention.
Claims (10)
1. a minisize liquid reaction unit, separates pipe (1), sample feeding pipe (2) and reagent sample introduction including main
Pipe (3), it is characterised in that the described main pipe (1) that separates is connected with reaction tube (4), described reaction tube
(4) one end is formed with gas-liquid separator (5), and described gas-liquid separator (5) separates in pipe (1) main
Portion, sample feeding pipe (2) is all connected with described reaction tube (4) with reagent sample feeding pipe (3), described master
Separating pipe (1) and have air inlet (6), gas outlet (7) and liquid outlet (8), described main separation manages (1)
Inside is additionally provided with bladeless fan (9), and described bladeless fan (9) is positioned at gas-liquid separator (5) and air inlet
(6) between.
A kind of minisize liquid reaction unit the most according to claim 1, it is characterised in that also include small-sized
Nebulizer (10), described miniature atomising device (10) is arranged at the outer wall of described reaction tube (4), with described
Reaction tube (4) outer wall that miniature atomising device (10) connects is equipped with micropore, described sample feeding pipe (2)
It is connected with miniature atomising device (10).
A kind of minisize liquid reaction unit the most according to claim 1, it is characterised in that also include sample storage
Box (11), described sample storage box (11) is divided into storage sample box and storage test kit.
A kind of minisize liquid reaction unit the most according to claim 1, it is characterised in that described gas-liquid separation
Device (5) is hollow spherical shape, and has gas-liquid separation hole.
A kind of minisize liquid reaction unit the most according to claim 4, it is characterised in that described bladeless fan
(9) hollow without the diameter of leaf part more than the diameter of gas-liquid separator (5).
A kind of minisize liquid reaction unit the most according to claim 1, it is characterised in that described sample feeding
Pipe (2) and reagent sample feeding pipe (3) are capillary tube.
A kind of minisize liquid reaction unit the most according to claim 1, it is characterised in that described sample feeding
It is internal that pipe (2) section of tubing is positioned at reaction tube (4), and this section of tubing has micropore.
A kind of minisize liquid reaction unit the most according to claim 1, it is characterised in that described sample feeding
Pipe (2) is 1-12.
A kind of minisize liquid reaction unit the most according to claim 1, it is characterised in that described gas outlet (7)
It is connected with atomic absorption analyzer.
10. utilizing the method that the minisize liquid reaction unit described in claim 1 carries out reaction test, it is special
Levy and be, comprise the following steps:
Step 1, uses sample feeding pipe (2) collecting test sample, uses reagent sample feeding pipe (3) to gather reducing agent,
Test sample and reducing agent is made fully to react at reaction tube (4);
Step 2, opens air inlet (6), gas outlet (7) and liquid outlet (8), and is passed through nitrogen at air inlet (6)
Gas or argon, start bladeless fan (9), and the gas that reaction produces is pushed out gas outlet (7);
Step 3, collects the gas that step 2 is pushed out, detection.
Priority Applications (1)
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CN201610408895.1A CN105973810A (en) | 2016-06-12 | 2016-06-12 | Miniature liquid reaction device and use method thereof |
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CN201610408895.1A CN105973810A (en) | 2016-06-12 | 2016-06-12 | Miniature liquid reaction device and use method thereof |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107037115A (en) * | 2017-04-17 | 2017-08-11 | 中国科学院海洋研究所 | A kind of ICP MS hydride sampling system and its method for detecting hydride |
CN110214269A (en) * | 2017-03-15 | 2019-09-06 | 株式会社岛津制作所 | Chemiluminescence detector reaction unit and the chemiluminescence detector and chemical luminescence detection method for having the reaction unit |
-
2016
- 2016-06-12 CN CN201610408895.1A patent/CN105973810A/en active Pending
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110214269A (en) * | 2017-03-15 | 2019-09-06 | 株式会社岛津制作所 | Chemiluminescence detector reaction unit and the chemiluminescence detector and chemical luminescence detection method for having the reaction unit |
CN107037115A (en) * | 2017-04-17 | 2017-08-11 | 中国科学院海洋研究所 | A kind of ICP MS hydride sampling system and its method for detecting hydride |
CN107037115B (en) * | 2017-04-17 | 2023-11-07 | 中国科学院海洋研究所 | ICP-MS hydride sampling system and hydride detection method thereof |
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Application publication date: 20160928 |