CN116577172A - Urine sample pretreatment device based on coprecipitation-separation oxidation method - Google Patents

Urine sample pretreatment device based on coprecipitation-separation oxidation method Download PDF

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Publication number
CN116577172A
CN116577172A CN202310862481.6A CN202310862481A CN116577172A CN 116577172 A CN116577172 A CN 116577172A CN 202310862481 A CN202310862481 A CN 202310862481A CN 116577172 A CN116577172 A CN 116577172A
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China
Prior art keywords
urine sample
heating
urine
lifting
sample
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CN202310862481.6A
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CN116577172B (en
Inventor
黄金峰
熊文俊
钟华强
龙晖
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Guangzhou Lantaisheng Technology Co ltd
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Guangzhou Lantaisheng Technology Co ltd
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    • 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D35/00Filtering devices having features not specifically covered by groups B01D24/00 - B01D33/00, or for applications not specifically covered by groups B01D24/00 - B01D33/00; Auxiliary devices for filtration; Filter housing constructions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00Other mixers; Mixing plants; Combinations of mixers
    • B01F33/45Magnetic mixers; Mixers with magnetically driven stirrers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/90Heating or cooling systems
    • B01F35/92Heating or cooling systems for heating the outside of the receptacle, e.g. heated jackets or burners
    • 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/90Heating or cooling systems
    • B01F2035/99Heating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F2101/00Mixing characterised by the nature of the mixed materials or by the application field
    • B01F2101/23Mixing of laboratory samples e.g. in preparation of analysing or testing properties of materials
    • 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

Abstract

The application belongs to the technical field of urine radioactive substance separation, and discloses a urine sample pretreatment device based on a coprecipitation-separation oxidation method, which comprises the following components: a holding mechanism provided with a plurality of holding units for holding urine samples; the liquid transferring mechanism is used for transferring the urine sample in the containing unit; the filtering mechanism is used for receiving the urine sample transferred by the pipetting mechanism and filtering out sediment from the urine sample; the shifting mechanism is connected with the filtering mechanism and is used for driving the filtering mechanism to move to a sample receiving position and a sample heating position; a heating mechanism for heating the precipitate; the sample adding mechanism is used for adding corresponding doses of reaction solution to the precipitate; compared with the prior art, the processing device does not need to be manually participated in the urine sample processing process, and the efficiency and the safety of the existing method for acquiring the plutonium content in urine are improved.

Description

Urine sample pretreatment device based on coprecipitation-separation oxidation method
Technical Field
The application belongs to the technical field of urine radioactive substance separation, and particularly relates to a urine sample pretreatment device based on a coprecipitation-separation oxidation method.
Background
According to the nuclear industry department standard EJ/T274-1987, analysis method of plutonium in urine, the method for measuring the content of plutonium in urine comprises separating and purifying the plutonium in urine, preparing a source by electrodeposition, measuring by an alpha energy spectrometer and measuring by an alpha counter; most of the components in urine are water, urea, uric acid and inorganic salts, and the content of the radioactive substance plutonium is very small, so that sample concentration and substance separation are needed for pretreatment of urine samples.
In the pretreatment flow of urine sample of the standard EJ/T274-1987 of the Ministry of nuclear industry, comprising the steps of centrifuging the urine sample, removing supernatant and obtaining Pu (IV), the existing method mainly comprises the steps of adding 20mL of concentrated nitric acid and 10mL of 30% hydrogen peroxide to precipitate by staff to destroy organic substances, placing the reacted solvent on a heating plate, and heating to obtain white residues; dissolving the residue with 20ml of 7.5mol/L nitric acid, adding 1mol/L sodium nitrite to oxidize plutonium into Pu (IV), and heating on an electric heating plate to remove sodium nitrite; this approach is not suitable for batch processing of urine samples, concentrated nitric acid is a highly toxic corrosive substance, and can splash during titration to harm the health of staff.
Therefore, the conventional method for obtaining the plutonium content in urine has problems of low obtaining efficiency and low safety.
Disclosure of Invention
The application provides a urine sample pretreatment device based on a coprecipitation-separation oxidation method, which is used for improving the efficiency and the safety of the existing method for acquiring the plutonium content in urine.
The first technical scheme adopted by the application is as follows:
a urine sample pretreatment device based on a coprecipitation-separation oxidation method, comprising:
a holding mechanism provided with a plurality of holding units for holding urine samples;
a pipetting mechanism for transferring urine samples in the holding unit;
a filtering mechanism for receiving the urine sample transferred by the pipetting mechanism and filtering out sediment from the urine sample;
the filter mechanism is connected with the shifting mechanism and is used for driving the filter mechanism to move to a sample receiving position and a sample heating position;
the heating mechanism is used for heating the sediment when the shifting mechanism drives the filtering mechanism to move to a sample heating position;
and the sample adding mechanism is used for adding corresponding doses of reaction solution to the sediment when the sediment is heated by the heating mechanism.
Through the technical scheme, the containing mechanism is provided with the plurality of containing units, and compared with the manual treatment of urine samples, a large quantity of urine samples can be contained, so that the urine samples are kept still for precipitation; after a large amount of urine samples are settled, transferring the urine samples to a filtering mechanism by a liquid transferring mechanism for filtering so as to filter supernatant liquid of the urine samples and keep sediment; the shifting mechanism can drive the filtering mechanism to move to a sample receiving position so as to receive and filter urine samples, and can also drive the filtering mechanism to move to a sample heating position so that the filtering mechanism carries sediment to be placed on the heating mechanism for heating; in the process of heating the sediment by the heating mechanism, adding a corresponding dose of reaction solution into the sediment by the sampling mechanism to extract Pu (IV); compared with the prior art, the processing device does not need to be manually participated in the urine sample processing process, achieves the effect of automatically processing urine samples in a large scale, and improves the efficiency and the safety of the existing plutonium content acquisition mode in urine.
