CN213749593U - Atomic spectrum detection device for 3D printing field analysis - Google Patents
Atomic spectrum detection device for 3D printing field analysis Download PDFInfo
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- CN213749593U CN213749593U CN202022621314.7U CN202022621314U CN213749593U CN 213749593 U CN213749593 U CN 213749593U CN 202022621314 U CN202022621314 U CN 202022621314U CN 213749593 U CN213749593 U CN 213749593U
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Abstract
The utility model belongs to the technical field of check out test set, a 3D prints site analysis's atomic spectrum detection device is disclosed. The utility model comprises a photochemical vapor generation system, a hydride generation system, a gas-liquid separation system and a PD excitation source system which are all printed by 3D; the gas-liquid separation system is respectively communicated with the photochemical steam generation system and the hydride generation system; and the PD excitation source system is respectively communicated with the gas-liquid separation system and the CCD spectrometer. The utility model discloses be used for 3D printing technique to establish whole miniaturized analysis detecting instrument, two kinds of steam generation methods of integration, can utilize the difference of steam generation efficiency under the different valence states of element, realize the colorless spectrum morphological analysis of element, each item analytical performance sign of device also is as little as different with other little plasma atomic emission spectrometers of the same type, but whole compacter stability, consequently can be effective, respond emergency environment incident fast, have important meaning to on-the-spot elemental morphological analysis.
Description
Technical Field
The utility model belongs to the technical field of check out test set, concretely relates to atomic spectrum detection device of 3D printing field analysis.
Background
1. The atomic spectrum is an important component in modern analysis and detection technology, has the advantages of high sensitivity, good selectivity, strong stability and good anti-interference capability, and therefore plays a very important role in the fields of environmental protection, food safety, advanced materials and clinical medicine. However, although commercial atomic spectrum instruments such as atomic absorption, atomic fluorescence, inductively coupled plasma-atomic emission, and inductively coupled plasma mass spectrometry can perform highly sensitive and highly selective detection, most of them are expensive, large in size, and high in energy consumption, and can only be used in research institutions and detection departments in developed areas, so that it is difficult to meet the requirements of on-site real-time online analysis. With the rapid development of industrial and agricultural production and economic construction in China in recent years, major sudden environmental pollution accidents are in a situation of rising year by year. And the chemical pollution accident of the environment often happens suddenly and rapidly, a large amount of pollutants are discharged instantly or in a short time, and the surrounding environment is seriously damaged. Therefore, for remote areas and areas to be developed, which have slightly lagged economic development, the development of cheap, portable and sensitive miniaturized detection instruments is urgently needed to deal with sudden environmental pollution events.
3D printing, based on CAD three-dimensional modeling, and the entity can be quickly constructed in a layered manufacturing layer-by-layer overlapping mode. The method is widely applied to various industries such as biological medical treatment, food processing, design and construction and the like. Compared with the traditional manufacturing technology, the 3D printing can provide a more uniform and standardized scheme, can conveniently, quickly and economically obtain instrument parts which cannot be manufactured by the traditional technology, and even needs no assembled integrated device. More importantly, 3D printed design files can be shared online, and one drawing can be used to produce the same instrument in a repeatable manner around the world. The spectrum detection device for 3D printing can meet the requirements of economy and detection accuracy on the basis of not changing the internal support principle of the miniaturized equipment.
2. The toxicity, bioavailability and migration of an element depend not only on its total amount but also on the chemical form in which it is present in the environment. Currently, the chromatographic coupling technique can easily accomplish the elemental morphology analysis. The analysis time of the combined technology is short, and more information about morphological distribution and structure can be provided. However, the methods currently used still have some serious disadvantages, including large volume, high reagent and gas consumption, high instrument and operation costs, etc. The properties of element toxicity, mobility and the like are closely related to the form of the element in the environment, and the real situation of the element form in the environment is difficult to reflect by the result obtained by a laboratory analysis method, so the strategy of the laboratory analysis is not ideal.
SUMMERY OF THE UTILITY MODEL
In order to solve the above problems existing in the prior art, the utility model aims to provide a 3D prints field analysis's atomic spectrum detection device.
