Mercury content detection method
By combining preliminary quantification with X-ray spectroscopy and sealing with a capped funnel and constant temperature water bath heating, along with inductively coupled plasma atomic emission spectrometry (ICP-AES) for detection, the instability and safety issues of mercury content detection in traditional chemical titration methods have been resolved, achieving efficient and safe mercury content detection.
Patent Information
- Application Number
- CN202511251070.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-09-03
- Publication Date
- 2025-11-11
AI Technical Summary
Traditional chemical titration methods for detecting mercury content in mercury-containing acid sludge during smelting are cumbersome, prone to mercury volatilization, affecting the stability and accuracy of test results, and endangering the health of operators.
X-ray spectroscopy was used for preliminary quantitative analysis of the sample. The bottle mouth was sealed with a capped funnel and decomposed by heating in a constant temperature water bath. A standard curve was plotted using inductively coupled plasma atomic emission spectrometry for detection.
It improves the accuracy and reliability of detection, avoids mercury volatilization loss, ensures operational safety and result stability, and reduces detection costs.
Smart Images
Figure CN120927786A_ABST
Abstract
Description
Technical Field
[0001] This application relates to the field of mercury detection technology, and in particular to a method for detecting mercury content. Background Technology
[0002] During the smelting process, it is necessary to test the mercury content of mercury-containing acid mud samples to ensure the safety of the products and their compliance with production standards.
[0003] Because the mercury content in mercury-containing acid sludge is low, and because mercury is volatile, the traditional chemical titration method for mercury content detection has significant technical drawbacks. Specifically, when performing traditional chemical titration, the sample needs to be decomposed to a near-dry state, the operation is complicated, the titration process is in an open environment, which leads to a large amount of mercury volatilization, making it difficult to guarantee the stability and accuracy of the analytical results, and also seriously endangering the health of the operators. Summary of the Invention
[0004] To address or partially address the problems existing in related technologies, this application provides a method for detecting mercury content, which can effectively ensure the stability and accuracy of the detection results.
[0005] This application provides a method for detecting mercury content, the method comprising: S1: Weigh the sample to be tested into an Erlenmeyer flask, add aqua regia, and seal the flask mouth with distilled water using a capped funnel; S2: After the conical flask has been heated and decomposed in a water bath, pour the solution from the capped funnel back into the conical flask and dilute it to the final volume. S3: Prepare a mercury standard solution, plot a standard curve using an inductively coupled plasma atomic emission spectrometer, and determine the mercury content of the sample.
[0006] Optionally, in some implementations of the first aspect: The method involves taking the sample to be tested into an Erlenmeyer flask, specifically including: Before sample analysis, X-ray spectrometer is used to perform preliminary quantification of the sample to be tested, and the sample to be tested is weighed according to the preliminary measured mercury content.
[0007] Optionally, in some implementations of the first aspect: The sample to be tested should be weighed based on the preliminary measured mercury content, specifically including: For the sample to be tested with a preliminary mercury content of less than 10%, weigh 1.0000g. For the sample to be tested with a preliminary mercury content of 10-20%, weigh 0.5000g. For the sample to be tested with a preliminary mercury content of 20-30%, weigh 0.2000g. For samples with a preliminary mercury content of 30% or higher, weigh 0.1000g.
[0008] Optionally, in some implementations of the first aspect: Based on the weight of the sample to be tested, add 15-30 mL of aqua regia to the conical flask containing the sample.
[0009] Optionally, in some implementations of the first aspect: Add 10-50 mL of distilled water to the funnel, depending on its size.
[0010] Optionally, in some implementations of the first aspect: The water bath heating is a constant temperature water bath with a temperature of 90℃ and a heating decomposition time of 40-60 minutes.
[0011] Optionally, in some implementations of the first aspect: The solution in the capped funnel should be poured back into the conical flask and diluted to volume, specifically including: Dilute the solution to 100-200 mL in a container, or dilute it 10-20 times depending on the size of the capped funnel.
[0012] Optionally, in some implementations of the first aspect: The diluent for this volumetric dilution is dilute nitric acid with a concentration of 5%.