The application is further provided with: the device also comprises a plurality of heating and stirring units, wherein the heating and stirring units are arranged at intervals; the heating stirring unit comprises an annular heater and a magnetic stirrer, the inner ring of the annular heater is attached to the outer wall of the holding unit, the magnetic stirrer is arranged at the bottom of the annular heater, and the bottom of the holding unit is abutted to the magnetic stirrer.
Through the technical scheme, the heating and stirring unit heats the urine sample in the holding unit through the annular heater to accelerate the acidification of the urine so as to meet the experimental requirements; when the pH value of the urine sample does not reach the preset standard, the urine sample is required to be subjected to neutralization titration, the magnetic stirrer is used for supporting the containing unit, and the urine sample and the neutralization titration solution are magnetically stirred so as to enable the urine sample and the neutralization titration solution to fully react.
The application is further provided with: the urine sampling device further comprises a waste liquid tank, wherein the bottom of the waste liquid tank is communicated with a negative pressure pipeline, so that when the shifting mechanism drives the filtering mechanism to a sample receiving position, the filtering mechanism extracts waste liquid filtered out of the urine sample.
Through above-mentioned technical scheme, when the shifter drives filtering mechanism and moves to the sample and receive the position, the liquid transferring mechanism shifts the urine sample to filtering mechanism, and in the waste liquid inflow waste liquid groove of filtering by filtering mechanism to take out waste liquid from the waste liquid inslot by negative pressure pipeline, with the possibility that reduces the too high influence filter effect of waste liquid water level.
The application is further provided with: the pipetting mechanism comprises a first lifting frame, a first lifting slide rail, a first lifting driving piece and a plurality of peristaltic pumps, wherein the first lifting frame is connected with the first lifting slide rail in a sliding manner, and the first lifting driving piece is arranged at the end part of the first lifting slide rail so as to drive the first lifting frame seat to move in a lifting manner; the liquid suction end of the peristaltic pump is communicated with a liquid suction long rod, the liquid suction long rod is fixedly connected to the first lifting frame, and a liquid suction head of the liquid suction long rod is opposite to the opening of the containing unit; the first lifting frame is provided with an acid-base meter, and the measuring end of the acid-base meter is opposite to the opening of the containing unit; the first crane is far away from one side of holding the unit fixedly connected with second crane, the play liquid end intercommunication of peristaltic pump has out the liquid stock, go out liquid stock fixedly connected with second crane, go out the liquid head orientation of liquid stock the waste liquid groove.
Through the technical scheme, the first lifting frame is used for driving the liquid suction long rod to do lifting motion along the first lifting sliding rail, so that the washing liquid head of the liquid suction long rod can penetrate into the containing unit and absorb urine samples in the containing unit; the first lifting driving piece is used for driving the first lifting frame to do lifting movement; the peristaltic pumps are used for providing negative pressure for the liquid suction long rod and positive pressure for the liquid suction long rod, so that urine samples in the containing unit can be sucked by the liquid suction long rod and pumped out by the liquid discharge long rod; the second lifting frame is fixedly connected to one side, far away from the containing unit, of the first lifting frame and can move up and down along with the first lifting frame; compared with the prior art, the acid-base meter is further arranged on the first lifting frame, the measuring end of the acid-base meter is opposite to the opening of the containing unit, and the PH value of the urine sample in the containing unit can be measured, so that a worker can conveniently neutralize and titrate the urine sample according to the PH value of the urine sample, and generation of precipitation is accelerated.
The application is further provided with: the filter mechanism comprises a filter cup bracket and a plurality of filter cups, wherein the filter cup bracket is provided with a plurality of cup placing holes which are arranged at intervals, and the filter cups are placed on the filter cup bracket through the cup placing holes; filter paper is arranged in the filter cup; an electric switch piece is arranged at the outlet end of the filter cup; the shifting mechanism comprises a horizontal sliding rail and a second lifting sliding rail, the second lifting sliding rail is connected with the horizontal sliding rail in a sliding manner, and the horizontal sliding rail is provided with a horizontal driving piece so as to drive the second lifting sliding rail to move horizontally; the filter bowl support is connected to the second lifting slide rail in a sliding mode, and a second lifting driving piece is arranged on the second lifting slide rail to drive the filter bowl support to move in a lifting mode.
Through the technical scheme, the filter mechanism consists of the filter cup bracket and a plurality of filter cups, and the filter cups are placed on the filter cup bracket through the cup placing holes, so that the filter cup bracket can drive the filter cups to move; the filter paper is arranged in the filter cup, so that when the sampling mechanism adds a corresponding dose of reaction solution to the sediment, the sediment is dissolved, and Pu (IV) falls into the heating mechanism; the outlet end of the filter cup is provided with an electric switch piece, when the electric switch piece is closed, the outlet of the filter cup is sealed, so that the sediment is soaked in the reaction solution for full reaction; the shifting mechanism consists of a horizontal sliding rail and a second lifting sliding rail, the second lifting sliding rail is connected with the horizontal sliding rail in a sliding way, and the filter cup support is connected with the second lifting sliding rail in a sliding way, so that the filter cup support can do horizontal movement and lifting movement; the horizontal driving piece is used for driving the second lifting frame to horizontally move along the horizontal sliding rail direction; the second lifting driving piece is used for driving the filter cup bracket to do lifting motion along the second lifting sliding rail; compared with the prior art, the shifting mechanism can drive the filtering mechanism to do lifting and horizontal movement so as to be beneficial to adjusting the sample receiving position and the sample heating position of the filtering mechanism.