The utility model discloses the technical scheme who adopts does:
an atomic spectrum detection device for 3D printing field analysis comprises a photochemical vapor generation system, a hydride generation system, a gas-liquid separation system and a PD excitation source system which are all printed in a 3D way;
a photochemical vapor generation system for generating a volatile target analyte after performing ultraviolet light reaction on the solution in the presence of a low molecular weight organic acid formic acid;
the hydride generating system is used for carrying out hydroboration reaction on different solutions to generate gaseous hydride;
the gas-liquid separation system is respectively communicated with the photochemical steam generation system and the hydride generation system and is used for carrying out gas-liquid separation on the volatile target analyte generated by the photochemical steam generation system or carrying out gas-liquid separation on the gaseous hydride generated by the hydride generation system;
and the PD excitation source system is respectively communicated with the gas-liquid separation system and the CCD spectrometer and is used for sending the gas-phase analyte separated by the gas-liquid separation system into the point discharge micro-plasma for excitation, recording an atomic emission peak signal generated by the excitation source system by the CCD spectrometer and then carrying out integral analysis.
Further preferably, the gas-liquid separation system comprises a primary gas-liquid separator and a secondary gas-liquid separator which are communicated with each other, the primary gas-liquid separator is respectively communicated with the photochemical steam generation system and the hydride generation system, and the secondary gas-liquid separator is communicated with the PD excitation source system.
It is still further preferred that the primary gas-liquid separator is connected to a carrier gas introducing pipe and a waste liquid discharging pipe.
More preferably, the photochemical steam generation system comprises a lamp holder, an ultraviolet lamp and a first liquid inlet pipeline, wherein an irradiation cavity is arranged in the lamp holder, and the ultraviolet lamp is arranged in the irradiation cavity; the outer winding of ultraviolet lamp has quartz spiral coil, and first feed liquor pipeline penetrates and links to each other with quartz spiral coil's one end after shining the intracavity, and quartz spiral coil's the other end is drawn forth and is shone the chamber and be connected with a gas-liquid separator behind the chamber.
It is further preferred that a layer of aluminum foil is mounted on the lamp holder outside the ultraviolet lamp.
It is further preferred that the aluminum foil is mounted on the inner wall of the irradiation chamber or on the outer wall of the lamp holder.
It is further preferred that the hydride generation system, the primary gas-liquid separator, the secondary gas-liquid separator and the PD excitation source system are all mounted on the upper end of the lamp holder.
Still further preferably, the hydride generation system is a three-way pipeline, the three-way pipeline is provided with two inlets and one outlet, and the outlet of the three-way pipeline is communicated with the primary gas-liquid separator.
Still preferably, the PD excitation source system includes an excitation unit and a tapered tungsten electrode, a discharge cavity is provided inside the excitation unit, and the secondary gas-liquid separator is communicated with the discharge cavity through a pipe; two conical tungsten electrodes with one ends positioned in the discharge cavity are arranged on the excitation unit; and the upper end of the excitation unit is provided with a waste gas discharge pipeline which is communicated with the top of the discharge cavity.
It is further preferred that the discharge chamber is a circular hole formed in the middle of the excitation unit, and quartz plates for sealing are disposed at both ends of the circular hole.
The utility model has the advantages that:
the utility model is divided into a photochemical steam generation system and a hydride generation system during operationOtherwise, first, the hydride generation system operates by introducing KBH4The solution and the sample/standard solution containing HCl react to generate gaseous hydride, the generated gaseous hydride enters a gas-liquid separation system for fully separating a water phase, the separated gas-phase analyte enters a PD excitation source system for excitation in the gas-liquid separation system, and an emission signal is recorded by a CCD spectrometer and then is subjected to integral analysis. The utility model discloses be used for 3D printing technique to establish whole miniaturized analysis detecting instrument, integrated two kinds of vapour generating method, hydride takes place and photochemical steam generating method, can utilize the difference of vapour generating efficiency under the different valence states of element, realize the colorless spectrum morphological analysis of element, each item analytical performance sign of device also is as good as with other little plasma atomic emission spectrometers of the same type, but whole compacter stability, consequently can be effective, respond abrupt environmental incident fast, it is significant to on-the-spot elemental morphological analysis.
Drawings
Fig. 1 is a schematic structural diagram of the present invention.
In the figure: 1-a photochemical vapour generation system; 101-a lamp holder; 102-an ultraviolet lamp; 103-a first liquid inlet pipeline; 104-an illumination chamber; a 2-hydride generation system; 3-a gas-liquid separation system; 4-PD excitation source system; 401-an excitation unit; 402-tapered tungsten electrodes; 403-a discharge chamber; 404-exhaust gas discharge line.
Detailed Description
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the present invention will be briefly described below with reference to the accompanying drawings and the description of the embodiments or the prior art, and it is obvious that the following description of the structure of the accompanying drawings is only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without any inventive work.
The technical solution provided by the present invention will be described in detail by way of embodiments with reference to the accompanying drawings. It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto.
In some instances, some embodiments are not described or not in detail, as they are conventional or customary in the art.
