CN117030637A - Solid sample detection device - Google Patents

Solid sample detection device Download PDF

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Publication number
CN117030637A
CN117030637A CN202310982791.1A CN202310982791A CN117030637A CN 117030637 A CN117030637 A CN 117030637A CN 202310982791 A CN202310982791 A CN 202310982791A CN 117030637 A CN117030637 A CN 117030637A
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China
Prior art keywords
liquid
clear water
control valve
pipeline
pump
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CN202310982791.1A
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Chinese (zh)
Inventor
孟雪
吕庆斌
赵海波
林青
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BEIJING INSTITUTE OF METROLOGY
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BEIJING INSTITUTE OF METROLOGY
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Priority to CN202310982791.1A priority Critical patent/CN117030637A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/34Purifying; Cleaning
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44Sample treatment involving radiation, e.g. heat
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/76Chemiluminescence; Bioluminescence
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
    • G01N2021/786Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour with auxiliary heating for reaction
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

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  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Plasma & Fusion (AREA)
  • Biomedical Technology (AREA)
  • Molecular Biology (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Automatic Analysis And Handling Materials Therefor (AREA)

Abstract

The invention relates to the technical field of detection equipment, in particular to a solid sample detection device which comprises an accurate liquid injection system, a liquid injection system and a liquid injection system, wherein the accurate liquid injection system is used for accurately controlling the injection amount of a reagent injected into a collecting bottle or a reaction tank; accurate annotate liquid system includes: the device comprises an infusion pipeline, a first one-way valve, a dosing pump, a liquid injection needle, a clear water pipeline, a clear water bottle, a clear water pump, a first control valve and a second one-way valve; when the quantitative pump stops working, the first control valve is restored to the normally open initial station under the action of the internal reset piece of the first control valve, so that the clear water pipeline is communicated; the clear water pump works and is used for pumping clear water in the clear water bottle into the first liquid section, further flushing the first liquid section, the quantitative pump and the second liquid section, and further pumping residual reagents in the first liquid section, the quantitative pump and the second liquid section into the collecting bottle or the reaction tank through the clear water. The preparation is made for the subsequent pumping of other reagents, the mutual interference and influence of different reagents are avoided, and the accuracy of reagent input dosage is ensured.

Description

Solid sample detection device
Technical Field
The invention relates to the technical field of detection equipment, in particular to a solid sample detection device.
Background
In the field of solid sample chemical element detection, the content of chemical elements in a solid sample to be detected is detected, and a specific solid sample is firstly required to be pretreated, wherein the pretreatment method comprises a chemical digestion method, an alkali extraction method and the like.
The method for detecting the semi-volatile organic matters of the solid sample can adopt a rapid solvent extraction method and has the advantages of small organic solvent consumption, rapidness and high recovery rate. The fast solvent extraction process is one kind of automatic organic solvent extraction process under raised temperature and pressure, and the main current apparatus is imported.
The pretreatment of the sample generally comprises the steps of sample decomposition, solvent extraction, sample filtration, quantitative concentration and the like, and in the pretreatment process, the pretreatment reaction processes of a chemical digestion method, a rapid solvent extraction method, an alkali extraction method and the like are required to be carried out, and the operation steps of chemical dissolution, filtration, flushing, acid removal, nitrogen blowing concentration, pH value adjustment, constant volume and the like are carried out. In addition, a plurality of instruments such as a graphite digestion instrument, a solvent extraction instrument, a filtering device, a nitrogen blowing concentrator and the like are configured in a laboratory, so that the equipment occupies a large space, the degree of automation is low, and the cost of sample detection is high.
In view of the foregoing, there is a need for a solid sample detection device.
Disclosure of Invention
The application aims to provide a solid sample detection device so as to solve the technical problem of high sample detection cost in the prior art. The application relates to a division application with the original application number of 2023107053668 and the name of 'a high-flux integrated solid sample detection device'.
In order to solve the technical problems, the high-flux integrated solid sample detection device provided by the application comprises a reaction tank and a heating module, wherein the reaction tank is arranged in a machine body and is used for containing a sample, the reaction tank is arranged in the heating module, and the heating module is used for heating the reaction tank;
the heating module at least comprises the following four types: the device comprises a water bath oscillation heating unit, a graphite digestion heating unit, a multi-site magnetic stirring heating unit and a metal bath heating unit, wherein the four heating modules are respectively used for sample pretreatment in different method steps, and each heating module is detachably and fixedly connected with a machine body.
Through the technical scheme of the improvement, when facing different processing steps, the four heating modules are selected according to the temperature required by the current processing step, the heating modules are fixedly connected with the machine body, and then the reaction tank is placed in the heating modules, so that one device can process the work of a plurality of original devices, and the purposes of saving space, automatically operating and reducing the cost of sample pretreatment are achieved.
Further, each heating module is electrically connected with the machine body through an aviation plug.
Through the technical scheme of above-mentioned improvement, with heating module and organism quick electric connection through aviation plug's form, the convenience when promoting heating module and changing.
Furthermore, each heating module is detachably and fixedly connected with the machine body through a hasp.
Through the technical scheme of the improvement, the mechanical connection between the instant heating module and the machine body is improved through the hasp, and the stability of the heating module after being connected with the machine body is improved.
Further, the organism still includes control host computer and collecting bottle, the collecting bottle is provided with a plurality of, and a plurality of the collecting bottle is all placed in the top of retort, the collecting bottle is used for collecting the liquid after the sample heating reaction, the collecting bottle passes through the vacuum pump and is connected with the retort, control host computer is used for adding reagent to retort and collecting bottle.
Preferably, the collecting bottle is placed on a collecting tray, a multi-position magnetic stirrer is arranged on the collecting tray, the multi-position magnetic stirrer is positioned at the bottom end of the collecting bottle, and the multi-position magnetic stirrer is used for magnetically stirring liquid in the collecting bottle.
Preferably, the collecting tray is fixedly connected with a weighing module for weighing the collecting bottle. The weighing module may be of the prior art, for example an electronic balance.
Preferably, the collecting tray is fixedly connected with an infrared sensor, and the infrared sensor is used for sensing the liquid level of the collecting bottle so as to perform preliminary volume fixing on the liquid in the collecting bottle.