The application is further provided with: the heating mechanism comprises a heating groove, a plurality of collecting units are arranged in the heating groove, and the collecting units are arranged at intervals corresponding to the filter cups.
According to the technical scheme, when the filter cup bracket drives the filter cups to move to the sample heating position, the heating groove can heat the sediment in each filter cup; when a corresponding dose of reaction solution is added to the precipitate in the sampling mechanism, the precipitate is dissolved, so that Pu (IV) falls into the collecting unit; the plurality of collecting units which are arranged at intervals are arranged, so that the batch collection of the sediment is facilitated.
The application is further provided with: the sample adding mechanism comprises a plurality of sample adding rods and a plurality of injection pumps internally provided with reaction solutions, the injection pumps are communicated with the sample adding rods, the sample adding rods are fixedly connected to the second lifting frames, and the liquid outlets of the sample adding rods face to the openings of the collecting units.
Through the technical scheme, the injection pump is communicated with the sample adding rod, and is internally provided with a reaction solution for pumping the corresponding reaction solution into the sample adding rod; the sample adding rod is fixedly connected to the second lifting frame, and the liquid outlet of the sample adding rod faces the opening of the collecting unit so as to add the reaction solution to the filter cup when the filter mechanism moves to the sample heating position.
The second object of the application is realized by the following technical scheme:
the urine sample pretreatment method based on the coprecipitation-separation oxidation method is applied to the urine sample pretreatment device based on the coprecipitation-separation oxidation method, and comprises the following steps:
based on the urine sample reserves and the heating sedimentation time, a pipetting signal is sent to the pipetting mechanism;
transmitting a sample receiving signal to the displacement mechanism based on the pipetting signal;
after the sample receiving signal is sent, a sediment shifting signal is sent to the shifting mechanism;
transmitting a warming signal to the heating mechanism based on the sedimentation displacement signal;
and after the heating mechanism is heated to a preset temperature, sending a solution throwing signal to the sampling mechanism.
According to the technical scheme, according to the urine sample reserves and the heating sedimentation time of the containing units, a pipetting signal is sent to the pipetting mechanism, so that the hydraulic mechanism starts to transfer the urine samples in the containing units, meanwhile, according to the pipetting signal, a sample receiving signal is sent to the pipetting mechanism, and the filtering mechanism moves to a sample receiving position to filter the urine samples transferred by the pipetting mechanism; after the filtering mechanism filters the urine sample, a sediment displacement signal is sent to the displacement unit, so that the displacement unit drives the filtering mechanism to move to the heating mechanism; after the filtering mechanism moves to the heating mechanism, the heating mechanism is heated to a preset temperature so as to adjust the reaction temperature of the precipitate, and finally, a solution throwing signal is sent to the sampling mechanism so that the precipitate reacts with the reaction solution at the preset temperature, thereby realizing the effect of automatically extracting Pu (IV) in the urine sample.
The application is further provided with: before sending a pipetting signal to the pipetting mechanism based on the urine sample reserves and the heated sedimentation time, the method further comprises:
acquiring the PH value of the urine sample;
generating a plurality of neutralization formulation combinations based on the PH;
acquiring combination selection information based on the neutralization formula combination;
based on the combination selection information, dose formulation information is issued.
Through the technical scheme, the pH value of the urine sample is regulated before the urine sample is pipetted; the pH value of the urine sample is obtained through the acid-base meter, and then a plurality of neutralization cooperation combinations are automatically generated according to the pH value so as to be selected by a worker, after the worker selects the corresponding neutralization formula combination, combination selection information is obtained, and dosage configuration information is sent to the corresponding executing mechanism or the worker is prompted to prepare the neutralization titration solution by himself, so that the efficiency of preparing the neutralization titration solution by the worker is improved.
The application is further provided with: based on the urine sample reserve and the heated settling time, sending a pipetting signal to the pipetting mechanism comprises:
and if the urine sample storage amount is higher than the storage threshold or the heating sedimentation time exceeds the preset time, sending a pipetting signal to the pipetting mechanism.
According to the technical scheme, when the urine sample storage amount is higher than the storage amount threshold value, a pipetting signal is sent to the pipetting mechanism, so that the possibility that the urine sample is excessively placed and flows out of the containing unit to pollute a working site is reduced; when the heating sedimentation time exceeds the preset time, a pipetting signal is sent to the pipetting mechanism, sediment in the holding unit is transferred in time, and the possibility of blocking the pipetting long rod due to excessive sediment accumulation is reduced.
The third object of the application is realized by the following technical scheme:
a computer device comprising a memory, a processor and a computer program stored in the memory and executable on the processor, the processor executing the computer program being a urine sample pretreatment device implementing the co-precipitation-separation oxidation method described above.
The fourth object of the application is realized by the following technical scheme:
a computer readable storage medium storing a computer program which when executed by a processor implements the urine sample pretreatment device based on the coprecipitation-separation oxidation method described above.
In summary, the present application includes at least one of the following beneficial technical effects:
1. compared with the prior art, the processing device does not need to be manually participated in the urine sample processing process, achieves the effect of automatically processing urine samples in a large scale, and improves the efficiency and the safety of the existing plutonium content acquisition mode in urine.
