CN113866396B - Method for analyzing transuranics in feces sample - Google Patents

Method for analyzing transuranics in feces sample Download PDF

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CN113866396B
CN113866396B CN202110925595.1A CN202110925595A CN113866396B CN 113866396 B CN113866396 B CN 113866396B CN 202110925595 A CN202110925595 A CN 202110925595A CN 113866396 B CN113866396 B CN 113866396B
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ashing
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CN113866396A (en
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尹云云
汪传高
庞洪超
骆志平
李爱云
董信芳
娄海林
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China Institute of Atomic of Energy
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/48—Biological material, e.g. blood, urine; Haemocytometers
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61B10/00—Other methods or instruments for diagnosis, e.g. instruments for taking a cell sample, for biopsy, for vaccination diagnosis; Sex determination; Ovulation-period determination; Throat striking implements
    • A61B10/0038—Devices for taking faeces samples; Faecal examination devices
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/34—Purifying; Cleaning
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44—Sample treatment involving radiation, e.g. heat
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
    • G01T1/00—Measuring X-radiation, gamma radiation, corpuscular radiation, or cosmic radiation
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    • G01T1/167—Measuring radioactive content of objects, e.g. contamination
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    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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    • Y02E30/30—Nuclear fission reactors

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Abstract

The invention relates to a transuranic nuclide analysis method in a feces sample, belonging to the technical field of nuclear monitoring, and the method comprises the following steps: s1, automatically sampling the excrement of a person to be sampled by using an automatic excrement sampling device, and automatically collecting the excrement in a sample tank; s2, putting the excrement sample into carbonization and ashing integrated equipment for carbonization and ashing treatment to obtain an ash sample; s3, carrying out digestion treatment and acidity modulation on the ash sample to obtain a feed liquid; s4, separating and purifying the feed liquid by using an automatic separation and purification device to obtain a sample; and S5, selecting different devices to measure the sample according to the measurement requirements of different nuclides. The method provided by the invention is used for completing the transuranic nuclide analysis in the feces sample based on the semi-automatic device, is simple and convenient in operation process and standard in analysis process, improves the analysis precision, accuracy and efficiency, and provides technical support for the intra-personnel irradiation monitoring and dose evaluation.

Description

Method for analyzing transuranic nuclide in feces sample
Technical Field
The invention belongs to the technical field of nuclear monitoring, and particularly relates to a method for analyzing transuranic nuclides in a stool sample.
Background
The nuclear fuel post-treatment plant mainly aims at transuranic nuclides to operate, particularly, radioactive particles such as aerosol are easily generated in a complex process and high-temperature and high-humidity environment, and internal irradiation damage to personnel is inevitable. Monitoring of irradiation of uranium and transuranic nuclides by personnel is one of the important problems for personnel protection in post-treatment plants. However, the current internal irradiation monitoring means such as biological sample urine sample and direct lung measurement technology have the problem of over-high detection lower limit, and the excretion fraction of transuranic nuclide in the biological sample feces is several orders of magnitude higher than that in urine, so that the measurement of transuranic nuclide in feces can obtain lower detection limit, thus the detection lower limit of the conventional monitoring process can be reduced, and the internal irradiation monitoring method has certain advantages in the aspect of internal irradiation monitoring.
Disclosure of Invention
In order to solve the defects in the prior art, the invention aims to provide a transuranic nuclide analysis method in a feces sample aiming at the requirement of internal irradiation monitoring of a post-treatment plant.
In order to achieve the above purposes, the invention adopts a technical scheme that:
a method for analyzing transuranic nuclides in a stool sample comprises the following steps:
s1, automatically sampling the excrement of a person to be sampled by using an automatic excrement sampling device, and automatically collecting the excrement in a sample tank;
s2, putting the excrement sample into carbonization and ashing integrated equipment for carbonization and ashing treatment to obtain an ash sample;
s3, carrying out digestion treatment and acidity modulation on the ash sample to obtain a feed liquid;
s4, separating and purifying the material liquid after acidity modulation by using an automatic separation and purification device to obtain a sample;
and S5, selecting different devices to measure the sample according to the measurement requirements of different nuclides.