Further, the control host is provided with a mechanical arm and a liquid storage bottle, the liquid storage bottle is internally used for storing required reagents, a plurality of pipelines are arranged on the mechanical arm, the mechanical arm moves in the host, and the mechanical arm is used for adding the reagents into the reaction tank and the collecting bottle through the pipelines.
Preferably, the liquid storage bottle comprises: solvent bottles, acid liquor bottles, alkali liquor bottles, chemiluminescent reagent bottles, color developing agent bottles and the like.
Preferably, the mechanical arm is provided with a storage device, and the storage device is used for storing and fixing a plurality of pipelines on the mechanical arm.
Preferably, the storage device is a buckle.
Preferably, the receiving means is a tie.
Further, a constant delivery pump is arranged in the machine body, and a liquid injection needle is arranged at the tail section of the mechanical arm; the liquid storage bottle is connected with the liquid injection needle through a liquid conveying pipeline, and the quantitative pump is arranged on the liquid conveying pipeline and used for quantitatively conveying the reagent into the reaction tank and/or the collecting bottle.
Further, the mechanical arm is also provided with a liquid suction device, an acidity electrode, a nitrogen blowing needle and a stirrer, and the liquid injection needle, the liquid suction device, the acidity electrode, the nitrogen blowing needle and the stirrer are detachably connected with the mechanical arm.
Further, the reaction tank comprises a tank body, a sealing cover, a suction and injection pipe and a filter element, wherein the sealing cover seals the tank body, the suction and injection pipe is fixedly connected with the sealing cover and is inserted into the tank body, the filter element is fixedly connected with the suction and injection pipe, the filter element is used for filtering liquid passing through the suction and injection pipe, and the suction and injection pipe is connected with a vacuum pump.
Through the technical scheme, after the sample in the reaction tank and the reagent are heated and react, the vacuum pump is started to suck the liquid in the reaction tank out of the tank body through the suction and injection pipe, and when the liquid passes through the filter element at the suction and injection pipe, the liquid enters the collecting bottle after being filtered.
Further, a filter membrane is arranged in the filter element and is used for filtering liquid passing through the filter element, and the filter element is detachably connected with the suction and injection pipe.
Through the technical scheme of the improvement, the filter element and the suction and injection pipe are arranged to be detachable, so that the filter element can be conveniently detached from the suction and injection pipe, and then the filter membrane in the filter element is replaced.
Further, the tank body is made of polytetrafluoroethylene, made of plastic and made of glass, and the tank bodies made of different materials are suitable for heating modules with different temperatures.
Preferably, when the reaction tank is used for accelerating solvent extraction, a metal bath heating unit is configured, a metal jacket is sleeved outside the reaction tank, the metal jacket comprises a metal jacket and a metal cap, the metal jacket is in threaded connection with the metal cap, and the metal jacket is used for improving the capacity of the reaction tank for bearing high pressure when accelerating solvent extraction.
Further, the control host is also provided with an ultraviolet-visible light spectrophotometer which is used for detecting the color reaction of the liquid in the collecting bottle.
Further, the control host is also provided with a chemiluminescent detector module, and the chemiluminescent detector module is used for carrying out chemiluminescent reaction detection on the liquid in the collecting bottle through the photomultiplier.
Further, the device also comprises a precise liquid injection system for precisely controlling the injection quantity of the reagent injected into the collecting bottle or the reaction tank;
accurate annotate liquid system includes: the infusion pipeline, the first one-way valve, the quantitative pump, the liquid injection needle, the clear water pipeline, the clear water bottle, the clear water pump, the first control valve and the second one-way valve;
the input end of the infusion pipeline is connected with a liquid storage bottle, the output end of the infusion pipeline is connected with the liquid injection needle, and the infusion pipeline is sequentially provided with the first one-way valve and the quantitative pump for pumping the reagent in the liquid storage bottle into a collecting bottle or a reaction tank;
the first one-way valve is used for limiting one-way flow of the reagent from the liquid storage bottle to the liquid injection needle;
the infusion pipeline comprises a first liquid section arranged between the first one-way valve and the quantitative pump and a second liquid section arranged between the quantitative pump and the liquid injection needle;
The clear water bottle is used for storing clear water such as distilled water or purified water; one end of the clear water pipeline is connected with the clear water bottle, and the other end of the clear water pipeline is connected with the first liquid section;
the clear water pipeline is sequentially provided with the clear water pump, a first control valve and a second one-way valve;
the second one-way valve is used for limiting one-way flow from the clear water bottle to the first liquid section;
the first control valve is a normally open two-position three-way valve, and a control port of the first control valve is communicated with the second liquid section through a first control pipeline; when the dosing pump works, part of reagent in the second liquid section enters a control port of the first control valve through the first control pipeline, and the reset force of the reset piece in the first control valve is overcome to force the first control valve to change a working position so as to disconnect the clear water pipeline;
when the quantitative pump stops working, the first control valve is restored to the normally open initial station under the action of the internal reset piece of the first control valve, so that the clear water pipeline is communicated; the clear water pump works and is used for pumping clear water in the clear water bottle into the first liquid section, further flushing the first liquid section, the quantitative pump and the second liquid section, and further pumping residual reagents in the first liquid section, the quantitative pump and the second liquid section into the collecting bottle or the reaction tank through the clear water.
According to the improved technical scheme, a chemiluminescent reagent, such as luminol and hydrogen peroxide mixed alkali solution, is added into a collecting bottle through a mechanical arm, after a chemical photoreaction occurs, the mixture is uniformly stirred by a magnetic stirrer, the collecting bottle is fixed in volume by an infrared sensor, and finally the reacted liquid is injected into a reaction tank of a chemiluminescent detector through a liquid absorber of the mechanical arm, and chemiluminescent detection is performed through a photomultiplier; or adding a color reagent through a mechanical arm, uniformly stirring by using a magnetic stirrer, fixing the volume of a collecting bottle by using an infrared sensor and a bottom electronic balance, and finally injecting the reacted liquid into a reaction tank of a spectrophotometer through a liquid absorber of the mechanical arm, and detecting through a colorimeter principle.
