Method and system for testing stability of proficiency testing solid sample

Abstract

The invention relates to a proficiency testing solid sample stability test method and test system, and the method comprises the steps: dividing a solid sample into N parts, randomly selecting M parts from the N parts of solid samples as to-be-treated solid samples, N and M being positive integers, and M being less than or equal to N; selecting stability influence parameters of a to-be-treated solid sample, and treating the to-be-treated solid sample in the inspection environment corresponding to the stability influence parameters to obtain a to-be-inspected solid sample; the stability influence parameter at least comprises humidity; measuring the radionuclides in the M parts of the solid samples to be detected to obtain a measured average value of the radionuclides in the M parts of the solid samples to be detected; according to the half-life period of the radionuclide, the measured average value is corrected to a preset inspection date, and a corrected average value is obtained; and obtaining a stability test conclusion of the solid sample under the stability influence parameters according to the corrected average value. According to the invention, the radionuclide can be subjected to stability test.

Description

Technical Field

[0001] The invention relates to the technical field of radionuclide analysis, and in particular to a capability verification solid sample stability testing method and testing system. Background Art

[0002] For some test samples with less stable properties, transportation and time may have an impact on the characteristic quantity of the test. Therefore, before the sample is sent to the laboratory, a stability test of the relevant conditions is required. For example, the invention patent with publication number CN114384215A discloses a method for determining the long-term stability of Qinghaosan, which is used for the long-term stability determination of Qinghaosan. There is currently no relevant research on the influence of radioactive nuclides on stability. Radioactive nuclides exist in a medium, such as a proficiency testing solid sample. Changes in the quality of the proficiency testing solid sample may cause changes in the concentration of radionuclides. During the process of analysis, testing, distribution and storage, there may be various reasons that cause the proficiency testing solid sample to be affected, resulting in insufficient stability, thereby affecting the concentration of radionuclides and affecting the reliability of the analysis results of the activity concentration of radionuclides. The above problems need to be solved urgently. Summary of the invention

[0003] The invention discloses a capability verification solid sample stability testing method and a testing system, aiming to solve the technical problems existing in the prior art.

[0004] The present invention adopts the following technical solutions:

[0005] The present invention provides a method for testing the stability of a solid sample for capability verification, which comprises the following steps:

[0006] Dividing the solid sample into N portions to obtain N portions of solid samples, and randomly selecting M portions from the N portions of the solid samples as solid samples to be processed, wherein N and M are positive integers, and M is less than or equal to N;

[0007] Selecting the stability influencing parameters of the solid sample to be processed, placing the solid sample to be processed in a testing environment corresponding to the stability influencing parameters for processing, and obtaining the solid sample to be tested; the stability influencing parameters at least include: humidity;

[0008] Measuring the radioactive nuclides in the M portions of the solid sample to be tested to obtain a measured average value of the radioactive nuclides in the M portions of the solid sample to be tested;

[0009] According to the half-life of the radionuclide, the measured average value is corrected to a preset inspection date to obtain a corrected average value;

[0010] According to the corrected average value, a stability test conclusion of the solid sample under the stability influencing parameter is obtained.

[0011] In a method for testing the stability of a solid sample for capability verification of the present invention, the steps of selecting a stability influencing parameter of the solid sample to be processed, placing the solid sample to be processed in a testing environment corresponding to the stability influencing parameter for processing, and obtaining the solid sample to be tested include:

[0012] Placing M portions of the solid sample to be processed in a first humidity environment for a first time to obtain M portions of first simulated processed solid samples;

[0013] Drying M portions of the first simulated treated solid sample at a first temperature to obtain M portions of dried samples;

[0014] A first weight is taken from each of the dried samples to obtain a solid sample to be tested.

[0015] In a capability verification solid sample stability testing method of the present invention, the stability influencing parameters also include: time;

[0016] The step of selecting a stability influencing parameter of the solid sample to be processed, placing the solid sample to be processed in a testing environment corresponding to the stability influencing parameter for processing, and obtaining the solid sample to be tested comprises:

[0017] Placing M portions of the solid sample to be processed in a second humidity environment for a second time to obtain M portions of second simulated processed solid samples;

[0018] Weighing a second weight from each of the second simulated treated solid samples to obtain a solid sample to be tested;

[0019] Wherein, the second time includes: a start time node and an end time node;

[0020] The starting time node is: the time node when each of the solid samples to be processed is placed in the second humidity environment;

[0021] The end time node is: the time node when the solid sample is distributed to the participant for proficiency testing and the testing result is obtained.

[0022] In a capability verification solid sample stability testing method of the present invention, the stability influencing parameters also include: sample packaging;

[0023] The step of selecting a stability influencing parameter of the solid sample to be processed, placing the solid sample to be processed in a testing environment corresponding to the stability influencing parameter for processing, and obtaining the solid sample to be tested comprises:

[0024] The M portions of the solid samples to be processed are respectively sealed and packaged in the same manner to obtain the packaged solid samples to be processed, wherein the sealing and packaging process is carried out at normal temperature and pressure;

[0025] Each of the solid samples to be processed is mailed to a preset distance via a delivery order to obtain a solid sample to be tested.