Further, according to the method for analyzing transuranic nuclides in the feces sample, the step S1 specifically comprises the following steps:
s101, before sampling, cleaning and drying each sample tank and each coverDry, number and weigh and record the weight of each of the sample cans and lids, noting that the weight of each of the sample cans is m 0 ；
S102, placing the weighed sample tank into a tank area of the automatic excrement sampling device, and placing a cover of the weighed sample tank into a cover area;
s103, a tested person presses down a switch of the automatic excrement sampling device, and after the sample tank is automatically transferred to a designated position below the closestool, the tested person sits down and aligns the anus to the tank opening to start sampling; after sampling is finished, the sample tank automatically slides away, is covered and sealed, and then automatically moves to the designated position of the left rear side of the device.
Further, according to the method for analyzing transuranic nuclides in a feces sample, in the step S2, the carbonization-ashing integrated equipment comprises an ashing furnace and a biological carbonization-ashing tail gas treatment system, wherein a tail gas port of the ashing furnace is connected with a tail gas inlet of the biological carbonization-ashing tail gas treatment system; the carbonization and the ashing of the excrement sample are realized through the microwave heating effect of the ashing furnace, and the purification treatment of tail gas in the carbonization and ashing processes is realized through the biological carbonization and ashing tail gas treatment system.
Still further, according to the method for analyzing transuranic nuclides in a stool sample, the concrete steps of carbonization and ashing in the step S2 include:
s201, weighing the total weight m of the sample tank and the excrement sample therein 1 Then taking off the cover of the sample tank, putting the sample tank into a quartz crucible, and putting the quartz crucible into an ashing furnace;
s202, setting various heating parameters of the ashing furnace;
s203, starting an automatic ashing program of the ashing furnace and the biological carbonization ashing tail gas treatment system in sequence, and starting a cooling water circulation system to start carbonization and ashing treatment;
s204, removing tar and malodorous gas in the tail gas through the tail gas generated in the carbonization and ashing processes by using the biological carbonization and ashing tail gas treatment system, and discharging the purified tail gas into the air through a tail gas outlet;
S205. after the automatic ashing program is finished, keeping the ashing furnace to continuously run for a preset time, then sequentially closing the ashing furnace and the power supply of the biological carbonization ashing tail gas treatment system, and keeping the closing state of the ashing furnace until the ashing furnace is naturally cooled to the room temperature; opening the ashing furnace door, taking out the sample tank, and weighing the total weight m of the sample tank and the sample ash again 2 And finally calculating the weight m of the sample ash.
Further, in the method for analyzing transuranic nuclides in the feces sample, in the step S202, the heating parameters are set to be the carbonization temperature of 300 ℃, the carbonization is completed after 10 hours of operation, the ashing temperature is 450 ℃, and the ashing is completed after 12 hours of operation.
Still further, in the method for analyzing transuranic nuclides in a stool sample, in step S205, the formula for calculating the weight of the sample ash is as follows: m = m 2 -m 0 。
Still further, the method for analyzing transuranic nuclides in a stool sample as described above further includes, after step S205: transferring the feces sample ash into a glass bottle with a cover for sealed preservation.
Further, in the method for analyzing transuranic nuclides in a feces sample, the digestion treatment in the step S3 specifically includes: and (4) putting the ash sample after carbonization and ashing are completed into a microwave digestion instrument for digestion.
Further, in the method for analyzing transuranic nuclides in the feces sample, nitric acid is used for acidity modulation in step S3.
Further, according to the method for analyzing transuranic nuclides in the feces sample, the step S4 specifically comprises the following steps:
s401, placing the prepared feed liquid into a sample tube, and then placing the sample tube filled with the feed liquid into a sample tube frame of the automatic separation and purification device;
s402, filling required reagents into corresponding reagent bottles in the automatic separation and purification device, and putting the gun heads into a gun head frame; moving the extraction column frame to the leftmost end, and filling the required resin into the resin column;
s403, turning on a power switch of the automatic separation and purification device, entering a software main interface, and editing the required extraction steps and parameters of each step;
s404, starting an operating system, and starting automatic separation and purification treatment;
s405, after the operation is finished, taking out the sample tube, and turning off the power supply.