[0013] Optionally, in some implementations of the first aspect: The preparation of the mercury standard solution specifically includes: Based on the mercury content in the raw materials, prepare mercury standard solutions, specifically including: preparing mercury standard solutions of 0, 5, 10, 20, 30, 40, and 50 ug / mL.
[0014] Optionally, in some implementations of the first aspect: The standard curve was plotted using inductively coupled plasma atomic emission spectrometry (ICP-AES), and the mercury content of the sample was determined, specifically including: Using an inductively coupled plasma atomic emission spectrometer (ICP-AES), the mercury standard solution was measured sequentially at selected wavelengths, and a standard curve was plotted under set conditions. Finally, the sample to be tested was measured using an ICP-AES.
[0015] The technical solution provided in this application may include the following beneficial effects: This application uses an X-ray spectrometer to perform preliminary quantification of the sample to be tested, which can quickly obtain the mercury content range of the sample to be tested. The sample to be tested is weighed based on the preliminary mercury content, which can ensure the accuracy and reliability of subsequent detection.
[0016] This application utilizes a constant-temperature water bath for heating, ensuring complete decomposition of the sample. Simultaneously, by pouring the solution from the capped funnel back into the conical flask, the mercury compounds that have volatilized after heating can be collected, preventing mercury content loss and further ensuring the stability and accuracy of subsequent test results.
[0017] This application utilizes a mercury standard solution prepared and detected using an inductively coupled plasma atomic emission spectrometer (ICP-AES). This eliminates the need for manual titration, provides excellent anti-interference capabilities, and enables accurate determination of mercury content, effectively ensuring the stability and accuracy of the test results.
[0018] It should be understood that the above general description and the following detailed description are exemplary and explanatory only, and do not limit this application. Attached Figure Description
[0019] The above and other objects, features and advantages of this application will become more apparent from the more detailed description of exemplary embodiments thereof in conjunction with the accompanying drawings, wherein the same reference numerals generally represent the same components in the exemplary embodiments thereof.
[0020] Figure 1 This is a schematic diagram of the process structure of a mercury content detection method in an embodiment of this application. Detailed Implementation
[0021] Embodiments of this application will now be described in more detail with reference to the accompanying drawings. While embodiments of this application are shown in the drawings, it should be understood that this application may be implemented in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided to make this application more thorough and complete, and to fully convey the scope of this application to those skilled in the art.
[0022] It should be understood that although the terms "first," "second," "third," etc., may be used in this application to describe various information, this information should not be limited to these terms. These terms are only used to distinguish information of the same type from one another. For example, without departing from the scope of this application, first information may also be referred to as second information, and similarly, second information may also be referred to as first information. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of this application, "multiple" means two or more, unless otherwise explicitly specified.
[0023] In the description of this application, it should be understood that the terms "length", "width", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings, and are only for the convenience of describing this application and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of this application.
[0024] Unless otherwise expressly specified and limited, the terms "installation," "connection," "linking," and "fixing," etc., should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral part; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; they can refer to the internal communication of two components or the interaction between two components. Those skilled in the art can understand the specific meaning of the above terms in this application according to the specific circumstances.
[0025] During the smelting process, it is necessary to test the mercury content of mercury-containing acid mud samples to ensure the safety of the products and their compliance with production standards.
[0026] Because the mercury content in mercury-containing acid sludge is low, and because mercury is volatile, the traditional chemical titration method for mercury content detection has significant technical drawbacks. Specifically, when performing traditional chemical titration, the sample needs to be decomposed to a near-dry state, the operation is complicated, the titration process is in an open environment, which leads to a large amount of mercury volatilization, making it difficult to guarantee the stability and accuracy of the analytical results, and also seriously endangering the health of the operators.
[0027] To address the aforementioned issues, this application provides a method for detecting mercury content, which effectively ensures the stability and accuracy of the detection results.
[0028] The technical solutions of the embodiments of this application are described in detail below with reference to the accompanying drawings.
[0029] Figure 1 This is a schematic diagram of the process structure of a mercury content detection method in an embodiment of this application.
[0030] See Figure 1 A method for detecting mercury content, the method comprising: S1: Weigh the sample to be tested into an Erlenmeyer flask, add aqua regia, and seal the flask mouth with distilled water using a capped funnel.
