ICP-MS (Inductively Coupled Plasma Mass Spectrometry)-based trace element detection uncertainty evaluation system and method
By constructing an ICP-MS trace element detection uncertainty assessment system, the problem of inaccurate uncertainty assessment in trace element detection is solved, and efficient and reliable detection result evaluation and method optimization are achieved.
Patent Information
- Application Number
- CN202510484479.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-17
- Publication Date
- 2025-08-01
AI Technical Summary
In the process of detecting trace elements, the prior art has problems such as inaccurate assessment of uncertainty, low evaluation efficiency, and difficulty in comprehensively identifying and controlling uncertain factors that affect the detection results.
A trace element detection uncertainty assessment system is built based on ICP-MS, including uncertainty data collection, calculation, result analysis, feedback and evaluation modules. By automatically processing the entire experimental process data, uncertainty factors are identified and controlled, and comprehensive evaluation is provided.
It improves the accuracy and efficiency of trace element detection, ensures the reliability and quality of detection results, and realizes the standardization and continuous optimization of detection methods.
Smart Images

Figure CN120412787A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of instrumental analysis in analytical detection technology, and particularly to a system and method for evaluating the uncertainty of trace element detection based on ICP-MS. Background Art
[0002] Due to its characteristics of high sensitivity, high throughput, reliable method, and easy combination with other technologies, ICP-MS technology is widely used in the fields of environmental monitoring, food safety, biomedicine, materials science, geological research, and industrial quality control. ICP-MS technology combines the high-temperature ionization characteristics of inductively coupled plasma and the detection limit characteristics of mass spectrometry to form a powerful elemental analysis technology for simultaneous determination of multiple elements with low detection limits. In the field of geological research, the application of ICP-MS technology is becoming increasingly extensive and in-depth, especially playing a key role in trace element analysis. Trace elements, as important indicators of geochemical composition, their distribution characteristics and content changes have important scientific significance for revealing the origin of rocks, the formation mechanism of ore deposits, and the geological evolution history. These trace elements often serve as "fingerprint" markers of geological processes and are attracting more and more attention in mineral resource exploration and environmental geological research. Therefore, accurate detection and uncertainty evaluation of trace elements are of great significance, which is exactly the technical problem to be solved by the present invention. Summary of the Invention
[0003] (1) Technical Problems to be Solved
[0004] Aiming at the deficiencies of the prior art, the present invention provides a system and method for evaluating the uncertainty of trace element detection based on ICP-MS, which has the advantages of high sensitivity, high throughput, reliable method, and easy combination with other technologies, and solves the problems of inaccurate uncertainty evaluation, low evaluation efficiency, and difficulty in comprehensively identifying and controlling the uncertain factors affecting the detection results in the process of trace element detection by traditional methods.
[0005] (2) Technical Solutions
[0006] To achieve the above object, the present invention provides the following technical solution: A system for evaluating the uncertainty of trace element detection based on ICP-MS, including an uncertainty data collection module, an uncertainty calculation module, an uncertainty result analysis module, an uncertainty analysis feedback module, and an uncertainty evaluation module;
[0007] The uncertainty data collection module collects the original data related to uncertainty in the entire experimental process and supports structured input and storage;
[0008] The uncertainty calculation module automatically calculates each uncertainty component and the combined expanded uncertainty according to the original data collected by the uncertainty data collection module;
[0009] The uncertainty result analysis module analyzes based on the combined standard uncertainty and expanded uncertainty obtained from the above calculations to evaluate the influence degree of uncertainty on the detection result;
[0010] If the uncertainty analysis and feedback module finds that the uncertainty is too large or there are other problems, it will promptly give feedback to the relevant links;
[0011] The uncertainty evaluation module comprehensively evaluates the detection of a certain trace element in the sample according to the data and analysis results provided by the above-mentioned various modules.
[0012] Preferably, the uncertainty data collection module includes a sample mass data unit and an instrument certificate data unit.
[0013] Preferably, the sample mass data unit includes the sample mass m.