The method has the following remarkable technical effects:
the method is based on a self-developed automatic excrement sampling device, carbonization and ashing integrated equipment and an automatic separation and purification device to carry out the collection, carbonization and ashing treatment, separation and purification of the excrement, can simplify and shorten the sampling process, realizes the standardization of the sampling process and improves the excrement sampling efficiency; tar, sulfide, carbide, nitride and other malodorous gases in the tail gas in the carbonization and ashing processes of the biological sample are removed, the operation of relevant facilities of a laboratory is maintained, the pollution of the tail gas to the laboratory and the surrounding air is prevented, and the body health of analysts and surrounding residents is protected; the automatic separation and purification device is used for replacing manual separation and purification steps of sample liquid, so that the experimental precision, accuracy and efficiency of separation and purification are improved, and the workload of operators is reduced.
Drawings
FIG. 1 is a flow chart of a method for analyzing transuranic nuclides in a stool sample according to an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of an automated fecal sampling apparatus;
FIG. 3 is a schematic structural diagram of a biological carbonization ashing tail gas treatment system;
FIG. 4 is a schematic structural diagram of an automatic separation and purification apparatus;
in fig. 2: 1-sample tank tray, 2-tray transmission device, 3-tank bin, 4-sample tank pushing device, 5-infrared position sensor, 6-sitting type sampler, 7-capping device, 8-capping bin, 9-tank lid transmission device;
in fig. 3: 11-instrument door, 12-tail gas inlet, 13-visible window, 14-tail gas outlet, 15-tar processing system, 16-condensed tail gas outlet, 17-electrostatic decomposition device and 18-active carbon adsorption device;
in fig. 4: 21-gun head frame, 22-sample pipe frame, 23-mechanical arm, 24-sample injection gun head, 25-waste gun head box, 26-extraction column, 27-waste liquid groove and 28-collection pipe frame.
Detailed Description
The invention is further described with reference to specific embodiments and drawings attached to the description.
Fig. 1 shows a flow chart of the method for analyzing transuranic nuclides in a stool sample, which comprises the following steps:
s1, automatic sampling of the excrement is carried out on a person to be sampled by using an automatic excrement sampling device, and the excrement is automatically collected in a sample tank.
The step uses a self-developed automatic fecal sample sampling device (patent No. CN 110710991B) to complete fecal sample sampling, and the structure of the step is shown in figure 2. The automatic excrement sampling device who self-develops reforms transform and has installed automatic sampling system with current bathroom as the basis, has main functions such as sample automatic collection, the seal of sample jar, sample information record, the temporary storage of sample jar. In order to avoid cross contamination of samples, the appliance of each person to be sampled is disposable and convenient to process; the sampling room has simple disinfection and deodorization functions.
The excrement sample of not engaged in radioactive personnel is gathered earlier, collects the excrement sample in ceramic material's sample jar automatically through automatic excrement sample sampling device.
The specific steps of collecting the excrement sample by using the automatic excrement sample sampling device are as follows:
s101, before sampling, cleaning, drying, numbering and weighing each sample tank and each cover, recording the weight of each sample tank and each cover, and recording the weight of each sample tank as m 0 。
Cleaning the sample tanks made of ceramic materials with decontamination powder, washing with deionized water and drying, marking a certain number on the outer side of each sample tank by a pencil, and accurately weighing the tank weight m 0 And the weight of each sample tank was recorded in the laboratory manual and the outer wall of the sample tank. A batch of sample pots were oven dried after cleaning, accurately weighed and marked with a marker to record numbers and weights on the outside wall.
S102, placing the weighed sample tank into a tank area of an automatic sampling system, placing the weighed sample tank into a cover area, and starting to sample the human excrement sample.
Before formal sampling, an experimenter firstly debugs and prepares a sample refrigerator, a label printer, a wastepaper basket and the like, cleans and sterilizes the inside of the system, and confirms that the running state of the system is normal.
S103, a tested person presses down a switch of the automatic excrement sampling device, and after the sample tank is automatically transferred to a designated position below the closestool, the tested person sits down and aligns the anus to the tank opening to start sampling; after sampling is finished, the sample tank automatically slides away, is covered and sealed, and then automatically moves to the designated position of the left rear side of the device.