Furthermore, the technical features described herein, or the steps of all methods or processes disclosed, may be combined in any suitable manner in one or more embodiments, in addition to the mutually exclusive features and/or steps. It will be readily appreciated by those of skill in the art that the order of the steps or operations of the methods associated with the embodiments provided herein may be varied. Any order in the drawings and examples is for illustrative purposes only and does not imply that a certain order is required unless explicitly stated to be required.
The numbering of the components as such, e.g., "first", "second", etc., is used herein only to distinguish the objects as described, and does not have any sequential or technical meaning. The terms "connected" and "coupled" when used in this application, encompass both direct and indirect connections (and couplings) where appropriate and where not necessary contradictory.
Example (b):
as shown in fig. 1, the atomic spectrum detection device for 3D printing field analysis of the present embodiment includes a photochemical vapor generation system 1, a hydride generation system 2, a gas-liquid separation system 3, and a PD excitation source system 4, all using 3D printing;
a photochemical vapor generation system 1 as a photochemical vapor generation method for generating a volatile target analyte by performing an ultraviolet light irradiation reaction on a solution;
the hydride generating system 2 is used as a cold steam generating method and is used for carrying out hydroboration reaction on different solutions to generate gaseous hydride;
the gas-liquid separation system 3 is respectively communicated with the photochemical vapor generation system 1 and the hydride generation system 2 and is used for carrying out gas-liquid separation on the volatile target analyte generated by the photochemical vapor generation system or carrying out gas-liquid separation on the gaseous hydride generated by the hydride generation system; it should be noted that the photochemical vapor generation system 1 and the hydride generation system 2 are alternately connected to the gas-liquid separation system 3 to avoid interference between them, and when the photochemical vapor generation system 1 is used in the state shown in fig. 1, and the hydride generation system 2 needs to be used, the input pipeline of the photochemical vapor generation system 1 is disconnected and the input pipeline of the hydride generation system 2 is connected.
And the PD excitation source system 4 is respectively communicated with the gas-liquid separation system 3 and the CCD spectrometer and is used for sending the gas-phase analyte separated by the gas-liquid separation system into the point discharge microplasma for excitation, recording the generated atomic emission peak signal by the CCD spectrometer and then carrying out integral analysis.
The utility model discloses the during operation, system 2 is worked respectively to photochemistry vapour generation system 1 and hydride, firstly, system 2 during operation takes place for the hydride, KBH4 solution and the sample/standard solution that contains HCL can be introduced, two kinds of solution reactions, be used for producing gaseous hydride, the gaseous hydride of production gets into gas-liquid separation system 3 in, this system is used for the fully separated aqueous phase, in gas-liquid separation system, the gaseous phase analysis thing of isolating gets into PD excitation source system 4, PD excitation source system 4 sends the gaseous phase analysis thing that gas-liquid separation system separates into in the little plasma of point discharge and arouses, its transmitting signal is recorded by CCD spectrometer, then integral analysis. The utility model discloses be used for 3D printing technique to establish whole miniaturized analysis detecting instrument, integrated two kinds of vapour generating method, hydride takes place and photochemical steam generating method, can utilize the difference of vapour generating efficiency under the different valence states of element, realize the colorless spectrum morphological analysis of element, each item analytical performance sign of device also is as good as with other little plasma atomic emission spectrometers of the same type, but whole compacter stability, consequently can be effective, respond abrupt environmental incident fast, it is significant to on-the-spot elemental morphological analysis.
It should be further described in this embodiment that the gas-liquid separation system 3 includes a primary gas-liquid separator and a secondary gas-liquid separator that are communicated with each other, and the gas-liquid separation is realized by the cooperation of the two separators, so that the separation effect is also better, the primary gas-liquid separator is respectively communicated with the photochemical steam generation system 1 and the hydride generation system 2, and the primary gas-liquid separator is communicated with the PD excitation source system 4. The volatile target analytes generated by the photochemical vapor generation system 1 and the hydride generation system 2 are separated from the liquid phase in the primary gas-liquid separator and then transferred to the primary gas-liquid separator to remove excess water.
It should be further noted that in this embodiment, the primary gas-liquid separator is connected to a carrier gas introducing pipe 303 and a waste liquid discharging pipe 304. The volatile substances generated by photochemical vapour generation and hydride generation are fed successively into a gas-liquid separation system consisting of two gas-liquid separator chambers (20mm x 48mm) of the same size for the complete separation of the aqueous phase. In the gas-liquid separation system, Ar is introduced, and it is noted that Ar not only serves as a carrier gas to accomplish efficient separation of volatile analytes from the liquid phase, but also serves as a working gas for tip discharge microplasma atom emission.