By adopting the technical scheme, the invention has the following beneficial effects:
1. according to the solid sample detection device provided by the invention, when the four heating modules face different processing steps, the proper heating modules are selected according to the temperature required by the current processing step, the heating modules are connected and fixed with the machine body, and then the reaction tank is placed in the heating modules, so that one device can process the work of a plurality of original devices, and the purposes of saving space, automatically operating and reducing the cost of sample pretreatment are achieved; particularly, in the detection of heavy metals in soil and the analysis and detection of food ingredients, when a large number of samples need to be detected, high-throughput automatic detection equipment is urgently needed to carry out automatic standard flow operation. In addition, the solid sample pretreatment experiment often needs to be used for searching and optimizing methods and conditions by a large number of parallel experiments, and a plurality of experiments under different conditions are generally manually carried out, so that the solid sample detection device can switch different pretreatment methods, and a plurality of samples can be automatically treated in parallel, thereby improving the efficiency and reducing the error.
2. A solid sample detection device comprises the functions of sample chemical digestion, solvent extraction, alkali extraction, automatic filtration, reaction liquid collection, nitrogen blowing concentration, automatic pH value adjustment, constant volume, chemiluminescence detection, colorimeter detection and the like, and realizes that a plurality of pretreatment steps and detection of a solid sample are automatically carried out on one instrument.
3. The sample reaction and filtration collection module are integrally connected, so that the filtration and liquid transfer are convenient, the nitrogen blowing concentration, the automatic pH value adjustment and the constant volume can be automatically carried out, the experimental operation steps and the complicated process are simplified, the manual labor and time cost can be reduced, and the experimental safety and the experimental error are improved. The method is suitable for multi-step automatic operation of pretreatment experiments of a plurality of different solid samples, can also be used for searching experimental conditions of pretreatment of a certain solid sample, such as researching effects and influences of steps of different pretreatment methods, carrying out parallel experiments of influence factors and condition optimization of the pretreatment methods, and the like, is also suitable for developing standard substances such as heavy metal content standard substances and matrix component content standard substances in a matrix, can be used for sample pretreatment experiments of uniformity, stability examination and fixed values, can reduce human errors, and is beneficial to controlling experimental parallel conditions.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings which are required in the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the description below are some embodiments of the invention and that other drawings may be obtained from these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic structural diagram of a high-throughput integrated solid sample detection device provided in embodiment 1 of the present invention;
FIG. 2 is a schematic view of the hidden door of FIG. 1 showing a reaction tank and a heating module;
FIG. 3 is a schematic structural view of a reaction tank;
FIG. 4 is a cross-sectional view of a reaction tank;
FIG. 5 is a schematic diagram of the operation of the precision liquid injection system of example 2;
FIG. 6 is a schematic diagram of the operation of the precision liquid injection system of example 3;
FIG. 7 is a schematic diagram of the operation of the precision liquid injection system of example 4;
fig. 8 is a schematic diagram of the operation of the hydraulic delay device in example 4.
Reference numerals:
1-a reaction tank; 11-a tank body; 12-sealing the cover; 13-a suction and injection tube; 14-a filter element; 2-a heating module; 3-controlling a host; 4-collecting bottles; 5-a mechanical arm; 6-filtering membrane; 7-a liquid storage bottle; 20-a precise liquid injection system; 21-a fixed displacement pump; 22-a liquid injection needle; 23-an infusion line; 231-a first fluid path section; 232-a second section of fluid; 24-a first one-way valve; 30-one-outlet multi-inlet reversing valve; 41-a clear water bottle; 42-a clean water pipeline; 43-a clean water pump; 44-a first control valve; 45-a second one-way valve; 51-gas line; 52-an air pump; 53-a second control valve; 54-a third one-way valve; 55-an air filtration device; 56-a second control line; 57-a third control valve; 58-a third control line; 60-a hydraulic delay device; 61-main way; 62-a first branch; 63-a fourth one-way valve; 64-adjustable throttle valve; 65-pouch.
Detailed Description
The invention is further illustrated with reference to specific embodiments.
Example 1
As shown in fig. 1 and 2, the high-throughput integrated solid sample detection device provided in this embodiment includes a reaction tank 1 and a heating module 2, which are disposed in a body, wherein the reaction tank 1 is used for containing a sample, the reaction tank 1 is disposed in the heating module 2, and the heating module 2 is used for heating the reaction tank 1; the heating module 2 comprises at least the following four types: the device comprises a water bath oscillation heating unit, a graphite digestion heating unit, a multi-site magnetic stirring heating unit and a metal bath heating unit, wherein four heating modules 2 are respectively used for sample pretreatment in different steps, and each heating module 2 is detachably and fixedly connected with a machine body; in this embodiment, each heating module 2 is electrically connected to the machine body through an aviation plug, and each heating module 2 is detachably and fixedly connected to the machine body through a buckle.
As shown in fig. 1 and 2, the machine body further comprises a control host 3 and a collection bottle 4, the collection bottle 4 is provided with a plurality of collection bottles 4, the collection bottles 4 are all placed above the reaction tank 1, all the collection bottles 4 are placed on a collection tray, the collection tray is fixed in the machine body, the collection bottles 4 and the reaction tank 1 are divided into an upper layer and a lower layer, the collection bottle 4 is placed on the upper layer and is used as a collection tray, the reaction tank 1 is placed on the lower layer and is used as a heating reaction tray, the collection tray and the heating reaction tray are rotatable, the collection tray is provided with a liquid injection hole, the lower part of the liquid injection hole is used as a liquid injection station of the reaction tank 1 on the heating reaction tray, and the liquid injection hole is used for injecting liquid into the reaction tank 1 on the heating reaction tray; the collecting bottle 4 is used for collecting liquid after sample heating reaction, the collecting bottle 4 is connected with the reaction tank 1 through a vacuum pump, and the control host 3 is used for adding reagents to the reaction tank 1 and the collecting bottle 4.
