A solid sample detection device

Abstract

The present application relates to detection equipment technical field, especially to a kind of solid sample detection device, it includes accurate liquid injection system, for accurately control the reagent injection amount of injection collection bottle or reaction tank;Accurate liquid injection system includes: infusion pipeline, first check valve, dosing pump, liquid injection needle, clean water pipeline, clean water bottle, clean water pump, first control valve and second check valve;When dosing pump stops working, first control valve recovers to the initial position of normal open under the action of its internal reset piece, and then connects the clean water pipeline;The clean water pump works, for pumping clean water in the clean water bottle into the first liquid path section, and then flushing first liquid path section, dosing pump and second liquid path section, and then pumping the reagent remaining in first liquid path section, dosing pump and second liquid path section into collection bottle or reaction tank by clean water pump.Prepare for subsequent other reagent pumping, avoid different reagents interfering and influencing each other, also ensure the accuracy of reagent input dose.

Description

Technical Field

[0001] This invention relates to the field of testing equipment technology, and in particular to a solid sample testing device. Background Technology

[0002] In the field of chemical element detection of solid samples, the first step in detecting the chemical element content of a solid sample is to perform pretreatment on the sample. Pretreatment methods include chemical digestion and alkaline extraction.

[0003] Rapid solvent extraction (RFE) is a viable method for detecting semi-volatile organic compounds in solid samples. It offers advantages such as low solvent consumption, speed, and high recovery rates. RFE is an automated method that uses organic solvents under elevated temperature and pressure conditions; currently, most instruments for this method are imported.

[0004] Sample pretreatment generally consists of several steps, including sample decomposition, solvent extraction, sample filtration, and quantitative concentration. The pretreatment process involves chemical digestion, rapid solvent extraction, and alkaline extraction, as well as chemical dissolution, filtration, rinsing, acid removal, nitrogen blowing concentration, pH adjustment, and volume determination. In existing technologies, these steps are typically performed separately using independent instruments or containers, resulting in cumbersome procedures, high labor costs, multiple manual transfers and additions of liquids, poor safety, and significant experimental errors. Furthermore, the laboratory setup requires multiple instruments such as graphite digesters, solvent extraction instruments, filtration equipment, and nitrogen blowing concentrators, leading to large equipment footprint, low automation, and high sample testing costs.

[0005] In view of the aforementioned requirements, a solid sample detection device is needed. Summary of the Invention

[0006] The purpose of this invention is to provide a solid sample detection device to solve the technical problem of high sample detection cost in the prior art. This application is a divisional application of the original application number 2023107053668 entitled "A High-Throughput Integrated Solid Sample Detection Device".

[0007] To solve the above-mentioned technical problems, the present invention provides a high-throughput integrated solid sample detection device, including a reaction vessel and a heating module disposed within the device body. The reaction vessel is used to hold the sample, and the heating module is disposed within the heating module for heating the reaction vessel.

[0008] The heating module includes at least four types: a water bath oscillation heating unit, a graphite digestion heating unit, a multi-site magnetic stirring heating unit, and a metal bath heating unit. The four types of heating modules are used for sample pretreatment in different method steps, and each heating module is detachably and fixedly connected to the machine body.

[0009] Through the above-mentioned improved technical solution, by selecting the appropriate heating module according to the temperature required for the current processing step when facing different processing steps, connecting and fixing the heating module to the machine body, and then placing the reaction vessel inside the heating module, one device can handle the work of multiple devices, thus achieving the goals of saving space, automating operation, and reducing the cost of sample pretreatment.

[0010] Furthermore, each of the heating modules is electrically connected to the aircraft body via an aviation plug.

[0011] The improved technical solution described above allows for quick electrical connection between the heating module and the aircraft body via an aviation plug, enhancing the ease of replacing the heating module.

[0012] Furthermore, each of the heating modules is detachably and securely connected to the body via a snap fastener.

[0013] The improved technical solution described above enhances the mechanical connection between the instant heating module and the body by using a snap fastener, thereby improving the stability of the connection between the heating module and the body.

[0014] Furthermore, the device also includes a control unit and a collection bottle. Several collection bottles are provided and are placed above the reaction vessel. The collection bottles are used to collect the liquid after the sample is heated and reacted. The collection bottles are connected to the reaction vessel via a vacuum pump. The control unit is used to add reagents to the reaction vessel and the collection bottles.

[0015] Preferably, the collection bottle is placed on a collection tray, and the collection tray is equipped with a multi-position magnetic stirrer located at the bottom of the collection bottle. The multi-position magnetic stirrer is used to magnetically stir the liquid in the collection bottle.

[0016] Preferably, a weighing module is fixedly connected to the collection tray for weighing the collection bottles. The weighing module can be existing technology, such as an electronic balance.

[0017] Preferably, an infrared sensor is fixedly connected to the collection tray. The infrared sensor is used to sense the liquid level in the collection bottle, thereby performing preliminary volume adjustment of the liquid in the collection bottle.

[0018] Furthermore, the control host is equipped with a robotic arm and a storage bottle. The storage bottle is used to store the required reagents. The robotic arm is equipped with several pipes. The robotic arm moves within the machine body and adds reagents to the reaction vessel and collection bottle through the pipes.

[0019] Preferably, the storage bottles include: solvent bottles, acid bottles, alkali bottles, chemiluminescent reagent bottles, color developer bottles, etc.

[0020] Preferably, the robotic arm is equipped with a storage device for storing and fixing several pipes to the robotic arm.

[0021] Preferably, the storage device is a snap fastener.

[0022] Preferably, the storage device is a cable tie.