[0014] Preferably, the instrument certificate data unit includes the verification certificate of the sample weighing balance, the verification certificate of the sample weighing balance, and the pipette certificate. By consulting the pipette certificate used, the tolerances of the 200 μL adjustable pipette are: ±0.n%, and the tolerances of the 1000 μL adjustable pipette are: ±0.m%.
[0015] Preferably, the uncertainty calculation module includes a component measurement unit, a chemical pretreatment method unit, a standard stock solution unit, an instrument measurement unit, and an experiment unit.
[0016] Preferably, the component measurement unit calculates the relative uncertainty U of component measurement based on the component vector of the measurement result r(测) , and its calculation formula is:
[0017]
[0018] In the formula, U r(测) represents the relative uncertainty of component measurement, n represents the total number of uncertainty components, x i represents the i-th uncertainty component, represents the average value of component measurement, S a represents the standard deviation of component measurement, U 测(a) represents the relative uncertainty of a component measurement.
[0019] Preferably, the chemical pretreatment method unit calculates the uncertainty U of the recovery rate of the chemical pretreatment method r(ec) , and the digestion recovery rate of a certain element is: for example, 98% - 102%, and its calculation formula is:
[0020] b + =(102 - 100)% = 2% b -=(100 - 98)% = 2%
[0021]
[0022] In the formula, U r(ec) represents the uncertainty of the recovery rate of the chemical pretreatment method, and b + represents the maximum deviation of the recovery rate of the chemical pretreatment method, that is, (102 - 100)% = 2%, and b - represents the minimum deviation of the recovery rate of the chemical pretreatment method, that is, (100 - 98)% = 2%.
[0023] Preferably, the standard stock solution unit obtains the uncertainty U of the standard substance by referring to the certificate of the reference material used in the test r(标)(a) , and the instrument measurement unit calculates the uncertainty U of the electronic balance and the uncertainty U of the volumetric balance according to the sample mass m and the verification certificate of the volumetric weighing instrument for the solution r(m) and the uncertainty U of the volumetric balance r(ml) , and the formula for calculating the uncertainty U of the electronic balance r(m) is:
[0024]
[0025] In the formula, U r(m) represents the uncertainty of the electronic balance, represents the sample mass, and the balance U given in the verification certificate of the sample weighing balance used in this experiment (m) = mg (K = 2);
[0026] The formula for calculating the uncertainty U of the volumetric balance r(ml) is:
[0027]
[0028] In the formula, U r(ml) represents the uncertainty of the volumetric balance, represents the sample mass, and the verification certificate of the volumetric balance of the solution used in this experiment gives the U of this balance (m) = mg (K = 2);
[0029] The instrument measurement unit obtains the instrument uncertainty U of the inductively coupled plasma mass spectrometer by referring to the tolerance of ±0.n% given in the verification certificate of the instrument used r(仪) , that is, U r(仪) = 0.n%;
[0030] The uncertainty U introduced in the dilution process r(移) , and its calculation formula is:
[0031]
[0032] In the formula, U r(移) represents the uncertainty introduced by the dilution process, ±0.n% represents the tolerance of the 200 μL adjustable pipette in the pipette certificate used, and ±0.m% represents the tolerance of the 1000 μL adjustable pipette in the pipette certificate used;
[0033] The experimental unit includes calculating the uncertainty of sample blank variability U r(空白) , calculating the uncertainty of the acid and water reagents for detection U r(试剂) , calculating the uncertainty of laboratory temperature and humidity U r(E) , calculating the uncertainty of the container volume U r(容) , and consider whether it can be ignored depending on the laboratory situation.