When a tested person enters the sampling room, the switch of the sampling device is turned on, the sample tank is automatically transferred to the designated position below the closestool, and the tested person can sit down and align the anus to the tank opening. Before sampling is finished, the tested person does not stand up to prevent the sample tank from automatically sliding away. After sampling is finished, the sample tank automatically slides away, is covered and sealed, and then automatically moves to the designated position on the left rear side of the device. The sample code is manually input by a human subject and the label is printed, the sample tank is lifted by the sample clamp, the label paper is pasted on the outer wall of the sample tank, and then the sample tank is placed in the refrigerated cabinet.
If the examined person needs to sample for a plurality of times in a certain period, all the excrement samples can be automatically collected into the same sample tank by only repeatedly putting the same sample tank into the last position of the tank bin and repeating the operation each time.
S2, putting the excrement sample into carbonization and ashing integrated equipment for carbonization and ashing treatment to obtain an ash sample.
In the step, carbonization and ashing treatment of the excrement sample are finished by using carbonization and ashing integrated equipment. The carbonization-incineration integrated equipment comprises an ashing furnace and a biological carbonization-incineration tail gas treatment system (with the patent number of CN 211886157U), wherein the ashing furnace utilizes a microwave heating method to realize carbonization and incineration of excrement samples, and the biological carbonization-incineration tail gas treatment system is used for purifying tail gas generated in the carbonization and incineration processes of the ashing furnace, and the structure of the carbonization-incineration tail gas treatment system is shown in FIG. 3. The functions that carbonization-ashing integrated equipment possesses include: the microwave and auxiliary heat functions; the working temperature is 0-900 ℃, and the automatic temperature control operation of a series of processes such as evaporation, carbonization, ashing and the like can be realized; and (4) deodorizing.
The carbonization and ashing integrated equipment is used for carbonizing and ashing the excrement sample and comprises the following specific steps:
s201, transferring the collected sample from the refrigerated cabinet to a laboratory by an experimenter, and accurately weighing the total weight m of the sample tank and the sample 1 Then the lid of the sample tank is taken off, the sample tank is placed in a quartz crucible, the quartz crucible is placed in an ashing furnace, the crucible lid is lowered, the furnace door is closed, and the thermocouple is lowered.
S202, setting experiment parameters. Various heating parameters of the ashing furnace are adjusted through a touch screen, in the embodiment, the carbonization temperature is set to be 300 ℃, and carbonization is completed after 10 hours of operation; the ashing temperature was set at 450 ℃ and run for 12h to complete ashing.
And S203, connecting a tail gas port of the ashing furnace with a tail gas inlet of a biological carbonization and ashing tail gas treatment system, starting an automatic ashing program, then starting the biological carbonization and ashing tail gas treatment system, and simultaneously starting a cooling water circulation system.
And S204, removing tar in the tail gas through a tar treatment system from the tail gas generated in the carbonization and ashing processes, then removing malodorous gases such as sulfide, carbide and nitride in the tail gas through a cold-condensed tail gas outlet and entering an electrostatic decomposition device and an active carbon adsorption device, and discharging the purified tail gas into the air through a tail gas outlet. The circulating water amount and the cooling water temperature can be observed through the visual window.
And S205, after the automatic ashing program is finished, the ashing furnace continues to operate for a period of time, in the embodiment, the operation is set to continue for half an hour, then the power supplies of the ashing furnace and the biological carbonization ashing tail gas treatment system are sequentially closed, and the closing state of the ashing furnace is kept until the ashing furnace is naturally cooled to the room temperature. Opening the ashing oven door, carefully removing the sample tank, weighing the tank and sample ash combined weight m 2 Calculating the weight m = m of the sample ash 2 -m 0 . And transferring the feces sample ash into a glass bottle with a cover for sealed preservation for subsequent experiments.
And S3, carrying out digestion treatment and acidity modulation on the ash sample to obtain a feed liquid.