[0023] Furthermore, the machine body is equipped with a metering pump, and the end of the robotic arm is equipped with an injection needle; the storage bottle is connected to the injection needle through an infusion line, and the metering pump is installed on the infusion line to quantitatively deliver the reagent to the reaction vessel and / or collection bottle.

[0024] Furthermore, the robotic arm is also equipped with a liquid aspirator, an acidity electrode, a nitrogen blowing needle, and a stirrer, all of which are detachably connected to the robotic arm.

[0025] Furthermore, the reaction vessel includes a vessel body, a sealing cap, a suction pipe, and a filter element. The sealing cap seals the vessel body, the suction pipe is fixedly connected to the sealing cap and inserted into the vessel body, the filter element is fixedly connected to the suction pipe, and the filter element is used to filter the liquid passing through the suction pipe. The suction pipe is connected to a vacuum pump.

[0026] With the above-mentioned improved technical solution, after the sample and reagent in the reaction vessel have completed the heating reaction, the vacuum pump is started to draw the liquid in the reaction vessel out of the vessel through the suction pipe. When the liquid passes through the filter at the suction pipe, the liquid enters the collection bottle after being filtered.

[0027] Furthermore, the filter element is provided with a filter membrane, which is used to filter the liquid passing through the filter element, and the filter element is detachably connected to the suction pipe.

[0028] The improved technical solution described above makes the filter element and the suction pipe detachable, which makes it easy to remove the filter element from the suction pipe and then replace the filter membrane inside the filter element.

[0029] Furthermore, the tank can be made of polytetrafluoroethylene, plastic, or glass, with different materials suitable for heating modules at different temperatures.

[0030] Preferably, when the reaction vessel is used to accelerate solvent extraction, it is equipped with a metal bath heating unit. The reaction vessel is covered with a metal jacket, which includes a metal sleeve and a metal cap. The metal sleeve and the metal cap are threaded together. The metal jacket is used to enhance the reaction vessel's ability to withstand high pressure during accelerated solvent extraction.

[0031] Furthermore, the control unit is also equipped with a UV-Vis spectrophotometer, which is used to detect the colorimetric reaction of the liquid in the collection bottle.

[0032] Furthermore, the control unit is also equipped with a chemiluminescence detector module, which uses a photomultiplier tube to detect the chemiluminescence reaction of the liquid in the collection bottle.

[0033] Furthermore, it also includes a precision injection system for precisely controlling the amount of reagent injected into the collection bottle or reaction vessel;

[0034] The precision infusion system includes: the infusion tubing, a first check valve, a metering pump, an infusion needle, a clean water tubing, a clean water bottle, a clean water pump, a first control valve, and a second check valve;

[0035] The infusion line is connected to the storage bottle at its input end and to the injection needle at its output end. The infusion line is provided with the first one-way valve and the metering pump in sequence, which are used to pump the reagent in the storage bottle into the collection bottle or reaction vessel.

[0036] The first one-way valve is used to limit the one-way flow of reagent from the storage bottle to the injection needle;

[0037] The infusion line includes a first fluid passage section disposed between the first one-way valve and the metering pump, and a second fluid passage section disposed between the metering pump and the injection needle;

[0038] The water bottle is used to store distilled water or purified water, etc.; one end of the water pipe is connected to the water bottle, and the other end of the water pipe is connected to the first liquid channel section.

[0039] The clean water pipeline is sequentially equipped with the clean water pump, the first control valve, and the second check valve.

[0040] The second check valve is used to limit the one-way flow of water from the water bottle to the first liquid path section;

[0041] The first control valve is a normally open two-position three-way valve. The control port of the first control valve is connected to the second liquid circuit through the first control pipeline. When the metering pump is working, part of the reagent in the second liquid circuit enters the control port of the first control valve through the first control pipeline, which overcomes the reset force of the internal reset element of the first control valve and forces the first control valve to change its working position and disconnect the clean water pipeline.

[0042] When the metering pump stops working, the first control valve returns to its normally open initial position under the action of its internal reset component, thereby connecting the water pipeline; the water pump works to pump water from the water bottle into the first liquid path section, thereby flushing the first liquid path section, the metering pump, and the second liquid path section, and then pumping the reagents remaining in the first liquid path section, the metering pump, and the second liquid path section into the collection bottle or reaction vessel through the water pump.

[0043] With the above-mentioned improved technical solution, a chemiluminescent reagent, such as a mixture of luminol and hydrogen peroxide, is added to the collection bottle via a robotic arm. After a chemiluminescent reaction occurs, the mixture is stirred evenly using a magnetic stirrer, and the collection bottle is brought to volume using an infrared sensor. Finally, the liquid after the reaction is injected into the reaction cell of a chemiluminescence detector using a liquid aspirator attached to the robotic arm, and chemiluminescence detection is performed using a photomultiplier tube. Alternatively, a colorimetric reagent is added via a robotic arm, stirred evenly using a magnetic stirrer, and the collection bottle is brought to volume using an infrared sensor and a bottom electronic balance. Finally, the liquid after the reaction is injected into the reaction cell of a spectrophotometer using a liquid aspirator attached to the robotic arm, and detection is performed using a colorimeter.

[0044] By adopting the above technical solution, the present invention has the following beneficial effects:

[0045] 1. This invention provides a solid sample detection device. By selecting the appropriate heating module based on the temperature required for different processing steps, and connecting and fixing the heating module to the main body, the reaction vessel is placed inside the heating module. This allows one device to handle the work of multiple devices, achieving space saving, automated operation, and reduced sample pretreatment costs. Especially in soil heavy metal detection and food component analysis, where large batches of samples need to be tested, high-throughput automated detection equipment is urgently needed for standardized and automated processes. Furthermore, solid sample pretreatment experiments often require numerous parallel experiments to explore and optimize methods and conditions. These are typically conducted manually under different conditions. This solid sample detection device can switch between different pretreatment methods and automatically process multiple samples in parallel, improving efficiency and reducing errors.