[0026] In a capability verification solid sample stability testing method of the present invention, the stability influencing parameters also include: time and sample packaging;

[0027] The method further comprises:

[0028] Obtaining a first stability conclusion in which the stability influencing parameter is humidity, a second stability conclusion in which the stability influencing parameter is time, and a third stability conclusion in which the stability influencing parameter is sample packaging;

[0029] A stability conclusion of the solid sample is determined based on the first stability conclusion, the second stability conclusion and the third stability conclusion.

[0030] In a capability verification solid sample stability testing method of the present invention, the step of determining the stability conclusion of the solid sample according to the first stability conclusion, the second stability conclusion and the third stability conclusion comprises:

[0031] If the first stability conclusion, the second stability conclusion and the third stability conclusion are all stable, then the stability conclusion of the solid sample is stable.

[0032] Otherwise, the stability of the solid sample is concluded to be unstable.

[0033] In a method for testing the stability of a solid sample for capability verification of the present invention, the step of measuring the radioactive nuclides in M ​​portions of the solid sample to be tested to obtain the measured average value of the radioactive nuclides in the M portions of the solid sample to be tested comprises:

[0034] Performing parallel determination of the radioactive nuclides in the M portions of the solid sample to be tested according to a standard analytical method to obtain a measured value of the radioactive nuclides in each portion of the solid sample to be tested;

[0035] Repeat the measurement of the first number of times for each of the solid samples to be tested to obtain a measurement value of the total number of times of measurement; the total number of times of measurement is the product of the first number and M;

[0036] A measurement average value is determined based on the measurement values ​​of the total number of measurements.

[0037] In a method for testing the stability of a solid sample for capability verification of the present invention, the step of obtaining a stability test conclusion of the solid sample under the stability influencing parameter according to the corrected average value comprises:

[0038] Determining a statistical value according to the modified average value;

[0039] Get the critical value of stability test;

[0040] If the statistical value is less than the critical value, the stability conclusion of the solid sample under the stability influencing parameter is determined to be stable.

[0041] In a capability verification solid sample stability testing method of the present invention, the statistical value is calculated by the following formula:

[0042]

[0043] Where t represents the statistical value; μ is the specified value; n represents the total number of measurements for stability testing; It represents the corrected mean value of the stability test n times; s represents the standard deviation of the measured values ​​of the stability test n times.

[0044] In a second aspect, the present invention also provides a capability verification solid sample stability testing system, comprising:

[0045] A sample acquisition module to be processed is used to divide the solid sample into N parts to obtain N solid samples, and randomly select M parts from the N solid samples as solid samples to be processed, wherein N and M are positive integers, and M is less than or equal to N;

[0046] The sample acquisition module to be tested is used to select the stability influencing parameters of the solid sample to be processed, place the solid sample to be processed in the testing environment corresponding to the stability influencing parameters for processing, and obtain the solid sample to be tested; the stability influencing parameters at least include: humidity;

[0047] A calculation module, used for measuring the radioactive nuclides in the M portions of the solid sample to be tested, and obtaining a measured average value of the radioactive nuclides in the M portions of the solid sample to be tested;

[0048] A correction module, used for correcting the measured average value to a preset inspection date according to the half-life of the radionuclide to obtain a corrected average value;

[0049] The conclusion acquisition module is used to obtain the stability test conclusion of the solid sample under the stability influencing parameter according to the corrected average value.

[0050] The technical solution adopted by the present invention can achieve the following beneficial effects:

[0051] The present invention mainly provides a method for testing the stability of a proficiency testing solid sample, which is used for testing the stability of a proficiency testing solid sample for radionuclide detection, and determines factors that affect the stability of the proficiency testing solid sample. In the process of analyzing the activity concentration of the radionuclide, the influence of these factors is avoided, thereby improving the reliability of the analysis result of the activity concentration of the radionuclide. BRIEF DESCRIPTION OF THE DRAWINGS

[0052] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following briefly introduces the drawings required for describing the embodiments, which constitute a part of the present invention. The exemplary embodiments of the present invention and their descriptions explain the present invention and do not constitute improper limitations on the present invention. In the drawings:

[0053] Figure 1 A flow chart of a method for testing the stability of a solid sample for capability verification according to the present invention;

[0054] Figure 2 This is a solid sample processing flow chart when the stability influencing parameter is humidity in the present invention;

[0055] Figure 3 This is a solid sample processing flow chart when the stability influencing parameter is time in the present invention;

[0056] Figure 4 This is a solid sample processing flow chart when the stability influencing parameter in the present invention is sample packaging;

[0057] Figure 5 It is a flow chart of judging the stability conclusion when there are multiple stability influencing parameters in the present invention;

[0058] Figure 6 The present invention is a schematic structural diagram of a capability verification solid sample stability testing system. DETAILED DESCRIPTION

[0059] In order to make the purpose, technical solution and advantages of the present invention clearer, the technical solution of the present invention will be clearly and completely described below in conjunction with the specific embodiments of the present invention and the corresponding drawings. In the description of the present invention, it should be noted that the term "or" is usually used in the sense of including "and / or", unless the content clearly indicates otherwise.