2. Compared with the prior art, when the shifting mechanism drives the filtering mechanism to move to the sample receiving position, the liquid transferring mechanism transfers the urine sample to the filtering mechanism, waste liquid flowing through the filtering mechanism flows into the waste liquid tank, and the waste liquid is pumped out of the waste liquid tank through the negative pressure pipeline, so that the possibility that the filtering effect is influenced by the excessive water level of the waste liquid is reduced.
3. Compared with the prior art, when the filter cup bracket drives the filter cups to move to the sample heating position, the heating groove can heat the sediment in each filter cup; when a corresponding dose of reaction solution is added to the precipitate in the sampling mechanism, the precipitate is dissolved, so that Pu (IV) falls into the collecting unit; the plurality of collecting units which are arranged at intervals are arranged, so that the batch collection of the sediment is facilitated.
Drawings
FIG. 1 is a schematic diagram showing a structure of a urine sample pretreatment apparatus based on a coprecipitation-separation oxidation method according to an embodiment of the present application;
FIG. 2 is a front view of a urine sample pretreatment apparatus based on a coprecipitation-separation oxidation method according to an embodiment of the present application;
FIG. 3 is a cross-sectional view of a filtration mechanism and waste tank in accordance with a first embodiment of the present application;
FIG. 4 is a flow chart of a urine sample pretreatment method based on a coprecipitation-separation oxidation method in accordance with an embodiment of the application;
fig. 5 is a schematic diagram of a computer device in a third embodiment of the application.
Reference numerals illustrate:
100. a frame; 1. a holding mechanism; 2. a pipetting mechanism; 21. a first lifting frame; 22. a first lifting slide rail; 23. a first lifting driving member; 24. a peristaltic pump; 25. a liquid suction long rod; 26. acid and alkali meter; 27. a second lifting frame; 28. a liquid outlet long rod; 3. a filtering mechanism; 31. a filter bowl support; 32. a filter cup; 321. a filter paper; 322. an electric switch member; 4. a displacement mechanism; 41. a horizontal slide rail; 42. the second lifting slide rail; 421. a second lifting driving member; 5. a heating mechanism; 51. a heating tank; 52. a collection unit; 6. a sample adding mechanism; 61. a sample adding rod; 62. a syringe pump; 7. a heating and stirring unit; 71. an annular heater; 72. a magnetic stirrer; 8. a waste liquid tank; 81. negative pressure pipeline.
Detailed Description
The technical solutions of the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present application, and it is apparent that the described embodiments are some embodiments of the present application, but not all embodiments, and all other embodiments obtained by those skilled in the art without making creative efforts based on the embodiments of the present application are included in the protection scope of the present application.
The embodiment of the application provides a urine sample pretreatment device based on a coprecipitation-separation oxidation method, which is used for improving the efficiency and safety of the existing method for acquiring the plutonium content in urine.
Example 1
As shown in fig. 1 and 2, the urine sample pretreatment device based on the coprecipitation-separation oxidation method according to the embodiment of the present application includes a frame 100, a holding mechanism 1, a pipetting mechanism 2, a filtering mechanism 3, a shifting mechanism 4, a heating mechanism 5 and a sampling mechanism 6, the frame 100 being used for supporting and fixing the respective mechanisms of the device according to the present application; the holding mechanism 1 is provided with a plurality of holding units, in the embodiment, the holding units are 2L beakers, and the number of the holding units is 8, so that a large amount of urine samples can be contained, and the urine samples are allowed to stand and sediment; the pipetting mechanism 2 is used for transferring the urine sample in the holding unit to the filtering mechanism 3 for filtering, the filtering mechanism 3 filters out supernatant of the urine sample, and sediment is reserved; the filtering mechanism 3 is connected with the shifting mechanism 4, and the shifting mechanism 4 is used for driving the filtering mechanism 3 to move to a sample receiving position so as to receive and filter the urine sample; the shifting mechanism 4 can also drive the filtering mechanism 3 to move to a sample heating position, so that the filtering mechanism 3 carries sediment to be placed on the heating mechanism 5 for heating; when the precipitate is placed on the heating mechanism 5 for heating, the sampling mechanism 6 adds a corresponding dose of reaction solution to the precipitate, thereby extracting Pu (IV); compared with the prior art, the processing device does not need to be manually participated in the process of transferring, filtering, heating and reacting the urine sample, achieves the effect of automatically processing the urine sample in a large scale, and improves the efficiency and the safety of the existing method for acquiring the plutonium content in the urine.
Referring to fig. 1 and 2, the device of the present application further comprises 8 heating and stirring units 7, and the 8 heating and stirring units 7 are arranged at intervals; the heating and stirring unit 7 comprises an annular heater 71 and a magnetic stirrer 72, and the inner ring of the annular heater 71 is attached to the outer wall of the holding unit so as to uniformly heat the urine sample in the holding unit, thereby accelerating the acidification of the urine and meeting the experimental requirements; the magnetic stirrer 72 is fixedly connected to the bottom of the annular heater 71 and is used for bearing the holding unit and magnetically stirring the urine sample in the holding unit, when the urine sample needs to be subjected to neutralization titration to adjust the pH value, the magnetic stirrer 72 works and stirs the urine sample in the holding unit and the solvent for neutralization titration so as to accelerate neutralization of acid and alkali and generate precipitate.