[0046] 2. A solid sample detection device, comprising functions such as sample chemical digestion, solvent extraction, alkali extraction, automatic filtration, reaction solution collection and nitrogen blowing concentration, automatic pH adjustment and volume adjustment, chemiluminescence detection and colorimeter detection, realizing the automatic performance of multiple pretreatment steps and detection of solid samples on one instrument.

[0047] 3. The sample reaction and filtration collection modules are integrated into a single unit, facilitating filtration and liquid transfer. It enables automated nitrogen blowing concentration, automatic pH adjustment, and volume determination, simplifying experimental procedures and reducing labor and time costs. Automated operation improves experimental safety and reduces errors. It is suitable for multi-step automated operation of pretreatment experiments on multiple different solid samples, and can also be used to explore experimental conditions for the pretreatment of a single solid sample, such as studying the effects and influences of different pretreatment methods, conducting parallel experiments to optimize the influencing factors and conditions of pretreatment methods, etc. It is also suitable for the development of standard materials such as heavy metal content standards in the matrix and matrix component content standards. It can be used for sample pretreatment experiments to examine homogeneity, stability, and determine values, reducing human error and facilitating the control of parallel experimental conditions. Attached Figure Description

[0048] To more clearly illustrate the specific embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the specific embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of the present invention. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.

[0049] Figure 1 This is a schematic diagram of the high-throughput integrated solid sample detection device provided in Embodiment 1 of the present invention;

[0050] Figure 2 for Figure 1 The diagram of the reaction vessel and heating module is hidden in the middle.

[0051] Figure 3 This is a schematic diagram of the reaction vessel.

[0052] Figure 4 This is a cross-sectional view of the reaction vessel;

[0053] Figure 5 This is a schematic diagram illustrating the working principle of the precision injection system in Example 2;

[0054] Figure 6 This is a schematic diagram illustrating the working principle of the precision injection system in Example 3;

[0055] Figure 7 This is a schematic diagram illustrating the working principle of the precision injection system in Example 4;

[0056] Figure 8 This is a schematic diagram of the working principle of the hydraulic delay device in Example 4.

[0057] Figure label:

[0058] 1-Reaction vessel; 11-Vat body; 12-Sealing cap; 13-Suction pipe; 14-Filter element; 2-Heating module; 3-Control unit; 4-Collection bottle; 5-Robotic arm; 6-Filter membrane; 7-Storage bottle; 20-Precision injection system; 21-Quantitative pump; 22-Injection needle; 23-Infusion line; 231-First liquid path; 232-Second liquid path; 24-First check valve; 30-One-outlet multi-inlet reversing valve; 41-Clear water bottle; 4 2-Clear water pipeline; 43-Clear water pump; 44-First control valve; 45-Second check valve; 51-Gas pipeline; 52-Air pump; 53-Second control valve; 54-Third check valve; 55-Air filter; 56-Second control pipeline; 57-Third control valve; 58-Third control pipeline; 60-Hydraulic delay device; 61-Main line; 62-First branch line; 63-Fourth check valve; 64-Adjustable flow valve; 65-Bag. Detailed Implementation

[0059] The present invention will be further explained below with reference to specific embodiments.

[0060] Example 1

[0061] like Figure 1 and Figure 2 As shown in the figure, this embodiment provides a high-throughput integrated solid sample detection device, including a reaction vessel 1 and a heating module 2 disposed within the device body. The reaction vessel 1 is used to hold the sample and is disposed within the heating module 2, which is used to heat the reaction vessel 1. The heating module 2 includes at least four types: a water bath oscillation heating unit, a graphite digestion heating unit, a multi-site magnetic stirring heating unit, and a metal bath heating unit. The four types of heating modules 2 are used for sample pretreatment in different steps, and each type of heating module 2 is detachably and fixedly connected to the device body. In this embodiment, each heating module 2 is electrically connected to the device body via an aviation plug, and each heating module 2 is detachably and fixedly connected to the device body via a buckle.

[0062] like Figure 1 and Figure 2As shown, the machine body also includes a control host 3 and collection bottles 4. Several collection bottles 4 are provided, and all collection bottles 4 are placed on top of the reaction vessel 1. All collection bottles 4 are placed on a collection tray, which is fixed inside the machine body. The collection bottles 4 and the reaction vessel 1 are divided into upper and lower layers. The upper layer, where the collection bottles 4 are placed, is a collection tray, and the lower layer, where the reaction vessel 1 is placed, is a heating reaction tray. Both the collection tray and the heating reaction tray can be rotated. The collection tray has a liquid injection hole, and below the liquid injection hole is a liquid injection station for the reaction vessel 1 on the heating reaction tray. The liquid injection hole is used to inject liquid into the reaction vessel 1 on the heating reaction tray. The collection bottles 4 are used to collect the liquid after the sample is heated and reacted. The collection bottles 4 are connected to the reaction vessel 1 through a vacuum pump. The control host 3 is used to add reagents to the reaction vessel 1 and the collection bottles 4.

[0063] The bottom of the collection tray is equipped with a multi-position magnetic stirrer and an electronic balance. The magnetic stirrer is used to magnetically stir the collection bottle 4, and the electronic balance is used to weigh the collection bottle 4. An infrared sensor is installed on the side wall of the collection tray to sense the liquid level in the collection bottle 4. The infrared sensor and the electronic balance are used to perform preliminary volume adjustment of the liquid in the collection bottle 4.