[0034] Preferably, the uncertainty evaluation module conducts the evaluation of the expanded uncertainty U (a) , and its evaluation method is as follows:
[0035] (1) Calculate the relative uncertainty of all uncertainty components of the influencing factors in the detection process, where U r(空白) , U r(试剂) , U r(E) and U r(容) are ignored, and its calculation formula is:
[0036]
[0037] (2) The calculation formula for the combined standard uncertainty U c(合成) is:
[0038]
[0039] In the formula, U c(合成) represents the combined standard uncertainty, represents the average value of the combined measurement result, and U rc(总) represents the relative uncertainty of all uncertainty components of the influencing factors in the detection process;
[0040] (3) The coverage factor k for a 95% confidence probability is 2. Multiply the combined standard uncertainty by the coverage factor to calculate the expanded uncertainty U (a) of the measurement result, and its calculation formula is:
[0041] U (a) = k × U c(合成)
[0042] In the formula, U (a) represents the expanded uncertainty U (a) , k represents the coverage factor for a 95% confidence probability, and k = 2.
[0043] A method for evaluating the uncertainty of trace element detection based on ICP-MS, comprising the following steps:
[0044] S1. Data collection: Collect the original data related to uncertainty in the whole experimental process through the uncertainty data collection module;
[0045] S2. Data entry and storage: Enter and store the collected data in a structured manner in the database of the system;
[0046] S3. Uncertainty calculation: Use the uncertainty calculation module to calculate each uncertainty component and the combined expanded uncertainty according to the collected original data;
[0047] S4. Result analysis: Analyze the combined standard uncertainty and expanded uncertainty obtained by calculation through the uncertainty result analysis module;
[0048] S5. Feedback and improvement: When the uncertainty is too large or there are other problems, the uncertainty analysis feedback module will promptly feedback to the relevant links;
[0049] S6. Comprehensive evaluation: The uncertainty evaluation module comprehensively evaluates the detection of a certain trace element in the sample according to the data and analysis results provided by the above-mentioned modules.
[0050] Compared with the prior art, the present invention provides a system and method for evaluating the uncertainty of trace element detection based on ICP-MS, having the following beneficial effects:
[0051] 1. The present invention realizes the full - process management of the uncertainty evaluation for trace element detection by constructing an uncertainty data collection module, an uncertainty calculation module, an uncertainty result analysis module, an uncertainty analysis feedback module, and an uncertainty evaluation module. The uncertainty data collection module is responsible for systematically managing data to ensure the accuracy, integrity, and traceability of the original data related to uncertainty in the entire experimental process. The uncertainty calculation module automatically calculates each uncertainty component and the combined expanded uncertainty based on the collected data, which can not only improve the evaluation efficiency but also help comprehensively identify and control various uncertainty factors affecting the detection results. The uncertainty result analysis module analyzes the calculated combined standard uncertainty and expanded uncertainty to evaluate the influence degree of uncertainty on the detection results, further ensuring the reliability of the detection results. When the uncertainty analysis feedback module discovers that the uncertainty is too large or there are other problems, it will promptly feedback to the relevant links, which helps to quickly discover and solve problems, thereby improving the overall quality of the detection process. The uncertainty evaluation module comprehensively evaluates the detection of a certain trace element in the sample based on the data and analysis results provided by the above - mentioned modules. Through the above - mentioned detection process, the present invention can not only improve the accuracy of trace element detection but also, through the timely feedback and continuous improvement mechanism of the uncertainty analysis feedback module, improve the quality and efficiency of the detection process, and finally realize the standardization of the detection method and the continuous optimization of the technology, providing an efficient and reliable uncertainty evaluation method for the field of trace element detection. Description of the Drawings
[0052] Figure 1 is the flowchart of the method of the present invention;
[0053] Figure 2 is the source diagram of the uncertainty of the content of a certain element measured by ICP - MS of the present invention. Detailed Embodiments
[0054] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.