The bottom of the collecting tray is provided with a multi-position magnetic stirrer and an electronic balance, the magnetic stirrer is used for magnetically stirring the collecting bottle 4, and the electronic balance is used for weighing the collecting bottle 4; the lateral wall of collecting tray is provided with infrared inductor for respond to the liquid level of collecting bottle 4, infrared inductor and electronic balance are used for carrying out preliminary constant volume to the liquid in the collecting bottle 4 simultaneously.
The control host 3 is provided with a control panel which is used for programming method conditions and automatically running multiple sample sequences, and meanwhile, the control panel can be connected with a computer and is used for performing computer control and remote control; the back of the control host 3 is provided with a heat dissipation device.
The machine body is provided with a sealing door which is used for sealing the heating reaction plate, and the sealing door is provided with an exhaust pipe. When the chemical digestion module is used for acid digestion, acid can be removed, the upper and lower doors are closed, the exhaust pipe is led into the outdoor and ventilation pipelines, and the upper exhaust device is opened to accelerate acid removal and gas discharge.
In the embodiment, the upper top, the lower bottom, the periphery, the airtight door and the like of the heating reaction disk are all made of anti-corrosion and acid and alkali-resistant materials, so that the heating reaction disk can resist acid and alkali corrosion, has a detachable and replaceable structure, can be replaced locally, and the pipelines for connecting the acid liquor and the alkali liquor by the instrument are all made of the acid and alkali-resistant materials.
As shown in fig. 1, the control host 3 is provided with a mechanical arm 5 and a liquid storage bottle 7, the liquid storage bottle 7 is placed in a groove formed in the control host 3, the liquid storage bottle 7 is used for storing a required reagent, the mechanical arm 5 is provided with a plurality of pipelines, the mechanical arm 5 moves in the host, and the mechanical arm is used for adding the reagent into the reaction tank 1 and the collecting bottle 4 through the pipelines; a quantitative pump 21 is arranged in the machine body, and the quantitative pump 21 is used for quantitatively conveying the reagent into the reaction tank 1 and the collecting bottle 4; the mechanical arm 5 is provided with a liquid injection needle 22, a liquid suction device (not shown), an acidity electrode (not shown), a nitrogen blowing needle (not shown) and a stirrer (not shown), and the liquid injection needle 22, the liquid suction device, the acidity electrode, the nitrogen blowing needle and the stirrer are all detachably connected with the mechanical arm 5. The acidity electrode and the quantitative pump 21 are electrically connected with the control host 3, the quantitative pump 21 pumps the acid-base liquid in the liquid storage bottle 7 to the liquid injection needle 22 on the mechanical arm 5 through the liquid delivery pipeline 23, then the acid-base liquid is conveyed into the collecting bottle 4 (or the reaction bottle 1) through the liquid injection needle 22, and then the pH value is automatically adjusted to a preset pH value through the acidity electrode detection.
The liquid storage bottle 7 includes: solvent bottles, acid liquor bottles, alkali liquor bottles, chemiluminescent reagent bottles, color developing agent bottles and the like. Be provided with storage device on the arm 5, storage device is used for accomodating a plurality of pipeline and fixes on arm 5, and storage device is buckle or ribbon.
The control host 3 is also provided with an ultraviolet-visible light spectrophotometer module which is used for detecting the color reaction of the liquid in the collecting bottle 4; the control host 3 is also provided with a chemiluminescent detector module which is used for carrying out chemiluminescent reaction detection on the liquid in the collecting bottle 4 through a photomultiplier. Adding a chemiluminescent reagent into a collecting bottle through a mechanical arm, for example, adding mixed alkali liquor of luminol and hydrogen peroxide into the collecting bottle, uniformly stirring by using a magnetic stirrer after a chemiluminescent reaction occurs, fixing the volume of the collecting bottle by using an infrared sensor, and finally injecting the reacted liquid into a reaction tank of a chemiluminescent detector through a liquid suction device of the mechanical arm, and carrying out chemiluminescent detection through a photomultiplier; or adding a color reagent through a mechanical arm, uniformly stirring by using a magnetic stirrer, fixing the volume of the collecting bottle by using an infrared sensor, and finally injecting the reacted liquid into a reaction tank of a spectrophotometer through a liquid absorber of the mechanical arm, and detecting by using a colorimeter principle.
As shown in fig. 3 and 4, the reaction tank 1 includes a tank 11, a sealing cover 12, a suction and injection pipe 13 and a filter 14, and the tank 11 includes the tank 11 of four materials: the tank body 11 made of polytetrafluoroethylene, the tank body 11 made of para-position polyphenyl, the tank body 11 made of plastic and the tank body 11 made of glass, and the tank bodies 11 made of different materials are applicable to the heating modules 2 with different temperatures; the sealing cover 12 seals the tank 11, and the sealing cover 12 is provided with ventilation holes for balancing the atmospheric pressure inside and outside the reaction tank 1 when the liquid is sucked by the suction and injection pipe 13; the suction and injection pipe 13 is fixedly connected with the sealing cover 12 and inserted into the tank 11, the filter piece 14 is used for filtering liquid passing through the suction and injection pipe 13, the filter piece 14 is internally provided with the filter membrane 6, the filter membrane 6 is used for filtering the liquid passing through the filter piece 14, the filter piece 14 is detachably connected with the suction and injection pipe 13, and the suction and injection pipe 13 is connected with the collecting bottle 4 through the vacuum pump.
When the reaction tank 1 is used for accelerating solvent extraction, a metal bath heating unit is configured, a metal jacket is sleeved outside the reaction tank 1, the metal jacket comprises a metal jacket and a metal cap, the metal jacket is in threaded connection with the metal cap, and the metal jacket is used for improving the capacity of the reaction tank 1 for bearing high pressure when accelerating solvent extraction.
The implementation principle of the high-flux integrated solid sample detection device provided by the embodiment of the invention is as follows: when the sample detection device is used, firstly, proper materials of the tank body 11 and the heating module 2 are selected according to the processing temperature of a sample, the heating module 2 is moved to a machine body, the heating module 2 is connected with the machine body by utilizing an aviation plug, the heating module 2 and the machine body can be electrified to perform heating work, then the sample is put into the reaction tank 1, the reaction tank 1 is moved to the heating module 2, then a processing reagent is added into the reaction tank 1 through the mechanical arm 5, the reaction tank 1 is stirred at normal temperature by utilizing a stirrer on the mechanical arm 5, then the heating module 2 is started to heat the reaction tank 1 to the design temperature, and the heating module 2 is controlled to keep the temperature for the required time.