And (3) putting the ash sample after carbonization and ashing are completed into a microwave digestion instrument for digestion treatment, wherein the microwave digestion can complete the complete digestion of the ash sample within 2 hours. After digestion, the solution is subjected to acidity modulation by nitric acid for further separation and purification tests.
S4, separation and purification
In this step, a self-developed automatic separation and purification apparatus (patent No. CN 211652295U) was used to separate and purify the feed liquid, and the structure thereof is shown in fig. 4. The automatic separation and purification device mainly comprises a power unit, a flow path control unit, a heating unit, a mechanical arm platform, a pipeline system, a small column sealing structure, a controller and software. The device can automatically carry out the steps of loading, leaching, eluting and the like on the transuranic nuclide in the feed liquid.
The specific steps of separating and purifying by using the automatic separation and purification device are as follows:
s401, placing the prepared feed liquid into a sample tube, and then placing the sample tube filled with the feed liquid into a sample tube frame of an automatic separation and purification device.
S402, correspondingly filling required reagents into reagent bottles in the device, and putting the gun heads into a gun head frame of the device; the extraction column holder was moved to the far left, the desired resin was packed into the resin column, and the sealing plug under the resin was fitted.
In this example, reagents required for separation and purification include nitric acid (analytically pure), hydrogen peroxide (analytically pure), phosphoric acid (analytically pure), ammonia (analytically pure), hydrochloric acid (analytically pure), and hydrofluoric acid (analytically pure).
And S403, turning on a power switch of the automatic separation and purification device, entering a software main interface, and editing the required extraction steps and parameters of each step.
After the required materials are prepared, firstly, the running environment of the equipment is checked, the appearance and the circuit of the equipment are confirmed to be intact, a power switch of the device is turned on, and at the moment, the air exhaust and illumination functions are turned on. And after the correct user name and password are input, the user can enter a main interface of the software by clicking login. Editing required extraction steps, and editing parameters of each step in a method content area.
S404, starting an operating system, and starting automatic separation and purification treatment.
And after the extraction method is edited, returning to the main page of the software, selecting the required method name and channel, clicking 'operation' on the page, starting an operating system, and starting an automatic separation and purification process.
And S405, after the operation is finished, manually taking out the sample tube, and turning off the power supply.
And then, selecting different devices to measure the sample in the sample tube according to the measurement requirements of different nuclides.
The transuranic nuclide analysis method in the excrement sample is based on the self-developed automatic excrement sample sampling device, the carbonization and ashing integrated equipment and the automatic separation and purification device to carry out the collection, carbonization and ashing treatment, separation and purification of the excrement sample, can simplify and shorten the sampling process, realizes the standardization of the sampling process and improves the excrement sampling efficiency; tar, sulfide, carbide, nitride and other malodorous gases in the tail gas in the carbonization and ashing processes of the biological sample are removed, the operation of relevant facilities of a laboratory is maintained, the pollution of the tail gas to the laboratory and the surrounding air is prevented, and the body health of analysts and surrounding residents is protected; the automatic separation and purification device is used for replacing manual work to complete the separation and purification steps of the sample liquid, so that the experimental precision, accuracy and efficiency of separation and purification are improved, and the workload of operators is reduced.
The above-described embodiments are merely illustrative of the present invention, which may be embodied in other specific forms or in other specific forms without departing from the spirit or essential characteristics thereof. The described embodiments are, therefore, to be considered in all respects as illustrative and not restrictive. The scope of the invention should be indicated by the appended claims, and any changes that are equivalent to the intent and scope of the claims should be construed to be included therein.