[0055] Please refer to Figure 1 - Figure 2 , an uncertainty evaluation system for trace element detection based on ICP - MS, including an uncertainty data collection module, an uncertainty calculation module, an uncertainty result analysis module, an uncertainty analysis feedback module, and an uncertainty evaluation module;
[0056] The uncertainty data collection module collects the raw data related to uncertainty in the whole process of the experiment. The raw data includes sample information (sample submitting unit, sample name, testing items), experimental conditions (testing basis, instrument name and equipment number, instrument analysis conditions, environmental conditions between instruments), personnel information (approval, review, compilation), and testing time. It supports structured input and storage, which can ensure the accuracy, integrity, and traceability of the data. For the sample name, it is entered and stored in the system database in a specific format for convenient subsequent query and call;
[0057] The uncertainty calculation module automatically calculates each uncertainty component and the combined expanded uncertainty based on the raw data collected by the uncertainty data collection module;
[0058] The uncertainty result analysis module analyzes based on the combined standard uncertainty and expanded uncertainty obtained from the above calculations to evaluate the impact degree of uncertainty on the test results;
[0059] When the uncertainty analysis feedback module finds that the uncertainty is too large or there are other problems, it will promptly give feedback to the relevant links. The feedback content includes the specific uncertainty value, possible problems, and recommended improvement measures. When it is found that the combined standard uncertainty of a certain sample exceeds the preset range, the system will prompt the user to check whether there are problems in the experimental operation process, instrument status, or reagent quality (the feedback information is conveyed to the experimental operator or quality management personnel by means of popping up a message box on the system interface, sending an email, or generating a feedback report);
[0060] The uncertainty evaluation module comprehensively evaluates the detection of a certain trace element in the sample based on the data and analysis results provided by the above-mentioned modules, including judging whether the test results meet specific quality control requirements, comparing with the uncertainty limit values stipulated in national standards or industry specifications; comparing with the test results of other methods to evaluate the accuracy of this method (evaluating according to relevant national standards, industry standards, or internal quality control standards of the project).
[0061] The advantages are as follows: By constructing an uncertainty data collection module, an uncertainty calculation module, an uncertainty result analysis module, an uncertainty analysis feedback module, and an uncertainty evaluation module, the present invention realizes the full-process management of the uncertainty evaluation for trace element detection. The uncertainty data collection module is responsible for systematically managing data to ensure the accuracy, integrity, and traceability of the original data related to uncertainty in the entire experimental process. The uncertainty calculation module automatically calculates each uncertainty component and the combined expanded uncertainty based on the collected data, which can not only improve the evaluation efficiency but also help comprehensively identify and control various uncertain factors affecting the detection results. The uncertainty result analysis module analyzes the calculated combined standard uncertainty and expanded uncertainty to evaluate the influence degree of uncertainty on the detection results, further ensuring the reliability of the detection results. When the uncertainty analysis feedback module discovers that the uncertainty is too large or there are other problems, it will promptly feedback to the relevant links, which helps quickly discover and solve problems, thereby improving the overall quality of the detection process. The uncertainty evaluation module comprehensively evaluates the detection of a certain trace element in the sample based on the data and analysis results provided by the above-mentioned various modules. Through the above detection process, the present invention can not only improve the accuracy of trace element detection but also, through the timely feedback and continuous improvement mechanism of the uncertainty analysis feedback module, improve the quality and efficiency of the detection process, and ultimately realize the standardization of the detection method and the continuous optimization of the technology, providing an efficient and reliable uncertainty evaluation method for the field of trace element detection.
[0062] Based on all possible error-causing factors involved in the experimental scheme, draw a cause-and-effect analysis diagram as Figure 2 , that is, the source diagram of the uncertainty in the determination of the content of a certain element by ICP-MS.
[0063] According to Figure 2 Establish a module, including the following unit construction processes:
[0064] The uncertainty data collection module includes a sample mass data unit and an instrument certificate data unit.
[0065] The sample mass data unit includes the sample mass m.
[0066] The instrument certificate data unit includes the calibration certificate of the sample weighing balance, the calibration certificate of the sample weighing balance, and the pipette certificate. Therefore, by consulting the pipette certificate used, the tolerance of the 200 μL adjustable pipette is obtained as: ±0.n%, and the tolerance of the 1000 μL adjustable pipette is: ±0.m%.
[0067] The uncertainty calculation module includes a component measurement unit, a chemical pretreatment method unit, a standard stock solution unit, an instrument measurement unit, and an experiment unit. The component measurement unit calculates the relative uncertainty U of component measurement r(测) .