In this embodiment, it should be further noted that the photochemical steam generation system 1 includes a lamp holder 101, an ultraviolet lamp 102 and a first liquid inlet pipe 103, wherein an irradiation chamber 104 is disposed in the lamp holder 101, and the ultraviolet lamp 102 is installed in the irradiation chamber 104; the outer winding of ultraviolet lamp 102 has quartz spiral coil, and first feed liquor pipeline 103 penetrates and shines in the chamber 104 back and links to each other with quartz spiral coil's one end, and quartz spiral coil's the other end is drawn forth and is shone the chamber 104 back and be connected with a gas-liquid separator, can pass through the mode of pumping into, and after liquid got into first feed liquor pipeline 103, can be through shining chamber 104, then shone the ultraviolet lamp 102 in the chamber 104 and shine, then adopt the mode of stopping the pump, carry out abundant ultraviolet ray illumination reaction.
In this embodiment, a layer of aluminum foil is mounted on the lamp base 101 outside the ultraviolet lamp 102. The aluminum foil is mounted on the inner wall of the irradiation chamber 104 or on the outer wall of the lamp holder 101. To further protect the operator from uv radiation and maximize PVG efficiency, aluminum foil is mounted on the lamp housing of the uv lamp.
It should be further noted that, in this embodiment, the hydride generation system 2, the primary gas-liquid separator, the secondary gas-liquid separator and the PD excitation source system 4 are all installed on the upper end of the lamp holder 101, so that the overall installation is more compact and stable, and the emergency environment event can be effectively and quickly responded.
In this embodiment, it should be further noted that the hydride generating system 2 is a three-way pipe, the three-way pipe is provided with two inlets and one outlet, and the outlet of the three-way pipe is communicated with the primary gas-liquid separator. Two inlets may be used to introduce KBH separately4The solution and the HCl-containing sample/standard solution are then exported for reaction, although the solution introduced is not fixed, as the case may be.
In this embodiment, it should be further noted that the PD excitation source system 4 includes an excitation unit 401 and a tapered tungsten electrode 402, a discharge cavity 403 is disposed inside the excitation unit 401, and the secondary gas-liquid separator is communicated with the discharge cavity 403 through a pipeline; two conical tungsten electrodes 402 with one end in the discharge cavity 403 are arranged on the excitation unit 401; an exhaust gas discharge pipe 404 is arranged at the upper end of the excitation unit 401, and the exhaust gas discharge pipe 404 is communicated with the top of the discharge cavity 403. Two identical holes (1.6 mm diameter) were placed on the opposite and central axis of the cavity to place two tapered tungsten electrodes (1.6 mm diameter) to generate microplasma, with a 3mm electrode spacing. And collecting an emission spectrum generated by a point discharge excitation source by using an optical fiber, and finally recording the emission spectrum by using a micro optical fiber spectrometer.
In this embodiment, it should be further noted that the discharge cavity 403 is a circular hole disposed in the middle of the excitation unit 401, and two ends of the circular hole are both provided with sealing quartz plates. Two quartz plates were used to enclose the discharge region to concentrate the analyte introduced from the inner tube and to avoid severe dilution and diffusion.
It should be noted that, after the atomic spectrum detection device of the present invention is manufactured, the printed matter is put into a barrel filled with isopropyl alcohol (IPA), and the barrel is soaked for 10 minutes to wash away the uncured excess liquid resin. Then rinsed with 99.99% absolute ethanol and DIW water, respectively. The element form analysis needs to be carried out by respectively adopting a photochemical vapor generation system 1 and a hydride generation system 2 and utilizing the difference of the vapor generation efficiency of different element forms. A peristaltic pump was first used to pump in a blank solution to clean the 3D printing tubing set and the power was turned on to stabilize the plasma for at least 10 minutes. 2mL of standard solution or sample solution (containing 5% formic acid) was introduced into the UV light chemical reactor, and the UV light reaction was performed sufficiently by stopping the pump. The resulting volatile target analyte is separated from the liquid phase in a primary gas-liquid separator and then transferred to a primary gas-liquid separator to remove excess moisture. Subsequently, the gaseous analyte is excited by feeding it into a tip-discharge microplasma, the emission signal of which is recorded by a CCD spectrometer and then integrated for analysis.
The present invention is not limited to the above-mentioned optional embodiments, and any other products in various forms can be obtained by anyone under the teaching of the present invention, and any changes in the shape or structure thereof, all the technical solutions falling within the scope of the present invention, are within the protection scope of the present invention.