Then after the reaction tank 1 is cooled, the bottle cap is moved to drive the suction and injection pipe 13 to be inserted into the tank 11, the tank 11 is sealed by the sealing cover 12, the vacuum pump is started to suck the liquid reacted in the reaction tank 1 through the suction and injection pipe 13, when the liquid passes through the filter element 14 in the suction and injection pipe 13, the liquid is filtered by the filter membrane 6 in the filter element 14, and the filtered liquid enters the collecting bottle 4 through the suction and injection pipe 13 and the vacuum pump; then, the mechanical arm 5 is controlled to add the medicament into the collected collecting bottle 4, a series of operations such as pH adjustment and constant volume are performed on the collected liquid, and the heating module 2 is replaced to realize one machine with multiple purposes, so that the purposes of saving space, automatically operating and reducing the cost of sample pretreatment are achieved.
The following describes a specific application of the present embodiment in conjunction with specific practical cases.
1. The hexavalent chromium in the soil is measured by an alkali solution extraction method: a water bath oscillation heating unit or a water bath heating multi-site magnetic stirring heating unit is selected, a plastic material is selected as a reaction tank 1, 5.0g of air-dried, ground and sieved soil sample is weighed into the reaction tank 1 in a machine body, 50.0mL of sodium hydroxide/sodium carbonate extractant is added into the reaction tank through a mechanical arm 5, 0.4g of magnesium chloride and 0.50mL of dipotassium hydrogen phosphate-potassium dihydrogen phosphate buffer solution are added, a sealing cover is screwed up, the reaction tank is placed into a water bath oscillation heating module 2, normal temperature oscillation is carried out for 10min, the water bath oscillation heating unit is set with 95 ℃ and a certain oscillation frequency, and then the reaction tank is heated to 95 ℃ and oscillated with a certain frequency for 1h. Opening an instrument fan, radiating and cooling, after cooling a sample, connecting a pipeline between the reaction tank 1 and the collecting bottle 4, opening a pump to filter, collecting filtrate in the collecting bottle 4, flushing the reaction tank 1 for three times by adding water into the reaction tank 1 through the mechanical arm 5, opening the pump to filter, and collecting cleaning liquid in the collecting bottle 4. The cover of the collecting bottle 4 is opened, the pH electrode on the mechanical arm 5 is used for electrically controlling the automatic dropwise adding of nitric acid solution through the main control unit, and the pH is regulated to 7.5. Solvent addition is carried out through the mechanical arm 5, preliminary volume fixing is carried out through infrared rays, and accurate volume fixing is carried out through the electronic balance. The blank experiment was identical to the sample except that no sample was added. Establishing a working curve, respectively transferring a series of hexavalent chromium standard use solutions, preparing a working curve solution, controlling the rotation of a tray of an upper collecting tray through software according to the steps of sample preparation, transferring a certain collecting bottle 4 to a weighing tray of an electronic balance, adding a solvent through a mechanical arm 5, performing preliminary volume fixing through infrared rays, and performing accurate volume fixing through the electronic balance. The blank experiment is identical to the pretreatment except that no sample is added.
The method comprises the following steps: and extracting a proper amount of sample from the liquid with the constant volume of the collecting bottle 4, and detecting the hexavalent chromium content in the soil by using instruments such as a quadrupole Inductively Coupled Plasma Mass Spectrometer (ICPMS), an inductively coupled plasma emission spectrometer (ICP-OES), an atomic absorption photometer or an atomic fluorescence photometer and the like. The second method is as follows: when no interference of reducing substances, organic matters, chromaticity and the like exists, a certain amount of samples are taken from the collecting bottle 4 through the mechanical arm 5 under the magnetic stirring condition, are added into the empty collecting bottle 4 for neutralization, then are diluted with water to reach the constant volume of 50mL, sulfuric acid and phosphoric acid are added, 0.5mL of each of the sulfuric acid and the phosphoric acid is added, after the magnetic stirring is uniform, 2.0mL of a chromogenic reagent such as a dibenzoyl dihydrazide solution is added through the mechanical arm 5, and the mixture is placed for 10min after the magnetic stirring is uniform. And (3) taking water as a reference, measuring absorbance at 540nm, subtracting absorbance of a blank experiment, measuring hexavalent chromium content in the solution by a colorimeter principle, and calculating to obtain hexavalent chromium content in soil.
2. And (3) detecting the pH value in the soil: and (3) respectively placing 10g of the screened soil samples into the plastic reaction tank 1, respectively adding 25ml of water into the mechanical arm 5, vibrating the mechanical arm 5 in the room-temperature water bath vibration heating module 2 for 1min or stirring the mechanical arm by the multi-site magnetic stirring heating unit for 1min to fully disperse soil particles, placing the mechanical arm 5 for 30min, respectively inserting pH electrodes on the mechanical arm 5 into the liquid to be tested, and testing the pH value of the liquid in each open reaction tank 1.
3. The method for detecting the cadmium content in the soil comprises the following steps: adopt graphite to clear up the module, the retort selects polytetrafluoroethylene material, weigh 5.0g and air-dry, grind, the soil after sieving in the retort 1 of organism, add certain proportion's multiple acid through arm 5, under certain intensification procedure, carry out graphite and clear up sour, open the instrument fan, cool down in dispelling the heat, after the sample cooling, connect the pipeline between good and the collecting bottle 4, open the pump and filter, collect the filtrate in the collecting bottle 4, add water to the retort 1 through arm 5 and wash retort 1 three times, open the pump and filter, collect the washing liquid in the collecting bottle 4. Solvent addition is carried out through the mechanical arm 5, preliminary volume fixing is carried out through infrared rays, and accurate volume fixing is carried out through the electronic balance. The blank experiment is identical to the pretreatment except that no sample is added. Detecting by using a chemiluminescent detector or a spectrophotometer on the instrument; the liquid in the collecting bottle 4 can also be detected by using four-pole Inductively Coupled Plasma Mass Spectrometer (ICPMS), inductively coupled plasma emission spectrometer (ICP-OES), atomic absorption photometer and other instruments.