[0064] The control host 3 is equipped with a control panel, which is used for programming method conditions and automatic operation of multi-sample sequences. The control panel can also be connected to a computer for computer control and remote control. A heat dissipation device is provided on the back of the control host 3.

[0065] The machine body is equipped with a sealed door to enclose the heating reaction plate, and an exhaust pipe is installed on the sealed door. When using the chemical digestion module for acid digestion, acid can be expelled by closing the upper and lower doors, opening the exhaust pipe to the outside and ventilation ducts, and opening the upper exhaust device to accelerate the expulsion of acid and gas outdoors.

[0066] In this embodiment, the top, bottom, sides, and sealed door of the heating reaction plate are all made of corrosion-resistant and strong acid and alkali-resistant materials, which can resist acid and alkali corrosion and have a detachable and replaceable structure, allowing for partial replacement. The pipes connecting the instrument to the acid and alkali solutions are all made of strong acid and alkali-resistant materials.

[0067] like Figure 1As shown, the control host 3 is equipped with a robotic arm 5 and a storage bottle 7. The storage bottle 7 is placed in a groove on the control host 3 and is used to store the required reagents. The robotic arm 5 is equipped with several pipelines. The robotic arm 5 moves within the machine body and adds reagents to the reaction tank 1 and the collection bottle 4 through the pipelines. A metering pump 21 is installed within the machine body. The metering pump 21 is used to quantitatively deliver reagents to the reaction tank 1 and the collection bottle 4. The robotic arm 5 is equipped with an injection needle 22, a suction device (not shown), an acidity electrode (not shown), a nitrogen blowing needle (not shown), and a stirrer (not shown). The injection needle 22, the suction device, the acidity electrode, the nitrogen blowing needle, and the stirrer are all detachably connected to the robotic arm 5. The acidity electrode and metering pump 21 are electrically connected to the control host 3. The metering pump 21 pumps the acid and alkali solution in the storage bottle 7 to the injection needle 22 on the robotic arm 5 through the infusion line 23. Then, the injection needle 22 is used to deliver the acid and alkali solution to the collection bottle 4 (or reaction bottle 1). The pH value is then automatically adjusted to the preset pH value by detecting the acidity electrode.

[0068] The storage bottles 7 include: solvent bottles, acid bottles, alkali bottles, chemiluminescence reagent bottles, color developer bottles, etc. The robotic arm 5 is equipped with a storage device, which is used to store and fix several tubes to the robotic arm 5. The storage device is a buckle or cable tie.

[0069] The control host 3 is also equipped with a UV-Vis spectrophotometer module, which is used to detect the colorimetric reaction of the liquid in the collection bottle 4. The control host 3 is also equipped with a chemiluminescence detector module, which uses a photomultiplier tube to detect the chemiluminescence reaction of the liquid in the collection bottle 4. A chemiluminescence reagent, such as a mixture of luminol and hydrogen peroxide, is added to the collection bottle via a robotic arm. After the chemiluminescence reaction occurs, the mixture is stirred evenly using a magnetic stirrer, and the collection bottle is brought to volume using an infrared sensor. Finally, the liquid is injected into the reaction cell of the chemiluminescence detector using the robotic arm's suction device, and then detected by the photomultiplier tube. Alternatively, a colorimetric reagent can be added via the robotic arm, stirred evenly using a magnetic stirrer, and the collection bottle is brought to volume using an infrared sensor. Finally, the liquid is injected into the reaction cell of the spectrophotometer using the robotic arm's suction device, and then detected using a colorimeter.

[0070] like Figure 3 and Figure 4As shown, the reaction vessel 1 includes a vessel body 11, a sealing cap 12, a suction pipe 13, and a filter element 14. The vessel body 11 can be made of four different materials: polytetrafluoroethylene (PTFE), para-polystyrene (PPS), plastic, and glass. Different materials of the vessel body 11 are suitable for heating modules 2 at different temperatures. The sealing cap 12 seals the vessel body 11 and has a vent hole to balance the atmospheric pressure inside and outside the reaction vessel 1 when the suction pipe 13 draws liquid. The suction pipe 13 is fixedly connected to the sealing cap 12 and inserted into the vessel body 11. The filter element 14 is used to filter the liquid passing through the suction pipe 13. The filter element 14 has a filter membrane 6 inside, which is used to filter the liquid passing through the filter element 14. The filter element 14 is detachably connected to the suction pipe 13, and the suction pipe 13 is connected to the collection bottle 4 through a vacuum pump.

[0071] When reaction vessel 1 is used to accelerate solvent extraction, it is equipped with a metal bath heating unit. The reaction vessel 1 is covered with a metal outer jacket, which includes a metal sleeve and a metal cap. The metal sleeve and the metal cap are threaded together. The metal outer jacket is used to enhance the ability of reaction vessel 1 to withstand high pressure during accelerated solvent extraction.

[0072] The implementation principle of a high-throughput integrated solid sample detection device according to an embodiment of the present invention is as follows: When using the sample detection device, firstly, according to the sample processing temperature, select a suitable material for the container 11 and the heating module 2, move the heating module 2 to the machine body, and connect the heating module 2 to the machine body using an aviation plug, so that the heating module 2 and the machine body can be powered on to perform heating work. Then, put the sample into the reaction container 1, move the reaction container 1 to the heating module 2, and then add the processing reagent into the reaction container 1 through the robotic arm 5, and use the stirrer on the robotic arm 5 to stir the reaction container 1 at room temperature. Then, start the heating module 2 to heat the reaction container 1 to the design temperature, and control the heating module 2 to maintain the temperature for the required time.