[0031] Specifically: Before sample determination, the sample to be tested is preliminarily quantified using an X-ray spectrometer, and the sample to be tested is weighed according to the preliminarily measured mercury content.
[0032] The sample to be tested is weighed based on the preliminary measured mercury content, specifically including: For the sample to be tested with a preliminary mercury content of less than 10%, weigh 1.0000g. For the sample to be tested with a preliminary mercury content of 10-20%, weigh 0.5000g. For the sample to be tested with a preliminary mercury content of 20-30%, weigh 0.2000g. For samples with a preliminary mercury content of 30% or higher, weigh 0.1000g.
[0033] In this embodiment, by using an X-ray spectrometer to perform preliminary quantification of the sample, the mercury content range of the sample can be quickly obtained. The sample can be weighed based on the preliminary mercury content, which ensures the accuracy and reliability of subsequent detection.
[0034] Specifically: Add 15-30 mL of aqua regia to the conical flask containing the sample, based on the weight of the sample to be tested.
[0035] In this embodiment, 30 mL of aqua regia is added when the sample weight is 1.0000 g; 20 mL of aqua regia is added when the sample weight is 0.5000 g; 15 mL of aqua regia is added when the sample weight is 0.2000 g; and 10 mL of aqua regia is added when the sample weight is 0.1000 g. By establishing a precise ratio between sample weight and aqua regia dosage, the reaction decomposition efficiency can be ensured, operational safety can be improved, and reagents can be saved and detection costs reduced by controlling the dosage.
[0036] Specifically: Add 10-50 mL of distilled water to the funnel, depending on its size.
[0037] In this embodiment, for mercury content less than 10%, add 10 mL (minimum sealing amount); for mercury content between 10% and 30%, add 30 mL; for mercury content greater than 30%, add 50 mL. Using a capped funnel with distilled water ensures a good seal, preventing the volatilization of mercury compounds formed by thermal decomposition into the operating environment, thus guaranteeing the stability and accuracy of subsequent test results.
[0038] S2: After the conical flask has been heated and decomposed in a water bath, pour the solution from the capped funnel back into the conical flask and dilute it to the final volume.
[0039] Specifically: the water bath heating is a constant temperature water bath with a temperature of 90℃ and a heating decomposition time of 40-60 minutes.
[0040] Specifically: bring the solution to a volume of 100-200 mL in a container, and dilute it 10-20 times depending on the size of the capped funnel.
[0041] Specifically: the diluent for this volumetric dilution is dilute nitric acid with a concentration of 5%.
[0042] In this embodiment, heating in a constant-temperature water bath ensures complete decomposition of the sample. Simultaneously, by pouring the solution from the capped funnel back into the conical flask, the mercury compounds that have volatilized after heating can be collected, avoiding loss of mercury content and further ensuring the stability and accuracy of subsequent test results.
[0043] S3: Prepare a mercury standard solution, plot a standard curve using an inductively coupled plasma atomic emission spectrometer, and determine the mercury content of the sample.
[0044] Specifically: the preparation of the mercury standard solution includes: Based on the mercury content in the raw materials, prepare mercury standard solutions, specifically including: preparing mercury standard solutions of 0, 5, 10, 20, 30, 40, and 50 ug / mL.
[0045] Specifically: using an inductively coupled plasma atomic emission spectrometer, the mercury standard solution was measured sequentially at selected wavelengths, and the conditions were set to plot a standard curve. Finally, the sample to be tested was measured using an inductively coupled plasma atomic emission spectrometer.
[0046] In this embodiment, a mercury standard solution is prepared and detected using an inductively coupled plasma atomic emission spectrometer. This eliminates the need for manual titration, provides good anti-interference capabilities, and enables accurate determination of mercury content, effectively ensuring the stability and accuracy of the detection results.
[0047] The technical solution provided in this application may include the following beneficial effects: This application uses an X-ray spectrometer to perform preliminary quantification of the sample to be tested, which can quickly obtain the mercury content range of the sample to be tested. The sample to be tested is weighed based on the preliminary mercury content, which can ensure the accuracy and reliability of subsequent detection.
[0048] This application utilizes a constant-temperature water bath for heating, ensuring complete decomposition of the sample. Simultaneously, by pouring the solution from the capped funnel back into the conical flask, the mercury compounds that have volatilized after heating can be collected, preventing mercury content loss and further ensuring the stability and accuracy of subsequent test results.