4. Examination of uniformity of milk powder component analysis standard substances: adopt graphite to clear up the heating element, retort 1 selects polytetrafluoroethylene material, extract the milk powder ingredient analysis standard substance of a certain quantity of units, respectively weigh a certain amount of samples in retort 1 in the organism, add certain proportion's multiple acid through arm 5, under certain temperature elevation procedure, carry out graphite and clear up the acid, open the instrument fan, cool down that dispels the heat, after the sample cooling, connect the pipeline between good and the collecting bottle 4, open the pump and filter, collect the filtrate in collecting bottle 4, add water to retort 1 through arm 5 and wash retort 1 three times, open the pump and filter, collect cleaning fluid in the collecting bottle 4. Solvent addition is carried out through the mechanical arm 5, preliminary volume fixing is carried out through infrared rays, and accurate volume fixing is carried out through the electronic balance. The blank experiment was identical to the other steps except that no sample was added. And testing the content of various elements in the milk powder by using four-pole Inductively Coupled Plasma Mass Spectrometer (ICPMS), inductively coupled plasma emission spectrometer (ICP-OES) and other instruments, and checking the uniformity of the milk powder component analysis standard substance.
Example 2
The present embodiment discloses a high-throughput integrated solid sample detection device substantially identical to embodiment 1, except that:
the embodiment further comprises a precision liquid injection system 20 for precisely controlling the injection amount of the solution (solvent, acid solution, alkali solution, chemiluminescent reagent or color developer, etc. in the liquid storage bottle 7) injected into the collection bottle 4 or the reaction tank 1 (or receiving container).
Referring to fig. 5, the precision liquid injection system 20 includes: the infusion pipeline 23, the first one-way valve 24, the dosing pump 21, the liquid injection needle 22, the clear water pipeline 42, the clear water bottle 41, the clear water pump 43, the first control valve 44 and the second one-way valve 45;
the input end of the infusion pipeline 23 is connected with the liquid storage bottle 7, the output end of the infusion pipeline 23 is connected with the liquid injection needle 22, and the infusion pipeline 23 is sequentially provided with the first one-way valve 24 and the quantitative pump 21 for pumping the reagent in the liquid storage bottle 7 into the collecting bottle 4 or the reaction tank 1;
the first one-way valve 24 is used for limiting one-way flow of the reagent from the liquid storage bottle 7 to the liquid injection needle 22;
the infusion line 23 includes a first fluid path section 231 provided between the first check valve 24 and the dosing pump 21, and a second fluid path section 232 provided between the dosing pump 21 and the injection needle 22;
The clean water bottle 41 is used for storing clean water such as distilled water or purified water; one end of the clear water pipeline 42 is connected with the clear water bottle 41, and the other end of the clear water pipeline 42 is connected with the first liquid section 231;
the clear water pipeline 42 is sequentially provided with a clear water pump 43, a first control valve 44 and a second one-way valve 45;
the second one-way valve 45 is used for limiting one-way flow of clear water from the water bottle 41 to the first liquid path section 231;
the first control valve 44 is a normally open two-position three-way valve (i.e. under the condition of no external control hydraulic pressure, the first control valve 44 maintains a communication state under the action of a reset element such as a spring in a valve body of the first control valve, so that the clean water pipeline 42 maintains a communication state), and a control port of the first control valve 44 is communicated with the second liquid section 232 through a first control pipeline 441; when the dosing pump 21 works, part of the reagent in the second liquid section 232 enters the control port of the first control valve 44 through the first control pipeline 441, and the reset force of the reset piece in the first control valve 44 is overcome to force the first control valve 44 to change the working position so as to disconnect the clear water pipeline 42;
when the metering pump 21 stops working, the first control valve 44 is restored to the initial station which is normally open under the action of the internal reset piece of the first control valve, and then the clear water pipeline 42 is communicated; the clean water pump 43 is operative to input clean water in the clean water bottle 41 into the first liquid section 231, and further flush (part of) the first liquid section 231, the dosing pump 21 and the second liquid section 232, so as to input the reagents remaining in the first liquid section 231, the dosing pump 21 and the second liquid section 232 into the collection bottle 4 or the reaction tank 1 through the clean water.
The control host (the internal controller thereof) is connected with the clean water pump 43, and can control the starting time and the working time of the clean water pump 43 and the dosage of the clean water for flushing the pipeline.
More preferably, the device further comprises an out-multiple-inlet reversing valve 30 (or called an in-multiple-outlet reversing valve), wherein a plurality of input ports of the out-multiple-inlet reversing valve 30 are respectively connected with the plurality of liquid storage bottles 7 through different input branches, and an output port of the out-multiple-inlet reversing valve 30 is connected with an input end of the infusion pipeline 23 for the infusion pipeline 23 to be selectively connected with one of the liquid storage bottles 7, so that the delivery of different reagents is realized. The one-out multiple-in reversing valve 30 is a prior art and will not be described in detail herein.
The application can automatically and quickly start the clean water pump 43 and communicate with the clean water pipeline 42 after the quantitative pump 21 stops working, wash part of the first liquid section 231, the quantitative pump 21 and the second liquid section 232, and flush the residual reagent into the collecting bottle 4 or the reaction tank 1, thereby ensuring the accuracy of reagent dosage input, and simultaneously the cleaning work can prepare for the subsequent pumping of other reagents, avoid mutual interference and influence of different reagents and also ensure the accuracy of reagent dosage input.