[0060] Unless expressly indicated to the contrary, the numerical parameters in this specification and the appended claims may be approximate values ​​and can be changed according to the desired properties obtained by the content of the present invention. Specifically, all numbers used in the specification and claims to express the content of the composition, reaction conditions, etc., should be understood to be modified by the term "about" in all cases. In general, the meaning of the expression is to include a change of ±10% in some embodiments, a change of ±5% in some embodiments, a change of ±1% in some embodiments, and a change of ±0.5% in some embodiments by a specific number.

[0061] Furthermore, the word "comprising" does not exclude the presence of materials or steps not listed in the claims. Ordinal numbers such as "first", "second", "third" and Arabic numerals, letters, etc. used in the specification and claims to modify corresponding elements or steps do not themselves mean the order of the manufacturing method. The use of these ordinals is only used to make the steps clearly distinguishable.

[0062] In addition, unless the steps are specifically described or must occur in sequence, the order of the above steps is not limited to the above list, and can be changed or rearranged according to the required design. And the above embodiments can be mixed and matched with each other or with other embodiments based on design and reliability considerations, that is, the technical features in different embodiments can be freely combined to form more embodiments.

[0063] Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0064] In order to solve the problems existing in the prior art, the embodiments of the present application provide a capability verification solid sample stability testing method and testing system.

[0065] Example 1

[0066] This embodiment provides a method for testing the stability of solid samples for capability verification, which comprises the following steps:

[0067] Divide the solid sample into N parts to obtain N solid samples, and randomly select M parts from the N solid samples as solid samples to be processed, wherein N and M are positive integers, and M is less than or equal to N;

[0068] Selecting stability influencing parameters of the solid sample to be processed, placing the solid sample to be processed in a testing environment corresponding to the stability influencing parameters for processing, and obtaining the solid sample to be tested; the stability influencing parameters at least include: humidity;

[0069] Measuring the radioactive nuclides in the M portions of the solid sample to be tested to obtain a measured average value of the radioactive nuclides in the M portions of the solid sample to be tested;

[0070] According to the half-life of the radionuclide, the measured average value is corrected to the preset inspection date to obtain the corrected average value;

[0071] Based on the corrected average value, the stability test conclusion of the solid sample under the stability influencing parameters is obtained.

[0072] The invention discloses a method for testing the stability of a solid sample for capability verification, which is used for testing the stability of a solid sample for capability verification of radionuclide detection and determines factors affecting the stability of the solid sample for capability verification. In the process of analyzing the activity concentration of the radionuclide, the influence of these factors is avoided, thereby improving the reliability of the analysis result of the activity concentration of the radionuclide.

[0073] In some preferred embodiments, M portions of the solid sample to be processed can be randomly extracted from the original solid sample.

[0074] Preferably, the random sampling process may include: taking N solid samples as an example, the N solid samples are numbered sequentially, and a program for generating random numbers in Excel may be used to randomly generate M random numbers as the numbers of the randomly selected solid samples.

[0075] In some preferred embodiments, M parts can be selected as 3.

[0076] In some preferred embodiments, the solid sample may include multiple types, for example, biological ash samples, biological dry powder samples, soil samples, etc. The solid sample is a medium containing radionuclides. The present disclosure does not limit what the solid sample is specifically, and the following embodiments take the biological ash sample as an example.

[0077] The radioactive nuclide is not limited in the present disclosure and may be any radioactive nuclide. The radioactive nuclide strontium-90 is taken as an example in the present disclosure.

[0078] In some preferred embodiments, various reasons may have an impact on the solid sample, causing the solid sample to change, and ultimately causing the concentration of the radionuclide to change.

[0079] For example, during transportation, humidity may affect the solid sample, resulting in an increase in the overall weight of the solid sample or dilution of the radionuclides contained therein.

[0080] For example, in the actual proficiency testing process, if the solid sample is stored for too long, the stability of the solid sample will be affected.

[0081] For example, the packaging used to store solid samples may also affect the solid samples.

[0082] Preferably, when selecting the stability influencing parameter, the category of the stability influencing parameter can be determined according to the solid type;

[0083] For example, for biological ash samples, the parameters affecting stability may include humidity, time, and sample packaging.

[0084] If the soil sample is used, the stability influencing parameters may also include: factors that may affect the stability of the soil during transportation, for example, other impurities that may exist in the soil.