Claims (10)
1. The utility model provides a 3D prints atomic spectrum detection device of on-the-spot analysis which characterized in that: the device comprises a photochemical vapor generation system (1), a hydride generation system (2), a gas-liquid separation system (3) and a PD excitation source system (4) which are all printed by 3D;
the photochemical steam generation system (1) is used for generating a volatile target analyte after carrying out ultraviolet irradiation reaction on the solution;
the hydride generating system (2) is used for carrying out hydroboration reaction on different solutions to generate gaseous hydride;
the gas-liquid separation system (3) is respectively communicated with the photochemical steam generation system (1) and the hydride generation system (2) and is used for carrying out gas-liquid separation on the volatile target analyte generated by the photochemical steam generation system or carrying out gas-liquid separation on the gaseous hydride generated by the hydride generation system;
and the PD excitation source system (4) is respectively communicated with the gas-liquid separation system (3) and the CCD spectrometer and is used for sending the gas-phase analyte separated by the gas-liquid separation system into the point discharge micro-plasma for excitation, and an atomic emission peak signal generated by the excitation source system is recorded by the CCD spectrometer and then is subjected to integral analysis.
2. The atomic spectrum detection device for 3D printing field analysis according to claim 1, wherein: the gas-liquid separation system (3) comprises a primary gas-liquid separator and a secondary gas-liquid separator which are communicated with each other, the primary gas-liquid separator is respectively communicated with the photochemical steam generation system (1) and the hydride generation system (2), and the primary gas-liquid separator is communicated with the PD excitation source system (4).
3. The atomic spectrum detection device for 3D printing field analysis according to claim 2, wherein: the primary gas-liquid separator is connected with a carrier gas introduction pipe (303) and a waste liquid discharge pipe (304).
4. The atomic spectrum detection device for 3D printing field analysis according to claim 3, wherein: the photochemical steam generation system (1) comprises a lamp holder (101), an ultraviolet lamp (102) and a first liquid inlet pipeline (103), wherein an irradiation cavity (104) is arranged in the lamp holder (101), and the ultraviolet lamp (102) is arranged in the irradiation cavity (104); the ultraviolet lamp (102) is wound with a quartz spiral coil, a first liquid inlet pipeline (103) penetrates into the irradiation cavity (104) and then is connected with one end of the quartz spiral coil, and the other end of the quartz spiral coil is led out of the irradiation cavity (104) and then is connected with the primary gas-liquid separator.
5. An atomic spectrum detection device for 3D printing field analysis according to claim 4, wherein: and a layer of aluminum foil is arranged on the lamp holder (101) outside the ultraviolet lamp (102).
6. The atomic spectrum detection device for 3D printing field analysis according to claim 5, wherein: the aluminum foil is mounted on the inner wall of the irradiation cavity (104) or on the outer wall of the lamp holder (101).
7. The atomic spectrum detection device for 3D printing field analysis according to claim 4, wherein: the hydride generation system (2), the primary gas-liquid separator, the secondary gas-liquid separator and the PD excitation source system (4) are all arranged at the upper end of the lamp holder (101).
8. The atomic spectrum detection device for 3D printing on-site analysis according to any one of claims 2-7, wherein: the hydride generation system (2) is a three-way pipeline, the three-way pipeline is provided with two inlets and one outlet, and the outlet of the three-way pipeline is communicated with the primary gas-liquid separator.
9. The atomic spectrum detection device for 3D printing on-site analysis according to any one of claims 2-7, wherein: the PD excitation source system (4) comprises an excitation unit (401) and a conical tungsten electrode (402), a discharge cavity (403) is arranged in the excitation unit (401), and the secondary gas-liquid separator is communicated with the discharge cavity (403) through a pipeline; two conical tungsten electrodes (402) with one ends positioned in the discharge cavity (403) are arranged on the excitation unit (401); an exhaust gas discharge pipeline (404) is arranged at the upper end of the excitation unit (401), and the exhaust gas discharge pipeline (404) is communicated with the top of the discharge cavity (403).
10. The atomic spectrum detection device for 3D printing field analysis according to claim 9, wherein: the discharge cavity (403) is a circular hole formed in the middle of the excitation unit (401), and quartz plates for sealing are arranged at two ends of the circular hole.
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| CN202022621314.7U CN213749593U (en) | 2020-11-12 | 2020-11-12 | Atomic spectrum detection device for 3D printing field analysis |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114166809A (en) * | 2021-11-27 | 2022-03-11 | 埃坭克仪器(北京)有限公司 | Chemical reaction and separation integrated module of atomic fluorescence spectrophotometer |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114166809A (en) * | 2021-11-27 | 2022-03-11 | 埃坭克仪器(北京)有限公司 | Chemical reaction and separation integrated module of atomic fluorescence spectrophotometer |
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