In this embodiment, according to the experimental requirements, the urine sample placed in the holding unit needs to be subjected to sample concentration: adding a proper amount of standard liquid 242Pu into a urine sample which is kept stand for 24 hours, adding 10mL of concentrated nitric acid and 5mL of 30% hydrogen peroxide, heating to 100 ℃ by an annular heater 71, and boiling for 20 minutes to accelerate acidification of the urine sample; the ring heater 71 is cooled down, when the temperature is cooled down to about 80 ℃, 2mL of phosphoric acid is added to the urine sample in a constant-temperature water bath, ammonia water is added under magnetic stirring at the rotating speed of 1000-1500 rpm, and the pH of the urine sample is adjusted to 8-9, and then stirring is continued for 20min, so that the precipitation of plutonium in the urine sample and other cations is accelerated.
Referring to fig. 1 and 3, the filter mechanism 3 includes a filter bowl support 31 and a plurality of filter bowls 32, and in this embodiment, the filter bowl 32 is funnel-shaped to facilitate filtering of urine samples; the filter cup bracket 31 is provided with a plurality of cup placing holes which are arranged at intervals, and the filter cup 32 is placed on the filter cup bracket 31 through the cup placing holes, so that the filter cup 32 can be replaced at any time; filter paper 321 is arranged in filter cup 32, so that when sampling mechanism 6 adds corresponding dosage of reaction solution to the sediment, the sediment is dissolved, filter paper 321 filters impurities, and Pu (IV) falls into heating mechanism 5; the bottom of the filter cup 32 is provided with an electric switch piece 322, and when the electric switch piece 322 is closed, a dissolving mode of the precipitate adopts a soaking mode, so that the dissolved matters can fully react with the reaction solution; when the electric switch piece 322 is opened, pu (IV) generated after the reaction flows into the heating mechanism 5 along the outlet end of the filter bowl; in this embodiment, the precipitate dissolving mode adopts a soaking mode, so as to ensure that the precipitate is soaked and dissolved, the electric switch piece 322 can be set as an existing electric plug or an electric flashboard switch, and after the precipitate is fully soaked and dissolved, the bottom opening of the filter cup is opened, so that Pu (IV) falls into the heating mechanism 5.
Referring to fig. 1 and 3, the apparatus of the present application further includes a negative pressure pipe 81 connected to the bottom of the waste liquid tank 8, and when the filter bowl 32 is positioned at the top of the waste liquid tank 8 to perform the first filtration, the supernatant of the urine sample flows into the waste liquid tank 8 and the waste liquid is pumped out by the negative pressure pipe 81, thereby reducing the possibility that the frame 100 is polluted by the excessive waste liquid level and affecting the filtering effect.
Referring to fig. 1 and 2, the pipetting mechanism 2 includes a first lifting frame 21, a first lifting slide rail 22, a first lifting driving member 23 and a plurality of peristaltic pumps 24, wherein the first lifting frame 21 is slidably connected to the first lifting slide rail 22, so that the first lifting frame 21 can perform lifting movement along the direction of the first lifting slide rail 22; the first lifting driving piece 23 is arranged at the end part of the first lifting slide rail 22, in this embodiment, the first lifting driving piece 23 is a servo motor, and is controlled based on a PID control algorithm, and the first lifting driving piece 23 drives the first lifting frame 21 to automatically perform lifting motion along the direction of the first lifting slide rail 22 through the existing transmission mechanism (belt, screw rod, etc.); the peristaltic pump 24 is arranged at the top of the rack 100, the liquid suction end of the peristaltic pump 24 is communicated with the liquid suction long rod 25, the liquid suction long rod 25 is fixedly connected to the first lifting frame 21, the liquid suction head of the liquid suction long rod 25 is opposite to the opening of the containing unit, when the liquid suction mechanism 2 needs to transfer urine samples, the first lifting frame 21 descends to enable the liquid suction long rod 25 to extend into the containing unit, and the peristaltic pump 24 provides negative pressure for the liquid suction long rod 25 so as to absorb the urine samples in the containing unit; the first lifting frame 21 is also provided with an acid-base meter 26, the measuring end of the acid-base meter 26 is opposite to the opening of the containing unit, and the acid-base meter 26 moves up and down along with the first lifting frame 21 so as to measure the PH value of the urine sample, thereby facilitating the neutralization titration of the urine sample by staff according to the PH value of the urine sample and accelerating the generation of sediment; the second lifting frame 27 is fixedly connected to one side, far away from the containing unit, of the first lifting frame 21, a liquid outlet long rod 28 is communicated with a liquid outlet end of the peristaltic pump 24, the liquid outlet long rod 28 is fixedly connected to the second lifting frame 27, a liquid outlet head of the liquid outlet long rod 28 faces the waste liquid tank 8, urine samples sucked by the liquid suction long rod 25 flow out of the liquid outlet long rod 28 through the peristaltic pump 24 and are supplied to the filter cup 32 for filtration.
Referring to fig. 1 and 2, the displacement mechanism 4 includes a horizontal slide rail 41 and a second lifting slide rail 42, the second lifting slide rail 42 is slidably connected to the horizontal slide rail 41, the horizontal slide rail 41 is provided with a horizontal driving member, in this embodiment, the horizontal driving member is a servo motor, and is controlled based on a PID algorithm, and the horizontal driving member drives the second lifting slide rail 42 to horizontally move along the direction of the horizontal slide rail 41 through an existing transmission mechanism; the filter bowl support 31 is slidably connected to the second lifting slide rail 42, and the second lifting slide rail 42 is provided with a second lifting driving member 421, in this embodiment, the second lifting driving member 421 is a servo motor, and is controlled based on a PID algorithm, and the second lifting driving member 421 drives the filter bowl support 31 to move up and down through an existing transmission mechanism; compared with the prior art, the shifting mechanism 4 can drive the filtering mechanism 3 to do lifting and horizontal movement, so that the sample receiving position and the sample heating position of the filtering mechanism 3 can be adjusted conveniently.