[0085] In some preferred embodiments, a specific method for determining the stability influencing parameters of the solid sample to be processed may also include: according to the target type of the solid sample, traversing the historical stability test records of the solid samples of the target type from the database, obtaining a data set of the proficiency verification analysis results of the radionuclides when the solid samples of the target type are used as proficiency verification media for radionuclides according to the historical stability test records, obtaining the abnormal analysis results of the proficiency verification of the radionuclides from the data set, obtaining a first solid sample of the target type in the abnormal analysis process corresponding to the abnormal analysis result, and obtaining a second solid sample of the target type in the normal analysis process corresponding to the normal analysis result, comparing the first solid sample and the second solid sample to obtain the influencing factors of the stability of the first solid sample, and using the influencing factors as the stability influencing parameters.

[0086] In some preferred embodiments, the analysis method may include a standard analysis method for analyzing radionuclides, for example, it may include: HJ815-2016 standard analysis method, but the present disclosure is not limited thereto, and for different radionuclides, the corresponding standard analysis methods may also be different.

[0087] In some preferred embodiments, the method for obtaining the measurement average value of the radioactive nuclides may include: in the process of analyzing the radioactive nuclides in M ​​portions of solid samples to be tested according to the standard analysis method, the radioactive nuclides in the M portions of solid samples to be tested are detected in parallel to obtain the measurement value of the radioactive nuclides in each solid sample to be tested; for each solid sample to be tested, the first number of measurements are repeated on the radioactive nuclides to obtain the measurement value of the total number of measurements; the total number of measurements is the product of the first number and the M portions; and the measurement average value is determined based on the measurement value of the total number of measurements.

[0088] There are also many specific ways to analyze and measure radioactive nuclides. The present disclosure uses the α / β counter measurement method as an example, but is not limited to this.

[0089] Among them, the standard analysis methods include specific analysis processes for radioactive nuclides, and the series of analysis processes in the standard analysis methods will not be repeated in this disclosure.

[0090] The measurement value of each solid sample to be tested is obtained by the above standard analysis method. The measurement can be repeated for a preset number of times for each solid sample to be tested to obtain the measurement value of the total number of measurements, and the average value is determined.

[0091] The total number of measurements n is the product of the first number and M. In the present disclosure, the first number can be selected as 2, then n=6.

[0092] Among them, the measured value of the radionuclide is the activity concentration of strontium-90.

[0093] In some preferred embodiments, the radioactive nuclide has a half-life. After obtaining the measured average value, the measured average value needs to be corrected according to the half-life to a preset inspection date to obtain a corrected average value.

[0094] For example, if the current date when the measurement average value is obtained is September 2, 2024, and the preset inspection date can also be understood as a designated date, and the designated date is January 1, 2024, then the obtained measurement average value cannot represent the activity concentration value on the designated date, and should be corrected according to the half-life of the radionuclide to obtain the corrected average value of the radionuclide on January 1, 2024.

[0095] In some preferred embodiments, when performing stability testing on solid samples in the present disclosure, corresponding stability influencing parameters can be flexibly selected.

[0096] For example, if the stability influencing parameter only includes humidity, then only humidity can be selected as the stability influencing parameter. After the humidity test, the stability conclusion of the solid sample is stable, which means that the solid sample is stable.

[0097] Exemplarily, if the stability influencing parameters include humidity and time, for example, the solid sample may volatilize due to long storage time, then the stability influencing parameters can be selected as humidity and time. After testing the humidity and time, the stability conclusion of the solid sample is stable, which means that the solid sample is stable.

[0098] For example, if the stability influencing parameters include humidity, time, packaging and other parameters, all of them can be tested, and the stability conclusion corresponding to all the stability influencing parameters corresponding to the solid sample is stable, which means that the solid sample is stable.

[0099] like Figure 5As shown, in the present disclosure, taking the stability influencing parameters including humidity, time and sample packaging as an example, the method of determining whether the solid sample is stable may include: obtaining a first stability conclusion in which the stability influencing parameter is humidity, a second stability conclusion in which the stability influencing parameter is time, and a third stability conclusion in which the stability influencing parameter is sample packaging, and determining the stability conclusion of the solid sample based on the first stability conclusion, the second stability conclusion and the third stability conclusion.

[0100] Exemplarily, if the first stability conclusion, the second stability conclusion and the third stability conclusion are all stable, then the stability conclusion of the solid sample is stable.

[0101] For example, if the first stability conclusion and the second stability conclusion are stable, and the third stability conclusion is unstable, then the stability conclusion of the solid sample is unstable, and it can be concluded that the instability of the solid sample is caused by the sample packaging, and the sample packaging is improved. For example, during the stability test, the sample packaging is a plastic container, which is damaged during transportation, causing the solid sample to leak or seep out, resulting in a change in the quality of the solid sample. The sample packaging can be improved by replacing it with a stronger packaging to ensure the stability of the solid sample.