[0073] After the reaction vessel 1 cools down, the bottle cap is moved to insert the suction tube 13 into the vessel body 11, and the vessel body 11 is sealed with the sealing cap 12. The vacuum pump is started to draw the reacted liquid in the reaction vessel 1 through the suction tube 13. When the liquid passes through the filter element 14 in the suction tube 13, it is filtered by the filter membrane 6 in the filter element 14. The filtered liquid enters the collection bottle 4 through the suction tube 13 and the vacuum pump. Then, the robotic arm 5 is controlled to add reagents to the collected bottle 4. A series of operations such as pH adjustment and volume determination are performed on the collected liquid. By replacing the heating module 2, the equipment can be used for multiple purposes, achieving the goals of saving space, automatic operation, and reducing the cost of sample pretreatment.

[0074] The specific application of this embodiment will be described below with reference to specific practical examples.

[0075] 1. Determination of hexavalent chromium in soil by alkaline solution extraction: A water bath shaking heating unit or a water bath multi-site magnetic stirring heating unit is selected. The reaction vessel 1 is made of plastic. 5.0g of the air-dried, ground, and sieved soil sample is weighed into the reaction vessel 1 inside the instrument. 50.0mL of sodium hydroxide / sodium carbonate extractant, 0.4g of magnesium chloride, and 0.50mL of dipotassium hydrogen phosphate-potassium dihydrogen phosphate buffer are added through the robotic arm 5. The sealing cap is tightened, and the instrument is placed in the water bath shaking heating module 2. Shaking is performed at room temperature for 10min. The water bath shaking heating unit is set to 95℃ and a certain shaking frequency. Then, the temperature is raised to 95℃ and shaken at a certain frequency for 1h. The instrument fan is turned on to dissipate heat and cool the sample. After the sample cools, the pipeline between the reaction vessel 1 and the collection bottle 4 is connected, and the pump is turned on for filtration. The filtrate is collected in the collection bottle 4. The reaction vessel 1 is rinsed three times with water through the robotic arm 5, and the filtration is performed again. The washing solution is collected in the collection bottle 4. Open the cap of collection bottle 4. Using the pH electrode on robotic arm 5, and with electrical control from the main control unit, automatically add nitric acid solution to adjust the pH to 7.5. Add solvent via robotic arm 5, perform preliminary volume adjustment using infrared light, and then perform precise volume adjustment using an electronic balance. The blank experiment is identical to the sample experiment except that no sample is added. Establish a working curve. Transfer a series of volumes of hexavalent chromium standard working solution, following the sample preparation steps, to prepare the working curve solution. Control the rotation of the upper collection tray via software, transferring one of the collection bottles 4 to the weighing pan of the electronic balance. Add solvent via robotic arm 5, perform preliminary volume adjustment using infrared light, and then perform precise volume adjustment using an electronic balance. The blank experiment is identical to the pretreatment except that no sample is added.

[0076] Method 1: Extract an appropriate amount of sample from the liquid in collection bottle 4 after dilution. Detect the hexavalent chromium content in the soil using instruments such as quadrupole inductively coupled plasma mass spectrometry (ICPMS), inductively coupled plasma optical emission spectrometry (ICP-OES), atomic absorption spectrophotometer, or atomic fluorescence spectrophotometer. Method 2: When there are no reducing substances, organic matter, or color interferences, under magnetic stirring, use robotic arm 5 to take a certain amount of sample from collection bottle 4 and add it to an empty collection bottle 4 for neutralization. Dilute with water to a final volume of 50 mL, add 0.5 mL each of sulfuric acid and phosphoric acid, and stir magnetically until homogeneous. Then, use robotic arm 5 to add 2.0 mL of a colorimetric reagent, such as diphenylcarbazide solution, and stir magnetically until homogeneous. Let stand for 10 min. Using water as a reference, measure the absorbance at 540 nm. Subtract the absorbance of the blank experiment, and determine the hexavalent chromium content in the solution using a colorimeter. Calculate the hexavalent chromium content in the soil.

[0077] 2. Soil pH detection: Take 10g of multiple sieved soil samples and place them in plastic reaction vessel 1. Add 25ml of water to each sample using robotic arm 5. Shake the samples for 1 minute in a room temperature water bath oscillation heating module 2 or stir for 1 minute in a multi-point magnetic stirring heating unit to fully disperse the soil particles. Let the samples stand for 30 minutes. Then, insert the pH electrodes on robotic arm 5 into the test liquids to test the pH value of the liquids in each open reaction vessel 1.

[0078] 3. Detection and Method of Cadmium Content in Soil: A graphite digestion module was used. The reaction vessel was made of polytetrafluoroethylene (PTFE). 5.0g of air-dried, ground, and sieved soil was weighed into reaction vessel 1 within the instrument. A certain proportion of various acids were added via robotic arm 5. Graphite digestion was performed under a specific temperature program, followed by acid removal. The instrument fan was turned on for cooling. After the sample cooled, the tubing between the sample and collection bottle 4 was connected, and the pump was turned on for filtration. The filtrate was collected in collection bottle 4. Water was added to reaction vessel 1 three times via robotic arm 5 for rinsing, and the pump was turned on for filtration. The washing liquid was collected in collection bottle 4. Solvent was added via robotic arm 5, and preliminary volume adjustment was performed using infrared spectroscopy. Precise volume adjustment was then performed using an electronic balance. The blank experiment was conducted without adding any sample; all other steps were the same as the pretreatment. The cadmium content in the soil can be detected using a chemiluminescence detector or spectrophotometer. Alternatively, the liquid in collection bottle 4 can be analyzed using instruments such as quadrupole inductively coupled plasma mass spectrometry (ICPMS), inductively coupled plasma optical emission spectrometry (ICP-OES), or atomic absorption spectrophotometer.