[0068] The component measurement unit calculates the relative uncertainty U of component measurement based on the component vector of the measurement result r(测) , and its calculation formula is
[0069]
[0070] In the formula, U r(测) represents the relative uncertainty of component measurement, and its unit is %, n represents the total number of uncertainty components, and x i represents the i-th uncertainty component represents the average value of component measurement, and its unit is mg / kg, S a represents the standard deviation of component measurement, and its unit is mg / kg, and U 测(a) represents the relative uncertainty of a component measurement, and its unit is %.
[0071] The chemical pretreatment method unit calculates the uncertainty U of the recovery rate of the chemical pretreatment method r(ec) . Due to incomplete digestion of the sample or loss or contamination of a certain element during the digestion process and loss during the transfer of the digestion solution, the digestion recovery rate of a certain element when using the two-acid (HNO3+HF) digestion method in a high-pressure reactor to digest rock samples as given in the evaluation data of the global laboratory joint measurement is: for example, 98% - 102%. The digestion sampling of the analysis sample in this time is: the two-acid (HNO3+HF) high-pressure reactor method. Therefore, the calculation formula of the uncertainty U of the recovery rate of the chemical pretreatment method r(ec) is
[0072] b + =(102 - 100)% = 2% b - =(100 - 98)% = 2%
[0073]
[0074] In the formula, U r(ec) represents the uncertainty of the recovery rate of the chemical pretreatment method, and its unit is %, and b + represents the maximum deviation of the recovery rate of the chemical pretreatment method, that is, (102 - 100)% = 2%, and b - represents the minimum deviation of the recovery rate of the chemical pretreatment method, that is, (100 - 98)% = 2%.
[0075] The standard stock solution unit checks the uncertainty U of the reference substance by referring to the certificate of the reference substance used in the test r(标)(a) , and the instrument measurement unit calculates the uncertainty U of the electronic balance r(m) and the uncertainty U of the volumetric flask balance r(ml) according to the sample mass m and the verification certificate of the weighing instrument for volumetric solution preparation, and the uncertainty U of the electronic balancer(m) The calculation formula is as follows:
[0076]
[0077] In the formula, U r(m) represents the uncertainty of the electronic balance, and its unit is mg. represents the sample mass, and its unit is mg. The U of the balance given in the calibration certificate of the sample weighing balance used in this experiment (m) = mg (K = 2);
[0078] The uncertainty U of the volumetric balance r(ml) The calculation formula is as follows:
[0079]
[0080] In the formula, U r(ml) represents the uncertainty of the volumetric balance, and its unit is g. represents the sample mass, and its unit is g. The U of this balance given in the calibration certificate of the volumetric balance for the solution used in this experiment (m) = mg (K = 2);
[0081] The tolerance given by the instrument measurement unit by referring to the calibration certificate of the used instrument is ±0.n%, and the instrument uncertainty U of the inductively coupled plasma mass spectrometer is obtained r(仪) , that is, U r(仪) = 0.n%;
[0082] The uncertainty U introduced in the dilution process r(移) , and its calculation formula is as follows: [[ID=4�]]
[0083]
[0084] In the formula, U r(移) represents the uncertainty introduced in the dilution process, ±0.n% represents the tolerance of the 200 μL adjustable pipette by referring to the certificate of the used pipette, and ±0.m% represents the tolerance of the 1000 μL adjustable pipette by referring to the certificate of the used pipette;
[0085] The experimental unit includes calculating the uncertainty U of the sample blank variability r(空白) , calculating the uncertainty U of the acids and water reagents for detection r(试剂) , calculating the uncertainty U of the laboratory temperature and humidity r(E) , calculating the uncertainty U of the container volume r(容) ;
[0086] The uncertainty U of the sample blank variability r(空白), The whole process of pre-experiment treatment was carried out in a super-clean laboratory with a cleanliness of 1000, and the digestion process was carried out in a fume hood with a cleanliness of 100. Therefore, the pollution of elements during the pre-treatment process and the background variation during the placement for inspection can be ignored, and the uncertainty affecting the experimental results: U r(空白) Neglected;
[0087] Uncertainty U of acids and water reagents for detection r(试剂) Since the value is too small to be considered, during the analysis of this sample, the acids used for chemical pre-treatment were BV-Ⅲ grade concentrated nitric acid and hydrofluoric acid produced by Beijing Research Institute of Chemical Reagents purchased, and the concentration of a certain element was <10-8. The reagent water used was 18.2 (megaohm) ultrapure deionized water prepared by a Milli-Q pure water machine. Therefore, the reagent uncertainty: U r(试剂) Neglected;
[0088] Uncertainty U of laboratory temperature and humidity r(E) , During the analysis of this sample, both the chemical pre-treatment and the instrument analysis were carried out in a super-clean chemical laboratory and a purified instrument room with stable temperature and humidity. The temperature and humidity changes in the detection environment were extremely small, and the environmental change uncertainty U affecting the experimental results r(E) Neglected;
[0089] Uncertainty U of container volume r(容) , In this experiment, the mass method was used, and the dilution and volume fixation processes of the sample were not affected by the container volume.