[0102] In some preferred embodiments, after distributing solid samples to participants in one round of proficiency testing, the remaining solid samples are used as retained samples. When the retained samples are needed for a second round of proficiency testing and are distributed to participants again, the retained samples should be retested for stability before distributing the samples, and samples can be distributed again only after the stability test passes.

[0103] Among them, for a round of proficiency testing process, when conducting stability testing on solid samples, before distributing the solid samples to participants, it is necessary to complete the stability testing process with stability influencing parameters such as humidity and sample packaging. For the stability testing process with stability influencing parameters such as time, it is necessary to obtain the solid samples to be tested.

[0104] In some preferred embodiments, Figure 2 As shown, the steps of selecting stability influencing parameters of the solid sample to be processed, placing the solid sample to be processed in a testing environment corresponding to the stability influencing parameters for processing, and obtaining the solid sample to be tested include:

[0105] After placing M portions of the solid samples to be processed in a first humidity environment for a first processing time, M portions of first simulated processed solid samples are obtained; wherein the first humidity environment is an environment with a humidity greater than the first humidity.

[0106] Drying M portions of the first simulated treated solid sample at a first temperature to obtain M portions of dried samples; preferably, the dried solid sample is stored in a desiccator to avoid moisture absorption again;

[0107] A first weight is taken from each dried sample to obtain M solid samples to be tested.

[0108] Exemplarily, if the solid sample is a biological ash sample, the first humidity may be 60%; the first time may be 3 days; the first temperature may be 105° C.; and the first weight may be 15.0 g.

[0109] The time period from the time the solid sample is sent out to the time the participant starts proficiency testing can be called the time period for distributing the solid sample.

[0110] Exemplarily, taking a bio-ash sample as a solid sample, the maximum humidity condition is simulated by the above method, 3 samples are randomly selected, and placed in an environment with a humidity condition of more than 60% for 3 days to obtain a first simulated treated solid sample, the first simulated treated solid sample is placed in an oven at 105°C and dried to constant weight, then taken out and placed in a dryer. After reaching room temperature, a prepared solid sample is obtained, and 15.0 g of the prepared solid sample is taken as the solid sample to be tested.

[0111] In some preferred embodiments, Figure 3 As shown, the stability influencing parameters also include: time;

[0112] The steps of selecting a stability influencing parameter of a solid sample to be processed, placing the solid sample to be processed in a testing environment corresponding to the stability influencing parameter for processing, and obtaining the solid sample to be tested include:

[0113] After placing M portions of the solid samples to be processed in a second humidity environment and processing them for a second time, M portions of second simulated processed solid samples are obtained; wherein the second humidity environment is an environment with a humidity greater than the second humidity; specifically, the second humidity and the first humidity as well as the first time and the second time may be the same or different; when they are the same, it is preferred to maintain the same humidity during measurement, and when they are different, maintain the second humidity during measurement, such as the humidity of the second humidity conventional environment.

[0114] Weighing a second weight from each second simulated treated solid sample to obtain M portions of solid samples to be tested;

[0115] The second time includes: a start time node and an end time node;

[0116] The starting time node is: the time node when each solid sample to be processed is placed in the second humidity environment;

[0117] The end time node is: the time node when the solid samples are distributed to the participants for proficiency testing and the testing results are obtained.

[0118] In some preferred embodiments, taking the solid sample as a biological ash sample as an example, the second preset humidity may be 40%; and the second preset weight may be 15.0 g.

[0119] The purpose of placing the target time period is, first of all, to test the effect of time on stability in the results obtained by the participants in the proficiency testing. It can be understood that after the target time period, if the stability conclusion of the solid sample tested after the second time is stable, then the length of storage time has no effect on the stability of the solid sample, and the results obtained by the participants in the proficiency testing do not meet expectations and are not caused by the storage time. Secondly, the storage time can also be extended, and the time span for the storage time test can be 6 months.

[0120] In some preferred embodiments, there may be multiple sampling methods for solid samples for storage time inspection, which are not limited to a specific processing method. The following methods may be used to illustrate the sampling methods. Taking the solid sample as a biological ash sample as an example, the sampling methods may specifically include:

[0121] Method 1:

[0122] Three solid samples to be processed can be randomly selected from the solid samples, sealed with sealing film, and stored in an environment with an ambient humidity of less than 60%. After the time of the last participant to complete the analysis is obtained, that is, after waiting for the target time period, they are taken out to obtain the solid samples to be tested corresponding to the storage time test.

[0123] Method 2:

[0124] If the solid sample to be tested obtained during the humidity test has a remaining amount sufficient for storage time testing after the first weight of the solid sample to be tested is extracted, the remaining solid sample to be tested can be used to save solid samples and achieve the purpose of cost saving.