Example 3
The embodiment discloses a solid sample detection device which is the same as embodiment 2, except that:
referring to fig. 6, the present embodiment further includes: a gas line 51;
one end of the gas pipeline 51 is connected with a dry gas source (a nitrogen tank, an inert gas tank or one end of the gas pipeline 51 is opened and directly connected with the atmosphere), and the other end of the gas pipeline 51 is connected with the first liquid section 231;
the air pipe 51 is provided with an air pump 52, a second control valve 53 and a third one-way valve 54 in sequence;
the third one-way valve 54 is used to define a one-way flow of drying gas from the drying gas source to the first liquid path segment 231;
the second control valve 53 is a normally open two-position three-way valve (i.e. under the condition of no external control pressure, the second control valve 53 maintains a communication state under the action of a reset element such as a spring in a valve body of the second control valve 53, so that the gas pipeline 51 maintains a communication state), and a control port of the second control valve 53 is communicated with the second liquid pipeline section 232 through a second control pipeline 56; when the dosing pump 21 works, part of reagent in the second liquid path section 232 enters the control port of the second control valve 53 through the second control pipeline 56, and the reset force of the reset piece in the second control valve 53 is overcome to force the second control valve 53 to change the working position so as to disconnect the gas pipeline 51;
When the metering pump 21 stops working, the second control valve 53 is restored to the initial station which is normally open under the action of the internal resetting piece of the second control valve, and then the gas pipeline 51 is communicated; the air pump 52 is operated to pump dry air into the first liquid path 231 and air-dry (part of) the second liquid path 232, the dosing pump 21 and the second liquid path 232; namely, the first liquid path 231, the dosing pump 21 and the second liquid path 232 are removed.
Wherein, when the fixed displacement pump 21 is operated, the pressure in the second fluid path section 232 is defined as the reagent pressure P 0 The first control valve 44 controls the set pressure of the port (i.e., the threshold pressure forcing the replacement state of the first control valve 44) to the first threshold pressure P 1 The set pressure of the control port of the second control valve 53 (i.e., the threshold pressure forcing the replacement state of the second control valve 53) is the second threshold pressure P 2 Wherein the reagent pressure P 0 Respectively greater than the first threshold pressure P 1 And a second threshold pressure P 2 Thereby effecting control of the first control valve 44 and the second control valve 53.
When the clean water pump 43 is in operation, the pressure in the second fluid path section 232 is defined as the clean water pressure P 3 Clear water pressure P 3 Are all smaller than the first threshold pressure P 1 And a second threshold pressure P 2 Avoiding the need for a first control valve 44 and a second control valve 53.
Similarly, when the air pump 52 is operated, the pressure in the second fluid path segment 232 is defined as the air pressure P 4 Pressure of gas P 4 Are all smaller than the first threshold pressure P 1 And a second threshold pressure P 2 Control of the first control valve 44 and the second control valve 53 is avoided.
Wherein, the control host (the internal controller thereof) is connected with the air pump 52, and can control the starting time and the working time of the air pump 52.
More preferably, the air duct 51 is provided with an air filtering device 55 for filtering the dry air.
In this embodiment, the drying gas is used to air-dry the (part of) second liquid section 232, the dosing pump 21 and the second liquid section 232, so as to remove the residual liquid in the first liquid section 231, the dosing pump 21 and the second liquid section 232, thereby effectively avoiding the interference and influence of the residual liquid on the pumping amount of the subsequent reagent, and further improving the pumping amount and purity of the reagent.
Example 4
This embodiment is identical to embodiment 3 except that:
referring to fig. 7 and 8, more preferably, a solid sample detection device disclosed in the present embodiment further includes a third control valve 57 disposed on the clean water line 42;
The third control valve 57 is a normally open two-position three-way valve (i.e. under the condition of no external control pressure, the third control valve 57 maintains a communication state under the action of a reset element such as a spring in a valve body thereof, so that the clean water pipeline 42 maintains a communication state), and a control port of the third control valve 57 is communicated with the gas pipeline 51 through a third control pipeline 58;
when the air pump 52 works, part of dry gas in the gas pipeline 51 enters a control port of the third control valve 57 through the third control pipeline 58, and the third control valve 57 is forced to change working positions to disconnect the clean water pipeline 42 by overcoming the reset force of a reset piece in the third control valve 57;
when the air pump 52 stops working, the third control valve 57 is restored to the initial station which is normally open under the action of the reset piece in the air pump, and then the clear water pipeline 42 is communicated.
This ensures that the air pump 52 is operated, and when the second liquid path section 232, the dosing pump 21 and the second liquid path section 232 are (partially) air-dried, the clean water line 42 is kept in an open state, so that it is prevented from interfering with the drying process of the above-mentioned lines.
More preferably, the second control line 56 is provided with a hydraulic delay 60.
The hydraulic delay device 60 comprises a main circuit 61 and a first branch circuit 62 which are arranged in parallel, an adjustable throttle valve 64 is arranged on the main circuit 61, a fourth one-way valve 63 is arranged on the first branch circuit 62, and the fourth one-way valve 63 is used for limiting the one-way flow of the reagent from the second liquid section 232 to the second control valve 53;
The inlet and the outlet of the main circuit 61 are respectively connected to the second control pipeline 56 (or the main circuit 61 is used as a part of the pipeline to be connected to the second control pipeline 56);
and also comprises a bladder 65 made of elastic material, the inlet of bladder 65 being connected to the outlet of said main circuit 61 (the interface on the side close to said second control valve 53);
when the metering pump 21 works, part of the reagent in the second liquid path section 232 flows into the control port of the second control valve 53 through the first branch 62, so that the second control valve 53 is regulated and controlled, and part of the reagent enters the sac 65 to bulge the sac 65 (the sac 65 temporarily stores part of the reagent); when the metering pump 21 stops working, the pressure of the second fluid path 232 disappears, the reagent in the bag 65 is released under the action of the elastic force of the bag 65 and flows back (slowly) to the direction of the second fluid path 232 through the adjustable throttle valve 64, the control pressure at the control port of the second control valve 53 is reduced in a delayed manner, and the second control valve 53 is opened in a delayed manner (the duration of the delay is adjustable according to the limited flow of the adjustable throttle valve 64).