[0090] The uncertainty evaluation module conducts the evaluation of the expanded uncertainty U (a) in the following way:
[0091] (1) Calculate the relative uncertainty of all uncertainty components of the influencing factors during the detection process. The calculation formula is:
[0092]
[0093] (2) The calculation formula for the combined standard uncertainty U c(合成) is:
[0094]
[0095] In the formula, Uc (combined) represents the combined standard uncertainty, and its unit is mg / kg. represents the average value of the combined measurement result, and its unit is mg / kg. Urc (total) represents the relative uncertainty of all uncertainty components of the influencing factors during the detection process, and its unit is %.
[0096] (3) The coverage factor k for a 95% confidence probability is 2. Multiply the combined standard uncertainty by the coverage factor to calculate the expanded uncertainty U of the measurement result(a) , and its calculation formula is:
[0097] U (a) = k × U c(合成)
[0098] In the formula, U (a) represents the expanded uncertainty U (a) , whose unit is mg / kg, k represents the coverage factor for a 95% confidence probability, and k = 2.
[0099] A method for evaluating the uncertainty of trace element detection based on ICP-MS includes the following steps:
[0100] S1. Data collection: Collect the original data related to uncertainty in the entire experimental process through the uncertainty data collection module, including sample information, experimental conditions, personnel information, and detection time. By structuring the input and storage of the original data in the entire experimental process, the accuracy, integrity, and traceability of the data are ensured, which helps to improve the reliability of the trace element detection results, thereby providing more accurate data support for subsequent analysis and decision-making;
[0101] S2. Data entry and storage: Enter and store the collected data in a structured manner in the system database to ensure the accuracy, integrity, and traceability of the data;
[0102] S3. Uncertainty calculation: Use the uncertainty calculation module to calculate each uncertainty component and the combined expanded uncertainty based on the collected original data. Automatically calculate each uncertainty component and the combined expanded uncertainty through the uncertainty calculation module, which enhances the systematicness of the uncertainty evaluation of the method of the present invention. It can not only improve the evaluation efficiency but also help to more comprehensively identify and control various uncertain factors affecting the detection results;
[0103] S4. Result analysis: Analyze the combined standard uncertainty and expanded uncertainty calculated through the uncertainty result analysis module to evaluate the influence degree of the uncertainty on the detection results;
[0104] S5. Feedback and improvement: When the uncertainty is too large or there are other problems, the uncertainty analysis feedback module will promptly feedback to the relevant links. The feedback content includes the specific uncertainty value, possible problems, and recommended improvement measures. By using the uncertainty analysis feedback module to promptly discover that the uncertainty is too large or other problems, and feedback the specific value, possible problems, and improvement measures to the relevant personnel, this timely feedback mechanism helps to quickly discover and solve problems, thereby improving the overall quality and efficiency of the detection process;
[0105] S6. Comprehensive evaluation: The uncertainty evaluation module comprehensively evaluates the detection of a certain trace element in the sample based on the data and analysis results provided by each of the above modules, including determining whether the detection results meet specific quality control requirements, comparing with the uncertainty limits specified in national standards or industry specifications, comparing with the detection results of other methods, and evaluating the accuracy of this method. The comprehensive evaluation of the detection results through the uncertainty evaluation module, including comparison with national standards or industry specifications and accuracy evaluation with other methods, helps to standardize the detection method, and at the same time promotes the continuous optimization and progress of the detection technology through comparison and evaluation.