[0125] The remaining solid samples to be tested are used as solid samples to be extracted for the storage time test. The samples to be extracted for the storage time test are sealed with sealing films and stored in an environment with an ambient humidity of less than 60%. After the participants return the results, that is, after waiting for the target time period, the samples are taken out to obtain the solid samples to be tested corresponding to the storage time test.

[0126] It should be noted that in the present disclosure, different stability test types may be tested separately for different rounds. For example, only humidity test may be performed for the first round, and only storage time test may be performed for the second round.

[0127] It is also possible to carry out multiple inspection processes such as storage time inspection and humidity inspection at the same time for the same round. If multiple inspections are carried out at the same time, it is necessary to directly extract solid samples for storage time inspection and humidity inspection from the same batch of solid samples. It is necessary to extract the same batch of solid samples.

[0128] For example, taking the example of performing multiple tests simultaneously in the same round as an example, the specific method may include:

[0129] Taking N solid samples as an example, you can choose to use N1 for uniformity test, N2 for humidity test, N3 for distribution to participants for proficiency testing, and N4 for storage time test. If other types of stability influencing parameter test processes are required, you can continue to randomly select from the N solid samples.

[0130] It should be noted that when randomly generating the numbers of the solid samples to be processed, the numbers of the solid samples to be processed drawn will not be repeated with the numbers of the solid samples to be processed drawn previously.

[0131] Here, we only take 4 samples from N solid samples as an example, and the specific limit of quantity can be: N2 = N4 = 3. N2 is 3 randomly selected from N-N1, and N4 is 3 randomly selected from N-N1-N2-N3.

[0132] By the above method, after obtaining the solid sample to be tested for the storage time test, the stability conclusion corresponding to the storage time test is obtained.

[0133] In some preferred embodiments, Figure 4 As shown, the stability influencing parameters also include: sample packaging;

[0134] The steps of selecting a stability influencing parameter of a solid sample to be processed, placing the solid sample to be processed in a testing environment corresponding to the stability influencing parameter for processing, and obtaining the solid sample to be tested include:

[0135] The M portions of solid samples to be processed are respectively sealed and packaged in the same manner to obtain packaged solid samples to be processed, and the sealing and packaging process is carried out at normal temperature and pressure;

[0136] Each solid sample to be processed is mailed to a preset distance via a delivery order to obtain a solid sample to be inspected.

[0137] In some preferred embodiments, the sealed package may be a disposable sealed plastic bottle.

[0138] The delivery order is mailed over a preset distance, which can be greater than 1,000 kilometers, to ensure that enough time is left for the transportation process. After the preset distance is mailed, the solid samples to be tested are obtained, and then corresponding analysis and measurement are performed on the solid samples to be tested to obtain the corresponding stability conclusions of the sample packaging inspection.

[0139] In some preferred embodiments, the step of measuring the radioactive nuclides in M ​​portions of the solid sample to be tested and obtaining the measured average value of the radioactive nuclides in the M portions of the solid sample to be tested comprises:

[0140] Performing parallel determination of radioactive nuclides in M ​​portions of the solid sample to be tested according to the standard analytical method to obtain the measured value of the radioactive nuclides in each portion of the solid sample to be tested;

[0141] Repeat the measurement of the first number of radionuclides in each solid sample to be tested to obtain the measurement value of the total number of measurements; the total number of measurements is the product of the first number and M;

[0142] Based on the measured values ​​of the total number of measurements, the measurement average is determined.

[0143] In some preferred embodiments, the step of obtaining a stability test conclusion of the solid sample under the stability influencing parameter according to the corrected average value comprises:

[0144] Determine the statistical value based on the corrected mean value;

[0145] Get the critical value of stability test;

[0146] If the statistical value is less than the critical value, the stability conclusion of the solid sample under the stability influencing parameter is determined to be stable, otherwise, the stability conclusion is unstable.

[0147] In some preferred embodiments, the stability of the sample containing the radionuclide can be determined in a variety of ways based on the measured mean value of the radionuclide, including: t-test method, xy≤0.3σ criterion method, etc. Among them, the t-test method can include a variety of ways, such as: comparing a corrected mean value with a standard value / reference value / specified value, or whether there is a significant difference between two corrected mean values.

[0148] The specific method adopted can be illustrated by the following embodiments:

[0149] In the present disclosure, the t-test method can be selected to compare whether there is a significant difference between an average value and a specified value to determine stability.

[0150] Method 1: Whether there is a significant difference between the corrected mean value and the standard value / reference value / specified value to determine stability:

[0151] Determining the statistical value based on the corrected mean value may include the following steps: obtaining a specified value of the activity concentration of the radionuclide on a preset inspection date, and determining the statistical value based on the corrected mean value and the specified value of the stability inspection.