The working principle of this embodiment is that when the quantitative pump 21 stops working, the control pressure at the control port of the first control valve 44 first disappears, the first control valve 44 is first opened, the clear water pump 43 works, the clear water pump 43 in the clear water bottle 41 is put into the first liquid section 231, and then (part of) the first liquid section 231, the quantitative pump 21 and the second liquid section 232 are washed, and then the reagents remained in the first liquid section 231, the quantitative pump 21 and the second liquid section 232 are put into the collection bottle 4 or the reaction tank 1 through the clear water pump 43;
The hydraulic delay device 60 enables the control pressure of the control port of the second control valve 53 to be lower than the second threshold pressure P of the second control valve 53 after the control pressure is prolonged for a set time 2 The second control valve 53 is opened with a delay; the air pump 52 is operated, part of the dry gas in the gas pipeline 51 enters the control port of the third control valve 57 through the third control pipeline 58, and the reset force of the reset piece in the third control valve 57 is overcome to force the third control valve 57 to replace the working position so as to disconnect the clean water pipeline 42; that is, after the (part of) the first liquid path 231, the constant delivery pump 21, and the second liquid path 232 are rinsed with clean water for a set time, the air pump 52 is turned on, and the (part of) the first liquid path 231, the constant delivery pump 21, and the second liquid path 232 are dried with dry gas.
In this embodiment, degree of automation is high, and after every time reagent is carried, carry out clear water washing and drying treatment that bloies to the transfer line automatically to avoided the interference between the different reagents, guaranteed simultaneously and carried the accurate of dosage.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.

Claims (9)

1. The solid sample detection device is characterized by comprising a precise liquid injection system, wherein the precise liquid injection system is used for precisely controlling the injection amount of the reagent injected into a collecting bottle or a reaction tank;
accurate annotate liquid system includes: the device comprises an infusion pipeline, a first one-way valve, a dosing pump, a liquid injection needle, a clear water pipeline, a clear water bottle, a clear water pump, a first control valve and a second one-way valve;
the input end of the infusion pipeline is connected with a liquid storage bottle, the output end of the infusion pipeline is connected with the liquid injection needle, and the infusion pipeline is sequentially provided with the first one-way valve and the quantitative pump for pumping the reagent in the liquid storage bottle into a collecting bottle or a reaction tank;
the first one-way valve is used for limiting one-way flow of the reagent from the liquid storage bottle to the liquid injection needle;
the infusion pipeline comprises a first liquid section arranged between the first one-way valve and the quantitative pump and a second liquid section arranged between the quantitative pump and the liquid injection needle;
the clear water bottle is used for storing clear water such as distilled water or purified water; one end of the clear water pipeline is connected with the clear water bottle, and the other end of the clear water pipeline is connected with the first liquid section;
the clear water pipeline is sequentially provided with the clear water pump, a first control valve and a second one-way valve;
The second one-way valve is used for limiting one-way flow from the clear water bottle to the first liquid section;
the first control valve is a normally open two-position three-way valve, and a control port of the first control valve is communicated with the second liquid section through a first control pipeline; when the dosing pump works, part of reagent in the second liquid section enters a control port of the first control valve through the first control pipeline, and the reset force of the reset piece in the first control valve is overcome to force the first control valve to change a working position so as to disconnect the clear water pipeline;
when the quantitative pump stops working, the first control valve is restored to the normally open initial station under the action of the internal reset piece of the first control valve, so that the clear water pipeline is communicated; the clear water pump works and is used for pumping clear water in the clear water bottle into the first liquid section, further flushing the first liquid section, the quantitative pump and the second liquid section, and further pumping residual reagents in the first liquid section, the quantitative pump and the second liquid section into the collecting bottle or the reaction tank through the clear water.
2. The solid sample detection device according to claim 1, wherein the control host is connected to a clean water pump for controlling the start time, the working time and the clean water dosage for flushing the pipeline.
3. The solid sample detection device according to claim 1, further comprising an out-multiple-in reversing valve, wherein a plurality of input ports of the out-multiple-in reversing valve are respectively connected with a plurality of liquid storage bottles through different input branches, and an output port of the out-multiple-in reversing valve is connected with an input end of the infusion pipeline, so that the infusion pipeline can be selectively connected with one of the liquid storage bottles, and further conveying of different reagents is realized.
4. The solid sample testing device of claim 1, comprising a gas line;
one end of the gas pipeline is connected with a dry gas source, and the other end of the gas pipeline is connected with the first liquid section; the air pipeline is sequentially provided with an air pump, a second control valve and a third one-way valve;
the third one-way valve is used for limiting one-way flow of the drying gas from a drying gas source to the first liquid path section;
the second control valve is a normally open two-position three-way valve, and a control port of the second control valve is communicated with the second liquid section through a second control pipeline; when the dosing pump works, part of reagent in the second liquid section enters a control port of the second control valve through the second control pipeline, and the reset force of a reset piece in the second control valve is overcome to force the second control valve to change a working position so as to disconnect the gas pipeline;
When the quantitative pump stops working, the second control valve is restored to the normally open initial station under the action of the internal reset piece of the second control valve, and then the gas pipeline is communicated; the air pump works and is used for pumping dry gas into the first liquid section so as to air-dry the second liquid section, the quantitative pump and the second liquid section; namely, removing residual liquid in the first liquid path section, the constant delivery pump and the second liquid path section.
5. The solid sample detection device according to claim 4, wherein when the dosing pump works, the pressure in the second liquid path section is defined as the reagent pressure, the set pressure of the control port of the first control valve is a first threshold pressure, the set pressure of the control port of the second control valve is a second threshold pressure, and the reagent pressure is respectively larger than the first threshold pressure and the second threshold pressure, so that the control of the first control valve and the second control valve is realized.
6. The solid sample detection device according to claim 4, wherein when the clear water pump is in operation, the pressure in the second liquid path section is defined as clear water pressure, and the clear water pressure is smaller than the first threshold pressure and the second threshold pressure, so that the first control valve and the second control valve are prevented from being controlled.
7. The solid sample testing device according to claim 4, wherein the air pump is operated such that the pressure in the second fluid path section is defined as a gas pressure, and wherein the gas pressure is less than the first and second threshold pressures, thereby avoiding control of the first and second control valves.
8. The solid sample detection device according to claim 4, wherein the control host is connected to the air pump for controlling the start time and the operation time of the air pump.
9. The solid sample detection device according to claim 4, wherein an air filter device is provided on the gas line for filtering the dry gas.
CN202310982791.1A 2023-06-14 2023-06-14 Solid sample detection device Pending CN117030637A (en)

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