[0106] Advantages: The present invention provides a comprehensive, systematic and efficient method for evaluating the uncertainty of trace element detection. This method can ensure the accuracy and reliability of data, improve the systematicness of uncertainty evaluation, timely feedback and improve problems in the detection process, and promote the standardization and continuous optimization of the detection technology, thereby improving the overall quality of trace element detection.
[0107] Although the embodiments of the present invention have been shown and described, it will be understood by those of ordinary skill in the art that various changes, modifications, substitutions and variations can be made to these embodiments without departing from the principles and spirit of the present invention, and the scope of the present invention is defined by the appended claims and their equivalents.
Claims
1. An uncertainty evaluation system for trace element detection based on ICP-MS, characterized in that, It includes an uncertainty data collection module, an uncertainty calculation module, an uncertainty result analysis module, an uncertainty analysis feedback module, and an uncertainty evaluation module; The uncertainty data collection module collects the original data related to uncertainty in the entire experimental process and supports structured input and storage; The uncertainty calculation module automatically calculates each uncertainty component and the combined expanded uncertainty based on the original data collected by the uncertainty data collection module; The uncertainty result analysis module analyzes based on the combined standard uncertainty and expanded uncertainty obtained from the above calculations to evaluate the influence degree of uncertainty on the test results; When the uncertainty analysis feedback module finds that the uncertainty is too large or there are other problems, it will promptly give feedback to the relevant links; The uncertainty evaluation module comprehensively evaluates the detection of a certain trace element in the sample based on the data and analysis results provided by the above-mentioned various modules.
2. The uncertainty evaluation system for trace element detection based on ICP-MS according to claim 1, wherein: The uncertainty data collection module includes a sample mass data unit and an instrument certificate data unit.
3. A trace element detection uncertainty evaluation system based on ICP-MS according to claim 2, characterized in that: The sample mass data unit includes the sample mass m.
4. The uncertainty evaluation system for trace element detection based on ICP-MS according to claim 2, characterized in that: The instrument certificate data unit includes the verification certificate of the sample weighing balance, the verification certificate of the sample weighing balance, and the pipette certificate. By consulting the pipette certificate used, the tolerances of the 200 μL adjustable pipette are: ±0.n%, and the tolerances of the 1000 μL adjustable pipette are: ±0.m%.
5. A trace element detection uncertainty evaluation system based on ICP-MS according to claim 1, characterized in that: The uncertainty calculation module includes a component measurement unit, a chemical pretreatment method unit, a standard stock solution unit, an instrument measurement unit, and an experiment unit.
6. The uncertainty evaluation system for trace element detection based on ICP-MS according to claim 5, wherein: The component measurement unit calculates the relative uncertainty U of component measurement based on the component vector of the measurement result r(测) , and its calculation formula is as follows: In the formula, U r(测) represents the relative uncertainty of component measurement, n represents the total number of uncertainty components, and x i represents the i-th uncertainty component, represents the average value of component measurement, S a represents the standard deviation of component measurement, and U 测(a) represents the relative uncertainty of a-component measurement.
7. A trace element detection uncertainty evaluation system based on ICP-MS according to claim 5, characterized in that: The chemical pretreatment method unit calculates the uncertainty U of the recovery rate of the chemical pretreatment method r(ec) , the digestion recovery rate of a certain element is: for example, 98% - 102%, and its calculation formula is: b + =(102 - 100)% = 2%b - =(100 - 98)% = 2% In the formula, U r(ec) represents the uncertainty of the recovery rate of the chemical pretreatment method, and b + represents the maximum deviation of the recovery rate of the chemical pretreatment method, that is, (102 - 100)% = 2%, and b - represents the minimum deviation of the recovery rate of the chemical pretreatment method, that is, (100 - 98)% = 2%.