[0152] Exemplarily, the method of determining the statistical value may include: determining the deviation value based on the corrected mean value of the stability test and the specified value, determining the intermediate value based on the deviation value and the total number of measurements, determining the standard deviation of the measurement values ​​of the stability test under the total number of measurements, and determining the statistical value based on the intermediate value and the standard deviation.

[0153] Exemplarily, the statistical value may be determined by the following formula, as shown below:

[0154]

[0155] Where t represents the statistical value; μ is the specified value; n represents the total number of measurements for stability testing; It represents the corrected mean value of the stability test n times; s represents the standard deviation of the measured values ​​of the stability test n times.

[0156] Based on the first method, the method of obtaining the critical value of the stability test may include: determining the degree of freedom of the critical value according to the total number of measurements of the stability test, and determining the critical value in the t distribution according to the preset confidence level and degree of freedom.

[0157] For example, if n is 6, then n-1 is the degree of freedom, and the degree of freedom is 5. The significance level can be taken as α=0.05, and the critical value is determined as t in the t distribution. 0.05 (5).

[0158] If the statistical value t <t 0.05 (5), the stability of the solid sample meets the requirements, and the stability conclusion of the solid sample is stable.

[0159] Method 2: Select the t-test method to compare whether there is a significant difference between the two mean values ​​to determine stability.

[0160] Determining the statistical value based on the corrected mean value may include the following steps: obtaining the uniformity mean value of the uniformity test when testing the solid sample for uniformity, and correcting the uniformity mean value to a preset test date according to the half-life of the radioactive nuclide to obtain a uniformity corrected mean value, and determining the statistical value based on the uniformity corrected mean value and the corrected mean value of the stability test.

[0161] The statistical value can be determined by the formula below, as shown below:

[0162]

[0163] Where t represents the statistical value; n represents the total number of measurements for stability testing; represents the corrected mean value of the stability test n times; s represents the standard deviation of the stability test n times; n1 represents the total number of measurements of the uniformity test; It represents the uniformity corrected mean value of the uniformity test; s1 represents the standard deviation of the n measured values ​​of the uniformity test.

[0164] Based on the second method, the method of obtaining the critical value of the stability test may include: determining the degrees of freedom of the critical value according to the total number of measurements of the stability test and the total number of measurements of the uniformity test, and determining the critical value in the t distribution according to the preset confidence level and degrees of freedom.

[0165] Example 2

[0166] This embodiment provides a capability verification solid sample stability testing system, such as Figure 6 As shown, it includes:

[0167] A sample acquisition module to be processed is used to divide the solid sample into N parts to obtain N solid samples, and randomly select M parts from the N solid samples as solid samples to be processed, wherein N and M are positive integers, and M is less than or equal to N;

[0168] The sample acquisition module to be tested is used to select the stability influencing parameters of the solid sample to be processed, place the solid sample to be processed in the testing environment corresponding to the stability influencing parameters for processing, and obtain the solid sample to be tested; the stability influencing parameters at least include: humidity;

[0169] A calculation module, used for measuring the radioactive nuclides in the M portions of the solid sample to be tested, and obtaining a measured average value of the radioactive nuclides in the M portions of the solid sample to be tested;

[0170] A correction module, used to correct the measured average value to a preset inspection date according to the half-life of the radionuclide to obtain a corrected average value;

[0171] The conclusion acquisition module is used to obtain the stability test conclusion of the solid sample under the stability influencing parameters according to the corrected average value.

[0172] The embodiments of the present invention are described above in conjunction with the accompanying drawings, but the present invention is not limited to the above-mentioned specific implementation modes, which are merely illustrative rather than restrictive. Under the guidance of the present invention, ordinary technicians in this field can also make many forms without departing from the scope of protection of the present invention and the claims, all of which are within the protection of the present invention.

Claims

1. A method for testing the stability of solid samples for capability verification, characterized in that: The steps include: Dividing the solid sample into N portions to obtain N portions of solid samples, and randomly selecting M portions from the N portions of the solid samples as solid samples to be processed, wherein N and M are positive integers, and M is less than or equal to N; Selecting a stability influencing parameter of the solid sample to be processed, placing the solid sample to be processed in a testing environment corresponding to the stability influencing parameter for processing, and obtaining a solid sample to be tested; The stability influencing parameters include at least: humidity; Measuring the radioactive nuclides in the M portions of the solid sample to be tested to obtain a measured average value of the radioactive nuclides in the M portions of the solid sample to be tested; According to the half-life of the radionuclide, the measured average value is corrected to a preset inspection date to obtain a corrected average value; According to the corrected average value, a stability test conclusion of the solid sample under the stability influencing parameter is obtained.

2. A method for testing the stability of solid samples for capability testing according to claim 1, characterized in that: The step of selecting a stability influencing parameter of the solid sample to be processed, placing the solid sample to be processed in a testing environment corresponding to the stability influencing parameter for processing, and obtaining the solid sample to be tested comprises: Placing M portions of the solid sample to be processed in a first humidity environment for a first time to obtain M portions of first simulated processed solid samples; Drying M portions of the first simulated treated solid sample at a first temperature to obtain M portions of dried samples; A first weight is taken from each of the dried samples to obtain a solid sample to be tested.