Claims (7)

1. A transuranic nuclide analysis method in a feces sample comprises the following steps:
s1, automatically sampling a sample by using an automatic sample sampling device, and automatically collecting the sample in a sample tank;
s2, putting the excrement sample into carbonization and ashing integrated equipment for carbonization and ashing treatment to obtain an ash sample; the carbonization-ashing integrated equipment comprises an ashing furnace and a biological carbonization-ashing tail gas treatment system, wherein a tail gas port of the ashing furnace is connected with a tail gas inlet of the biological carbonization-ashing tail gas treatment system; the carbonization and ashing of the excrement sample are realized through the microwave heating effect of the ashing furnace, and the purification treatment of tail gas in the carbonization and ashing processes is realized through the biological carbonization and ashing tail gas treatment system; the carbonization and ashing comprises the following specific steps:
s201, weighing the total weight m of the sample tank and the excrement sample therein 1 Then taking off the cover of the sample tank, putting the sample tank into a quartz crucible, and putting the quartz crucible into an ashing furnace;
s202, setting various heating parameters of the ashing furnace;
s203, starting an automatic ashing program of the ashing furnace and the biological carbonization ashing tail gas treatment system in sequence, and starting a cooling water circulation system to start carbonization and ashing treatment;
s204, removing tar and malodorous gas in the tail gas through the tail gas generated in the carbonization and ashing processes by using the biological carbonization and ashing tail gas treatment system, and discharging the purified tail gas into the air through a tail gas outlet;
s205, after the automatic ashing program is finished, keeping the ashing furnace to continue to operate for a preset time, then sequentially closing the power supplies of the ashing furnace and the biological carbonization ashing tail gas treatment system, and keeping the closing state of the ashing furnace until the ashing furnace is naturally cooled to room temperature; opening the ashing furnace door, taking out the sample tank, and weighing the total weight m of the sample tank and the sample ash again 2 Finally, calculating the weight m of the sample ash;
s3, carrying out digestion treatment and acidity modulation on the ash sample to obtain a feed liquid;
s4, separating and purifying the feed liquid by using an automatic separation and purification device to obtain a sample, and specifically comprising the following steps:
s401, placing the prepared feed liquid into a sample tube, and then placing the sample tube filled with the feed liquid into a sample tube frame of the automatic separation and purification device;
s402, filling required reagents into corresponding reagent bottles in the automatic separation and purification device, and putting the gun heads into a gun head frame; moving the extraction column frame to the leftmost end, and filling the required resin into the resin column;
s403, turning on a power switch of the automatic separation and purification device, entering a software main interface, and editing the required extraction steps and parameters of each step;
s404, starting an operating system, and starting automatic separation and purification treatment;
s405, after the operation is finished, taking out the sample tube, and turning off a power supply;
and S5, selecting different devices to measure the sample according to the measurement requirements of different nuclides.
2. The method for analyzing transuranic nuclides in a stool sample according to claim 1, wherein the specific steps in step S1 include:
s101, before sampling, cleaning, drying, numbering and weighing each sample tank and each cover, recording the weight of each sample tank and each cover, and recording the weight of each sample tank as m 0 ；
S102, placing the weighed sample tank into a tank area of the automatic excrement sampling device, and placing the weighed sample tank cover into a cover area;
s103, a tested person presses down a switch of the automatic excrement sampling device, and after the sample tank is automatically transferred to a designated position below the closestool, the tested person sits down and aligns the anus to the tank opening to start sampling; after sampling is finished, the sample tank automatically slides away, is covered and sealed, and then automatically moves to the designated position of the left rear side of the device.
3. The method for analyzing transuranic nuclides in a stool sample according to claim 1, wherein in step S202, the heating parameters are set to a carbonization temperature of 300 ℃, the carbonization is completed after 10 hours of operation, the ashing temperature is 450 ℃, and the ashing is completed after 12 hours of operation.
4. The method for analyzing transuranic nuclides in a stool sample according to claim 1, wherein the formula for calculating the weight of the sample ash in step S205 is as follows: m = m 2 -m 0 。
5. The method for analyzing transuranic nuclides in a stool sample according to claim 1, further comprising, after step S205: the fecal sample ash was transferred to a glass bottle with a cap and stored in a sealed manner.
6. The transuranic nuclide analysis method in a stool sample according to claim 1, wherein the digestion treatment in step S3 specifically comprises: and (4) putting the ash sample after carbonization and ashing are completed into a microwave digestion instrument for digestion.
7. The method for analyzing transuranic nuclides in feces samples according to claim 6, wherein in step S3, nitric acid is used for acidity modulation.
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CN109239759A (en) * 2018-07-27 2019-01-18 国家海洋局南海环境监测中心（中国海监南海区检验鉴定中心） A kind of method of rapid-digestion sample measurement radionuclide
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