8. An uncertainty evaluation system for trace element detection based on ICP-MS according to claim 5, characterized in that: The standard stock solution unit obtains the uncertainty U of the reference substance by referring to the certificate of the reference substance for detection used in the detection r(标)(a) , the instrument measurement unit calculates the uncertainty U of the electronic balance r(m) and the uncertainty U of the volumetric balance r(ml) according to the sample mass m and the verification certificate of the weighing instrument for volumetric solution weighing. The calculation formula of the uncertainty U of the electronic balance r(m) is as follows: In the formula, U r(m) represents the uncertainty of the electronic balance, represents the sample mass. The balance U (m) =mg (K = 2) given in the verification certificate of the sample weighing balance used in this experiment; The uncertainty U of the volumetric balance r(ml) is calculated by the following formula: In the formula, U r(ml) represents the uncertainty of the volumetric balance, represents the sample mass. The verification certificate of the volumetric balance used in this experiment gives the U (m) of this balance as = mg (K = 2); The instrument measurement unit obtains the instrument uncertainty U of the inductively coupled plasma mass spectrometer by referring to the tolerance of ±0.n% given in the verification certificate of the instrument used r(仪) , that is, U r(仪) = 0.n%; The uncertainty U introduced by the dilution process r(移) , and its calculation formula is as follows: In the formula, U r(移) represents the uncertainty introduced by the dilution process, ±0.n% represents the tolerance of the 200 μL adjustable pipette in the pipette certificate used, and ±0.m% represents the tolerance of the 1000 μL adjustable pipette in the pipette certificate used; The experimental unit includes calculating the uncertainty U of the variability of the sample blank r(空白) , calculating the uncertainty U of the acid and water reagents for detection r(试剂) , calculating the uncertainty U of the laboratory temperature and humidity r(E) , calculating the uncertainty U of the container volume r(容) , and consider whether it can be ignored depending on the laboratory situation.
9. A trace element detection uncertainty evaluation system based on ICP-MS according to claim 5, characterized in that: The uncertainty evaluation module conducts the evaluation of the expanded uncertainty U (a) , and the evaluation method is as follows: (1) Calculate the relative uncertainty of all uncertainty components of the influencing factors in the detection process, where U r(空白) , U r(试剂) , U r(E) and U r(容) are neglected, and its calculation formula is: (2) Combined standard uncertainty U c(合成) The calculation formula is as follows: In the formula, U c(合成) represents the combined standard uncertainty, represents the mean value of the combined measurement result, U rc(总) represents the relative uncertainty of all the uncertainty components of the influencing factors in the detection process; (3) The coverage factor k for a 95% confidence probability is 2. The expanded uncertainty U of the measurement result is obtained by multiplying the combined standard uncertainty by the coverage factor. (a) , and its calculation formula is: U (a) = k × U c(合成) In the formula, U (a) represents the expanded uncertainty U (a) , k represents the coverage factor for a 95% confidence probability, and k = 2.
10. A method for evaluating the uncertainty of trace element detection based on ICP-MS, characterized in that, It includes the following steps: S1. Data collection: Collect the original data related to uncertainty in the entire experimental process through the uncertainty data collection module; S2. Data entry and storage: Enter and store the collected data in a structured manner in the system database; S3. Uncertainty calculation: Use the uncertainty calculation module to calculate each uncertainty component and the combined expanded uncertainty based on the collected original data; S4. Result analysis: Analyze the combined standard uncertainty and expanded uncertainty obtained from the calculation through the uncertainty result analysis module; S5. Feedback and improvement: When the uncertainty is too large or there are other problems, the uncertainty analysis feedback module will promptly give feedback to the relevant links; S6. Comprehensive evaluation: The uncertainty evaluation module comprehensively evaluates the detection of a certain trace element in the sample based on the data and analysis results provided by the above-mentioned various modules.