[0079] 4. Homogeneity Examination of Milk Powder Component Analysis Standard Material: A graphite digestion heating unit was used. Reaction vessel 1 was made of polytetrafluoroethylene (PTFE). A certain number of units of milk powder component analysis standard material were extracted, and a certain amount of sample was weighed into reaction vessel 1. Multiple acids in a certain proportion were added via robotic arm 5. Graphite digestion was performed under a specific temperature program to remove the acids. The instrument fan was turned on for cooling. After the sample cooled, the tubing between the sample and collection bottle 4 was connected, and the pump was turned on for filtration. The filtrate was collected in collection bottle 4. Reaction vessel 1 was rinsed three times with water via robotic arm 5, and the rinsing solution was collected in collection bottle 4. Solvent was added via robotic arm 5, and preliminary volume adjustment was performed using infrared spectroscopy. Precise volume adjustment was then performed using an electronic balance. The blank experiment was conducted identically to the other experiments, except that no sample was added. The content of multiple elements in milk powder was tested using instruments such as quadrupole inductively coupled plasma mass spectrometry (ICPMS) and inductively coupled plasma optical emission spectrometry (ICP-OES), and the uniformity of the standard substances for milk powder composition analysis was examined.

[0080] Example 2

[0081] This embodiment discloses a high-throughput integrated solid sample detection device, which is basically the same as that in Embodiment 1, except that:

[0082] This embodiment also includes a precision injection system 20, which is used to precisely control the injection volume of the solution (solvent, acid, alkali, chemiluminescent reagent or color developer, etc. in the storage bottle 7) into the collection bottle 4 or reaction vessel 1 (or receiving container).

[0083] Reference Figure 5 As shown, the precision injection system 20 includes: the infusion line 23, the first check valve 24, the metering pump 21, the injection needle 22, the clean water line 42, the clean water bottle 41, the clean water pump 43, the first control valve 44, and the second check valve 45.

[0084] The infusion line 23 is connected to the storage bottle 7 at its input end and to the injection needle 22 at its output end. The infusion line 23 is provided with the first one-way valve 24 and the metering pump 21 in sequence, which are used to pump the reagent in the storage bottle 7 into the collection bottle 4 or the reaction vessel 1.

[0085] The first one-way valve 24 is used to limit the one-way flow of reagent from the storage bottle 7 to the injection needle 22;

[0086] The infusion line 23 includes a first liquid section 231 disposed between the first one-way valve 24 and the metering pump 21, and a second liquid section 232 disposed between the metering pump 21 and the injection needle 22.

[0087] The water bottle 41 is used to store distilled water or purified water and other clean water; one end of the water pipe 42 is connected to the water bottle 41, and the other end of the water pipe 42 is connected to the first liquid section 231.

[0088] The clean water pipeline 42 is sequentially equipped with the clean water pump 43, the first control valve 44, and the second check valve 45.

[0089] The second one-way valve 45 is used to limit the one-way flow of clean water from the clean water bottle 41 to the first liquid path section 231;

[0090] The first control valve 44 is a normally open two-position three-way valve (that is, in the absence of external control hydraulic pressure, the first control valve 44 remains in a connected state under the action of springs and other reset components in its valve body, thereby keeping the clean water pipeline 42 connected). The control port of the first control valve 44 is connected to the second liquid section 232 through the first control pipeline 441. When the metering pump 21 is working, 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, overcoming the reset force of the reset component inside the first control valve 44 and forcing the first control valve 44 to change its working position and disconnect the clean water pipeline 42.

[0091] When the metering pump 21 stops working, the first control valve 44 returns to its normally open initial position under the action of its internal reset component, thereby connecting the water pipeline 42; the water pump 43 works to input the water in the water bottle 41 into the first liquid section 231, thereby rinsing (partially) the first liquid section 231, the metering pump 21 and the second liquid section 232, and then inputting the reagents remaining in the first liquid section 231, the metering pump 21 and the second liquid section 232 into the collection bottle 4 or the reaction vessel 1 through the water.

[0092] The control host (its internal controller) is connected to the clean water pump 43 and can control the start time, working time and clean water dosage of the clean water pump 43 and the flushing pipeline.

[0093] More preferably, it may also include a one-outlet-multiple-inlet reversing valve 30 (or a one-inlet-multiple-outlet reversing valve). Multiple inlet ports of the one-outlet-multiple-inlet reversing valve 30 are connected to multiple liquid storage bottles 7 via different inlet branches. The output port of the one-outlet-multiple-inlet reversing valve 30 is connected to the input end of the infusion line 23, allowing the infusion line 23 to be selectively connected to one of the liquid storage bottles 7, thereby realizing the delivery of different reagents. The one-outlet-multiple-inlet reversing valve 30 is prior art and will not be described in detail here.

[0094] This application can automatically and quickly start the clean water pump 43 and connect the clean water pipeline 42 after the metering pump 21 stops working, to flush part of the first liquid section 231, the metering pump 21 and the second liquid section 232, flushing the residual reagent into the collection bottle 4 or the reaction vessel 1, thereby ensuring the accuracy of the input reagent dosage. At the same time, the above cleaning work can prepare for the subsequent pumping of other reagents, avoiding mutual interference and influence between different reagents, and also ensuring the accuracy of the reagent input dosage.

[0095] Example 3

[0096] This embodiment discloses a solid sample detection device that is essentially the same as that in Embodiment 2, except that:

[0097] Reference Figure 6 As shown, this embodiment further includes: a gas pipeline 51;

[0098] One end of the gas pipeline 51 is connected to a dry gas source (nitrogen tank, inert gas tank, or one end of the gas pipeline 51 is open and directly connected to the atmosphere), and the other end of the gas pipeline 51 is connected to the first liquid section 231.