3. A capability testing solid sample stability testing method according to claim 1, characterized in that: The stability influencing parameters also include: time; The step of selecting a stability influencing parameter of the solid sample to be processed, placing the solid sample to be processed in a testing environment corresponding to the stability influencing parameter for processing, and obtaining the solid sample to be tested comprises: Placing M portions of the solid sample to be processed in a second humidity environment for a second time to obtain M portions of second simulated processed solid samples; Weighing a second weight from each of the second simulated treated solid samples to obtain a solid sample to be tested; Wherein, the second time includes: a start time node and an end time node; The starting time node is: the time node when each of the solid samples to be processed is placed in the second humidity environment; The end time node is: the time node when the solid sample is distributed to the participant for proficiency testing and the testing result is obtained.

4. A method for testing the stability of solid samples for capability testing according to claim 1, characterized in that: The stability influencing parameters also include: sample packaging; The step of selecting a stability influencing parameter of the solid sample to be processed, placing the solid sample to be processed in a testing environment corresponding to the stability influencing parameter for processing, and obtaining the solid sample to be tested comprises: The M portions of the solid samples to be processed are respectively sealed and packaged in the same manner to obtain the packaged solid samples to be processed, wherein the sealing and packaging process is carried out at normal temperature and pressure; Each of the solid samples to be processed is mailed to a preset distance via a delivery order to obtain a solid sample to be tested.

5. A method for testing the stability of solid samples for capability testing according to claim 1, characterized in that: The stability influencing parameters also include: time and sample packaging; The method further comprises: Obtaining a first stability conclusion in which the stability influencing parameter is humidity, a second stability conclusion in which the stability influencing parameter is time, and a third stability conclusion in which the stability influencing parameter is sample packaging; A stability conclusion of the solid sample is determined based on the first stability conclusion, the second stability conclusion and the third stability conclusion.

6. A method for testing the stability of solid samples for capability testing according to claim 5, characterized in that: The step of determining the stability conclusion of the solid sample according to the first stability conclusion, the second stability conclusion and the third stability conclusion comprises: If the first stability conclusion, the second stability conclusion and the third stability conclusion are all stable, then the stability conclusion of the solid sample is stable. Otherwise, the stability of the solid sample is concluded to be unstable.

7. A method for testing the stability of solid samples for capability testing according to claim 1, characterized in that: The step of measuring the radioactive nuclides in the M portions of the solid sample to be tested to obtain the measured average value of the radioactive nuclides in the M portions of the solid sample to be tested comprises: Performing parallel determination of the radioactive nuclides in the M portions of the solid sample to be tested according to a standard analytical method to obtain a measured value of the radioactive nuclides in each portion of the solid sample to be tested; Repeat the measurement of the first number of times for each of the solid samples to be tested to obtain a measurement value of the total number of times of measurement; the total number of times of measurement is the product of the first number and M; A measurement average value is determined based on the measurement values ​​of the total number of measurements.

8. A method for testing the stability of solid samples for capability testing according to claim 1, characterized in that: The step of obtaining a stability test conclusion of the solid sample under the stability influencing parameter according to the corrected average value comprises: Determining a statistical value according to the modified average value; Get the critical value of stability test; If the statistical value is less than the critical value, the stability conclusion of the solid sample under the stability influencing parameter is determined to be stable.

9. A method for testing the stability of solid samples for capability testing according to claim 7, characterized in that: The statistical value is calculated by the following formula; Where t represents the statistical value; μ is the specified value; n represents the total number of measurements for stability testing; It represents the corrected mean value of the stability test n times; s represents the standard deviation of the measured values ​​of the stability test n times.

10. A capability testing solid sample stability testing system, characterized in that: include: A sample acquisition module to be processed is used to divide the solid sample into N parts to obtain N solid samples, and randomly select M parts from the N solid samples as solid samples to be processed, wherein N and M are positive integers, and M is less than or equal to N; A sample acquisition module to be tested, used for selecting the stability influencing parameter of the solid sample to be processed, placing the solid sample to be processed in a testing environment corresponding to the stability influencing parameter for processing, and obtaining the solid sample to be tested; The stability influencing parameters include at least: humidity; A calculation module, used for measuring the radioactive nuclides in the M portions of the solid sample to be tested, and obtaining a measured average value of the radioactive nuclides in the M portions of the solid sample to be tested; A correction module, used for correcting the measured average value to a preset inspection date according to the half-life of the radionuclide to obtain a corrected average value; The conclusion acquisition module is used to obtain the stability test conclusion of the solid sample under the stability influencing parameter according to the corrected average value.

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