Referring to fig. 1 and 2, the heating mechanism 5 includes a heating tank 51 and 8 collection units 52, in this embodiment, the collection units 52 are 100ml beakers, the collection units 52 are arranged at intervals corresponding to the plurality of filter cups 32, when the filter cups 32 are placed at the sample heating position, the heating tank 51 heats the sediment in each filter cup 32, and the collection units 52 are used for collecting Pu (IV) generated after the sediment reacts with the reaction solution; the sampling mechanism 6 comprises 8 sampling rods 61 corresponding to the positions of the collecting units 52 and 8 injection pumps 62, each injection pump 62 is internally provided with a corresponding sampling rod 61 which is easy to react and is communicated with, and the injection pumps 62 are used for pumping corresponding reaction solutions into the sampling rods 61; the loading rod 61 is fixedly connected to the second lifting frame 27, and the liquid outlet of the loading rod 61 faces the opening of the collecting unit 52, so that the loading rod 61 can inject the reaction solution toward the filter cup 32 when the filter mechanism 3 moves to the sample heating position, and the collecting unit 52 obtains Pu (IV).
Example two
As shown in fig. 4, the embodiment of the application discloses a urine sample pretreatment method based on a coprecipitation-separation oxidation method, which is applied to the urine sample pretreatment device based on the coprecipitation-separation oxidation method, and comprises the following steps:
s10: based on the urine sample reserves and the heat sedimentation time, a pipetting signal is sent to the pipetting mechanism 2.
In this embodiment, the upper limit of urine sample reserves per holding unit is 2L; the upper limit of the heating sedimentation time in the urine sample of the holding unit is set according to the actual situation; the bottom of each heating and stirring unit is provided with a pressure sensor to measure urine sample reserves.
Specifically, according to the urine sample reserves and the heating sedimentation time of the heating stirring unit, a pipetting signal is sent to the pipetting mechanism 2, so that the hydraulic mechanism starts to transfer the urine samples in the holding units.
Wherein, step S10 includes: and if the urine sample storage amount is higher than the storage amount threshold value or the heating sedimentation time exceeds the preset time, a pipetting signal is sent to the pipetting mechanism 2.
In this embodiment, the reserve threshold of each heating and stirring unit is lower than 2L.
Specifically, when the urine sample storage amount is higher than the storage amount threshold value, a pipetting signal is sent to the pipetting mechanism 2 to reduce the possibility that the urine sample is excessively added and flows out of the containing unit to pollute the rack 100; when the heating sedimentation time exceeds the preset time, a pipetting signal is sent to the pipetting mechanism 2, and the sediment in the holding unit is transferred in time, so that the possibility of blocking the pipetting long rod 25 due to excessive sediment accumulation is reduced.
Wherein, before step S10, the processing method of the present application further includes:
acquiring the PH value of the urine sample;
generating a plurality of neutralization formulation combinations based on the PH;
acquiring combination selection information based on the neutralization formula combination;
based on the combination selection information, dose formulation information is issued.
In this example, the pH of the urine sample is measured by the pH meter 26; the pH value of the urine sample in each containing unit may be different; the PH value of each urine sample is an imbedded position mark so as to facilitate staff to distinguish which urine sample in the containing unit does not reach the standard and needs to be subjected to acid-base neutralization; the neutralization formula combination is an acidic reagent or alkaline reagent combination indicating the production of the pH of a urine sample; the combination selection information refers to combination selection information determined by a worker; the dose configuration information is the corresponding combination selection information, and the dose information of the acidic reagent or the alkaline reagent combination to be configured is the dose information.
Specifically, the PH value of the urine sample in each holding unit is adjusted before pipetting the urine sample; the PH value of the urine sample is obtained by the acid-base meter 26, and then a plurality of neutralization cooperation combinations are automatically generated according to the PH value for the selection of the staff, after the staff selects the corresponding neutralization formula combination, combination selection information is obtained, and dosage configuration information is sent to the corresponding executing mechanism or displayed on a preset display screen for the staff to refer to and prepare by himself, so that the efficiency of preparing neutralization titration solution by the staff is improved.
S20: based on the pipetting signal, a sample receiving signal is sent to the displacement mechanism 4.
In this embodiment, the pipetting signal and the sample receiving signal are transmitted at the same time.
Specifically, when the pipetting signal is sent out, the sample receiving signal is sent to the shifting mechanism 4 at the same time, so that the filtering mechanism 3 moves to the sample receiving position in time, the urine sample transferred by the pipetting mechanism 2 is filtered, and the possibility of urine sample permeation caused by the fact that the filtering mechanism 3 does not receive the urine sample in time is reduced.
S30: after the sample receiving signal is sent, a sediment displacement signal is sent to the displacement mechanism 4.
In this embodiment, the filtering mechanism 3 takes a certain time to filter the urine sample, at which time the displacement mechanism 4 remains stationary; after a predetermined time from the transmission of the sample receiving signal, a sediment displacement signal is transmitted to the displacement mechanism 4.