[0099] An air pump 52, a second control valve 53 and a third check valve 54 are sequentially installed on the gas pipeline 51.

[0100] The third one-way valve 54 is used to limit the one-way flow of drying gas from the drying gas source to the first liquid section 231;

[0101] The second control valve 53 is a normally open two-position three-way valve (i.e., in the absence of external control pressure, the second control valve 53 remains in a connected state under the action of a spring or other reset element within its valve body, thereby keeping the gas pipeline 51 connected). The control port of the second control valve 53 is connected to the second liquid section 232 through the second control pipeline 56. When the metering pump 21 is working, some of the reagent in the second liquid section 232 enters the control port of the second control valve 53 through the second control pipeline 56, overcoming the reset force of the reset element inside the second control valve 53 and forcing the second control valve 53 to change its working position and disconnect the gas pipeline 51.

[0102] When the metering pump 21 stops working, the second control valve 53 returns to its normally open initial position under the action of its internal reset component, thereby connecting the gas pipeline 51; the air pump 52 works to pump dry gas into the first liquid section 231, thereby drying (partially) the second liquid section 232, the metering pump 21, and the second liquid section 232; that is, removing residual liquid in the first liquid section 231, the metering pump 21, and the second liquid section 232.

[0103] When the metering pump 21 is working, the pressure in the second liquid path section 232 is defined as the reagent pressure P0, the set pressure of the control port of the first control valve 44 (i.e., the threshold pressure that forces the first control valve 44 to change its state) is the first threshold pressure P1; the set pressure of the control port of the second control valve 53 (i.e., the threshold pressure that forces the second control valve 53 to change its state) is the second threshold pressure P2; wherein the reagent pressure P0 is greater than the first threshold pressure P1 and the second threshold pressure P2, respectively, thereby realizing the control of the first control valve 44 and the second control valve 53.

[0104] When the clean water pump 43 is working, the pressure in the second liquid section 232 is defined as the clean water pressure P3. The clean water pressure P3 is less than the first threshold pressure P1 and the second threshold pressure P2, so as to avoid controlling the first control valve 44 and the second control valve 53.

[0105] Similarly, when the air pump 52 is working, the pressure in the second liquid section 232 is defined as the gas pressure P4. The gas pressure P4 is less than the first threshold pressure P1 and the second threshold pressure P2, so as to avoid controlling the first control valve 44 and the second control valve 53.

[0106] The control host (its internal controller) is connected to the air pump 52 and can control the start time and operating duration of the air pump 52.

[0107] More preferably, an air filter 55 is provided on the gas pipeline 51 for filtering the dry gas.

[0108] In this embodiment, the second liquid path section 232, the metering pump 21, and the second liquid path section 232 are dried by using a drying gas to remove residual liquid in the first liquid path section 231, the metering pump 21, and the second liquid path section 232. This can effectively avoid the interference and influence of residual liquid on the subsequent reagent pumping volume, and further improve the pumping volume and purity of the reagent.

[0109] Example 4

[0110] This embodiment is essentially the same as Embodiment 3, except that:

[0111] Reference Figure 7 and Figure 8 As shown, more preferably, the solid sample detection device disclosed in this embodiment further includes a third control valve 57 disposed on the water pipeline 42;

[0112] The third control valve 57 is a normally open two-position three-way valve (that is, in the absence of external control pressure, the third control valve 57 remains in the connected state under the action of springs and other reset components in its valve body, thereby keeping the clean water pipeline 42 in the connected state). The control port of the third control valve 57 is connected to the gas pipeline 51 through the third control pipeline 58.

[0113] When the air pump 52 is working, 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, overcoming the reset force of the internal reset component of the third control valve 57 and forcing the third control valve 57 to change its working position and disconnect the clean water pipeline 42.

[0114] When the air pump 52 stops working, the third control valve 57 returns to its normally open initial position under the action of its internal reset component, thereby connecting the clean water pipeline 42.

[0115] This ensures that the air pump 52 is working. When the (partial) second liquid section 232, metering pump 21 and the second liquid section 232 are being dried, the clean water pipeline 42 remains disconnected to avoid interfering with the drying process of the above pipelines.

[0116] More preferably, a hydraulic delay device 60 is provided on the second control line 56.

[0117] The hydraulic delay device 60 includes a main circuit 61 and a first branch circuit 62 arranged in parallel. An adjustable flow valve 64 is provided on the main circuit 61, and a fourth check valve 63 is provided on the first branch circuit 62. The fourth check valve 63 is used to limit the reagent to flow unidirectionally from the second liquid circuit section 232 to the second control valve 53.

[0118] The inlet and outlet of the main road 61 are respectively connected to the second control pipeline 56 (or the main road 61 is connected to the second control pipeline 56 as a part of the pipeline).

[0119] It also includes a pouch 65 made of elastic material, the inlet of which is connected to the outlet of the main channel 61 (the interface near the side of the second control valve 53);

[0120] When the metering pump 21 is working, some 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, thereby regulating the second control valve 53. At the same time, some reagent enters the capsule 65, causing the capsule 65 to bulge (the capsule 65 temporarily stores some reagent). When the metering pump 21 stops working, the pressure in the second liquid path section 232 disappears, and the reagent in the capsule 65 is released under the action of the capsule 65's own elastic force and flows back (slowly) to the second liquid path section 232 through the adjustable flow valve 64. The control pressure at the control port of the second control valve 53 decreases after a delay, and the second control valve 53 is opened after a delay (the delay time can be adjusted according to the limited flow rate of the adjustable flow valve 64).