Specifically, after the filtering mechanism 3 filters the urine sample, a sediment displacement signal is sent to the displacement unit, so that the displacement unit drives the filtering mechanism 3 to move to the heating mechanism 5 for heating.
S40: based on the sedimentation displacement signal, a warming signal is sent to the heating mechanism 5.
Specifically, after the filtering mechanism 3 moves to the heating mechanism 5, the heating mechanism 5 is heated to a preset temperature to adjust the reaction temperature of the precipitate.
S50: the mechanism to be heated 5 is heated to a preset temperature, and a solution throwing signal is sent to the sampling mechanism 6.
In this embodiment, the preset temperature is a suitable temperature for the reaction between the precipitate and the reaction solution, and the optimal preset temperature needs to be obtained through verification.
Specifically, a solution feeding signal is sent to the sample feeding mechanism 6, so that the sample feeding mechanism 6 feeds 20mL of concentrated nitric acid and 10mL of hydrogen peroxide with concentration of 30% to each filter bowl 32 to destroy organic substances, the organic substances are placed in the heating tank 51, the heating tank 51 heats the precipitate until white residues are generated, the sample feeding mechanism 6 feeds 20mL of 7.5mol/L nitric acid dissolution residues to the white residues, 1mol/L of hydroxylamine hydrochloride completely reduces the high-valence Pu to be trivalent, after 5min of reduction, 1mol/L of sodium nitrite is added to completely oxidize plutonium to Pu (IV), so that the generated Pu (IV) falls into the collecting unit 52, and the effect of automatically extracting Pu (IV) in urine samples is realized; after the concentrated nitric acid has fully volatilized, the tester then tests each of the collection units 52.
Example III
As shown in fig. 5, in the present embodiment, a computer device includes an internal memory, a network interface, a nonvolatile storage medium, a processor and a system bus, the nonvolatile storage medium includes an operating system, a computer program and a database, and the processor implements the following steps when executing the computer program:
based on the urine sample reserves and the heating sedimentation time, a pipetting signal is sent to the pipetting mechanism 2;
based on the pipetting signal, sending a sample receiving signal to the displacement mechanism 4;
after the sample receiving signal is sent, a sediment shifting signal is sent to the shifting mechanism 4;
based on the sedimentation displacement signal, sending a warming signal to the heating mechanism 5;
the mechanism to be heated 5 is heated to a preset temperature, and a solution throwing signal is sent to the sampling mechanism 6.
In this embodiment, there is provided a computer-readable storage medium storing a computer program which when executed performs the steps of:
based on the urine sample reserves and the heating sedimentation time, a pipetting signal is sent to the pipetting mechanism 2;
based on the pipetting signal, sending a sample receiving signal to the displacement mechanism 4;
after the sample receiving signal is sent, a sediment shifting signal is sent to the shifting mechanism 4;
based on the sedimentation displacement signal, sending a warming signal to the heating mechanism 5;
the mechanism to be heated 5 is heated to a preset temperature, and a solution throwing signal is sent to the sampling mechanism 6.
Those skilled in the art will appreciate that implementing all or part of the above described embodiment methods may be accomplished by way of a computer program stored on a non-transitory computer readable storage medium, which when executed, may comprise the steps of each of the above described embodiments. Any reference to memory, storage, database, or other medium used in each of the embodiments provided herein may include non-volatile and/or volatile memory. The nonvolatile memory can include Read Only Memory (ROM), programmable ROM (PROM), electrically Programmable ROM (EPROM), electrically Erasable Programmable ROM (EEPROM), or flash memory. Volatile memory can include Random Access Memory (RAM) or external cache memory. By way of illustration and not limitation, RAM is available in a number of forms such as Static RAM (SRAM), dynamic RAM (DRAM), synchronous DRAM (SDRAM), double Data Rate SDRAM (DDRSDRAM), enhanced SDRAM (ESDRAM), synchronous link (Synchlink), DRAM (SLDRAM), memory bus (Rambus) direct RAM (RDRAM), direct memory bus dynamic RAM (DRDRAM), and memory bus dynamic RAM (RDRAM), among others.
It will be apparent to those skilled in the art that, for convenience and brevity of description, only the above-described division of each functional unit and module is illustrated, and in practical application, the above-described functional allocation may be performed by different functional units and modules, that is, the internal result of the apparatus is divided into different functional units or modules, so as to perform all or part of the above-described functions.
The above embodiments are only for illustrating the technical solution of the present application, and not for limiting the same; although the application has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art will understand that; the technical scheme described in each embodiment can be modified or part of the characteristics can be replaced equivalently; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of each embodiment of the present application, and are intended to be included in the scope of the present application.