[0121] The working principle of this embodiment is that when the metering pump 21 stops working, the control pressure at the control port of the first control valve 44 disappears first, the first control valve 44 opens first, the water pump 43 works, and the water pump 43 in the water bottle 41 is pumped into the first liquid section 231, thereby rinsing (partial) the first liquid section 231, the metering pump 21 and the second liquid section 232, and then the reagents remaining in the first liquid section 231, the metering pump 21 and the second liquid section 232 are pumped into the collection bottle 4 or the reaction vessel 1 through the water pump 43;

[0122] The hydraulic delay device 60 causes the control pressure at the control port of the second control valve 53 to be lower than the second threshold pressure P2 of the second control valve 53 after a set time extension, and the second control valve 53 opens after a delay; the air pump 52 operates, and 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, overcoming the reset force of the internal reset element of the third control valve 57 and forcing the third control valve 57 to change its working position and disconnect the clean water pipeline 42; that is, after rinsing (partially) the first liquid section 231, the metering pump 21 and the second liquid section 232 with clean water for a set time, the air pump 52 is turned on, and the (partially) first liquid section 231, the metering pump 21 and the second liquid section 232 are dried with dry gas.

[0123] In this embodiment, the degree of automation is high. After each reagent delivery, the delivery pipeline is automatically rinsed with clean water and dried with air, thereby avoiding interference between different reagents and ensuring the accuracy of the delivery dosage.

[0124] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A solid sample detection device, characterized in that, Including a precision injection system for precisely controlling the amount of reagent injected into a collection bottle or reaction vessel; The precision infusion system includes: infusion tubing, a first check valve, a metering pump, an infusion needle, a clean water tubing, a clean water bottle, a clean water pump, a first control valve, and a second check valve; The infusion line is connected to the storage bottle at its input end and to the injection needle at its output end. The infusion line is provided with the first one-way valve and the metering pump in sequence, which are used to pump the reagent in the storage bottle into the collection bottle or reaction vessel. The first one-way valve is used to limit the one-way flow of reagent from the storage bottle to the injection needle; The infusion line includes a first fluid passage section disposed between the first one-way valve and the metering pump, and a second fluid passage section disposed between the metering pump and the injection needle; The water bottle is used to store clean water; one end of the water pipe is connected to the water bottle, and the other end of the water pipe is connected to the first liquid path section. The clean water pipeline is sequentially equipped with the clean water pump, the first control valve, and the second check valve. The second check valve is used to limit the one-way flow of water from the water bottle to the first liquid path section; The first control valve is a normally open two-position three-way valve. The control port of the first control valve is connected to the second liquid circuit through the first control pipeline. When the metering pump is working, part of the reagent in the second liquid circuit enters the control port of the first control valve through the first control pipeline, which overcomes the reset force of the internal reset element of the first control valve and forces the first control valve to change its working position and disconnect the clean water pipeline. When the metering pump stops working, the first control valve returns to its normally open initial position under the action of its internal reset component, thereby connecting the clean water pipeline; the clean water pump operates to pump clean water from the clean water bottle into the first liquid path section, thereby flushing the first liquid path section, the metering pump, and the second liquid path section, and then pumping the residual reagents in the first liquid path section, the metering pump, and the second liquid path section into the collection bottle or reaction vessel via clean water; Including gas pipelines; One end of the gas pipeline is connected to a drying gas source, and the other end of the gas pipeline is connected to the first liquid section; an air pump, a second control valve, and a third check valve are sequentially installed on the gas pipeline; The third one-way valve is used to limit the one-way flow of drying gas from the drying gas source to the first liquid path section; The second control valve is a normally open two-position three-way valve. The control port of the second control valve is connected to the second liquid section through the second control pipeline. When the metering pump is working, part of the reagent in the second liquid section enters the control port of the second control valve through the second control pipeline, overcoming the reset force of the internal reset element of the second control valve and forcing the second control valve to change its working position and disconnect the gas pipeline. When the metering pump stops working, the second control valve returns to its normally open initial position under the action of its internal reset component, thereby connecting the gas pipeline; the air pump works to pump dry gas into the first liquid section, thereby drying the second liquid section, the metering pump and the second liquid section; that is, removing residual liquid in the first liquid section, the metering pump and the second liquid section.

2. The solid sample detection device according to claim 1, characterized in that, The control unit is connected to the clean water pump and is used to control the start-up time, working duration, and clean water dosage for flushing the pipeline.

3. The solid sample detection device according to claim 1, characterized in that, It also includes a multi-inlet reversing valve, whose multiple input ports are connected to multiple liquid storage bottles through different input branches, and whose output port is connected to the input end of the infusion line, so that the infusion line can be selectively connected to one of the liquid storage bottles, thereby realizing the delivery of different reagents.

4. The solid sample detection device according to claim 1, characterized in that, When the metering pump is working, 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 the first threshold pressure, and the set pressure of the control port of the second control valve is the second threshold pressure. The reagent pressure is greater than the first threshold pressure and the second threshold pressure, respectively, thereby realizing the control of the first control valve and the second control valve.

5. The solid sample detection device according to claim 1, characterized in that, When the clean water pump is working, the pressure in the second liquid circuit section is defined as the clean water pressure. The clean water pressure is always less than the first threshold pressure and the second threshold pressure, so as to avoid controlling the first control valve and the second control valve.

6. The solid sample detection device according to claim 1, characterized in that, When the air pump is working, the pressure in the second liquid circuit section is defined as the gas pressure. The gas pressure is less than the first threshold pressure and the second threshold pressure, so as to avoid controlling the first control valve and the second control valve.

7. The solid sample detection device according to claim 2, characterized in that, The control host is connected to the air pump and is used to control the start-up time and operating duration of the air pump.

8. The solid sample detection device according to claim 1, characterized in that, An air filter is installed on the gas pipeline to filter the dry gas.

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