Claims (10)

1. Urine sample pretreatment device based on coprecipitation-separation oxidation method, characterized by comprising:
a holding mechanism (1) provided with a plurality of holding units for holding urine samples;
a pipetting mechanism (2) for transferring urine samples in the holding unit;
a filtering mechanism (3) for receiving the urine sample transferred by the pipetting mechanism (2) and filtering out sediment from the urine sample;
the displacement mechanism (4), the said filter mechanism (3) is connected to said displacement mechanism (4), the said displacement mechanism (4) is used for driving the said filter mechanism (3) to move to sample receiving position and sample heating position;
a heating mechanism (5) for heating the sediment by the heating mechanism (5) when the shifting mechanism (4) drives the filtering mechanism (3) to move to a sample heating position;
a sampling mechanism (6) for adding a corresponding dose of the reaction solution to the precipitate when the heating mechanism (5) heats the precipitate;
the pipetting mechanism (2) comprises a first lifting frame (21), a first lifting slide rail (22), a first lifting driving piece (23) and a plurality of peristaltic pumps (24), wherein the first lifting frame (21) is connected with the first lifting slide rail (22) in a sliding manner, and the first lifting driving piece (23) is arranged at the end part of the first lifting slide rail (22) so as to drive the first lifting frame (21) to do lifting movement; the liquid suction end of the peristaltic pump (24) is communicated with a liquid suction long rod (25), the liquid suction long rod (25) is fixedly connected to the first lifting frame (21), and a liquid suction head of the liquid suction long rod (25) is opposite to the opening of the containing unit; the first lifting frame (21) is provided with an acid-base meter (26), and the measuring end of the acid-base meter (26) is opposite to the opening of the containing unit; a second lifting frame (27) is fixedly connected to one side, far away from the containing unit, of the first lifting frame (21), and a liquid outlet end of the peristaltic pump (24) is communicated with a liquid outlet long rod (28);
the shifting mechanism (4) comprises a horizontal sliding rail (41) and a second lifting sliding rail (42), the second lifting sliding rail (42) is connected with the horizontal sliding rail (41) in a sliding mode, and the horizontal sliding rail (41) is provided with a horizontal driving piece to drive the second lifting sliding rail (42) to move horizontally; the filtering mechanism (3) is connected to the second lifting slide rail (42);
the sampling mechanism (6) comprises a plurality of sampling rods (61) and a plurality of injection pumps (62) with reaction solutions inside, and the injection pumps (62) are communicated with the sampling rods (61).
2. The urine sample pretreatment apparatus based on the coprecipitation-separation oxidation method according to claim 1, further comprising a plurality of heating and stirring units (7), wherein a plurality of the heating and stirring units (7) are disposed at intervals; the heating stirring unit (7) comprises an annular heater (71) and a magnetic stirrer (72), wherein the inner ring of the annular heater (71) is attached to the outer wall of the containing unit, the magnetic stirrer (72) is arranged at the bottom of the annular heater (71), and the bottom of the containing unit is abutted to the magnetic stirrer (72).
3. The urine sample pretreatment apparatus based on the coprecipitation-separation oxidation method according to claim 1, further comprising a waste liquid tank (8), wherein a negative pressure pipeline (81) is communicated with the bottom of the waste liquid tank (8) to pump out the waste liquid filtered by the filtering mechanism (3) from the urine sample when the shifting mechanism (4) drives the filtering mechanism (3) to a sample receiving position.
4. A urine sample pretreatment apparatus based on co-precipitation-separation oxidation process according to claim 3, wherein said liquid outlet long rod (28) is fixedly connected to said second elevating frame (27), and the liquid outlet head of said liquid outlet long rod (28) is directed to said waste liquid tank (8).
5. The urine sample pretreatment apparatus based on the coprecipitation-separation oxidation method according to claim 1, wherein the filtering mechanism (3) comprises a filter bowl support (31) and a plurality of filter bowls (32), the filter bowl support (31) is provided with a plurality of cup placement holes arranged at intervals, and the filter bowl (32) is placed on the filter bowl support (31) through the cup placement holes; filter paper (321) is arranged in the filter cup (32); an electric switch piece (322) is arranged at the outlet end of the filter cup (32); the filter bowl support (31) is slidably connected to the second lifting slide rail (42), and the second lifting slide rail (42) is provided with a second lifting driving piece (421) to drive the filter bowl support (31) to move up and down.
6. The urine sample pretreatment apparatus based on the coprecipitation-separation oxidation method according to claim 5, wherein the heating mechanism (5) comprises a heating tank (51), a plurality of collecting units (52) are placed in the heating tank (51), and the plurality of collecting units (52) are arranged at intervals corresponding to the filter cups (32).
7. The urine sample pretreatment apparatus based on the coprecipitation-separation oxidation method according to claim 6, wherein the sample addition rod (61) is fixedly connected to the second lifting frame (27), and a liquid outlet of the sample addition rod (61) is directed to an opening of the collecting unit (52).
8. A urine sample pretreatment method based on a coprecipitation-separation oxidation method, which is applied to the urine sample pretreatment device based on a coprecipitation-separation oxidation method according to claim 2, and comprises:
based on urine sample reserves and heating sedimentation time, sending a pipetting signal to the pipetting mechanism (2);
transmitting a sample receiving signal to the displacement mechanism (4) based on the pipetting signal;
after the sample receiving signal is sent, a sediment shifting signal is sent to the shifting mechanism (4);
sending a warming signal to the heating mechanism (5) based on the sedimentation displacement signal;
and when the heating mechanism (5) is heated to a preset temperature, a solution throwing signal is sent to the sampling mechanism (6).
9. The urine sample pretreatment method based on the coprecipitation-separation oxidation method according to claim 8, further comprising, before a pipetting signal is issued to the pipetting mechanism (2) based on a urine sample reserve and a heated precipitation time:
acquiring the PH value of the urine sample;
generating a plurality of neutralization formulation combinations based on the PH;
acquiring combination selection information based on the neutralization formula combination;
based on the combination selection information, dose formulation information is issued.
10. The urine sample pretreatment method based on the coprecipitation-separation oxidation method according to claim 8, wherein the step of sending a pipetting signal to the pipetting mechanism (2) based on the urine sample reserve and the heated precipitation time comprises:
and if the urine sample storage amount is higher than the storage threshold value or the heating sedimentation time exceeds the preset time, sending a pipetting signal to the pipetting mechanism (2).
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