[0049] This application utilizes a mercury standard solution prepared and detected using an inductively coupled plasma atomic emission spectrometer (ICP-AES). This eliminates the need for manual titration, provides excellent anti-interference capabilities, and enables accurate determination of mercury content, effectively ensuring the stability and accuracy of the test results.
[0050] Finally, it should be noted that in this document, relationships such as "first" and "second" are used merely to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "include," "contain," or any other variations are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such a process, method, article, or apparatus.
[0051] The units described as separate components may or may not be physically separate. The components shown as units may or may not be physical units; that is, they may be located in one place or distributed across multiple network units. Some or all of the units can be selected to achieve the purpose of this embodiment according to actual needs.
[0052] Furthermore, the functional units in the various embodiments of this application can be integrated into one processing unit, or each unit can exist physically separately, or two or more units can be integrated into one unit. The integrated unit can be implemented in hardware or as a software functional unit.
[0053] If the integrated unit is implemented as a software functional unit and sold or used as an independent product, it can be stored in a computer-readable storage medium. Based on this understanding, the technical solution of this application, in essence, or the part that contributes to the prior art, or all or part of the technical solution, can be embodied in the form of a software product. This computer software product is stored in a storage medium and includes several instructions to cause a computer device (which may be a personal computer, a server, or a network device, etc.) to execute all or part of the steps of the methods described in the various embodiments of this application.
[0054] The various embodiments of this application have been described above. These descriptions are exemplary and not exhaustive, nor are they limited to the disclosed embodiments. Many modifications and variations will be apparent to those skilled in the art without departing from the scope and spirit of the described embodiments. The terminology used herein is chosen to best explain the principles, practical application, or improvement of the technology in the market, or to enable others skilled in the art to understand the embodiments disclosed herein.
Claims
1. A method for detecting mercury content, characterized in that, The detection method includes: S1: Weigh the sample to be tested into an Erlenmeyer flask, add aqua regia, and seal the flask mouth with distilled water using a capped funnel; S2: After the conical flask has been heated and decomposed in a water bath, pour the solution from the capped funnel back into the conical flask and dilute it to the final volume. S3: Prepare a mercury standard solution, plot a standard curve using an inductively coupled plasma atomic emission spectrometer, and determine the mercury content of the sample.
2. The method for detecting mercury content according to claim 1, characterized in that: The weighing of the sample to be tested into the conical flask specifically includes: Before sample determination, X-ray spectrometer is used to perform preliminary quantification of the sample to be tested, and the sample to be tested is weighed according to the preliminary measured mercury content.
3. The method for detecting mercury content according to claim 2, characterized in that: The weighing of the sample to be tested based on the preliminary measured mercury content specifically includes: For the sample to be tested with a preliminary mercury content of less than 10%, weigh 1.0000g. For the sample to be tested with a preliminary mercury content of 10-20%, weigh 0.5000g. For the sample to be tested with a preliminary mercury content of 20-30%, weigh 0.2000g. For samples with a preliminary mercury content of 30% or higher, weigh 0.1000g.
4. The method for detecting mercury content according to claim 3, characterized in that: Based on the weight of the sample to be tested, add 15-30 mL of aqua regia to the conical flask containing the sample.
5. The method for detecting mercury content according to claim 1 or 4, characterized in that: Add 10-50 mL of distilled water to the funnel, depending on its size.
6. The method for detecting mercury content according to claim 5, characterized in that: The water bath heating is a constant temperature water bath with a temperature of 90℃ and a heating decomposition time of 40-60 minutes.
7. The method for detecting mercury content according to claim 6, characterized in that: The step of pouring the solution from the capped funnel back into the conical flask and then diluting it to a final volume includes: Dilute the solution to 100-200 mL in a container, or dilute it 10-20 times depending on the size of the capped funnel.
8. The method for detecting mercury content according to claim 7, characterized in that: The diluent used for volumetric dilution is dilute nitric acid with a concentration of 5%.
9. The method for detecting mercury content according to claim 8, characterized in that: The preparation of the mercury standard solution specifically includes: Based on the mercury content in the raw materials, prepare mercury standard solutions, specifically including: preparing mercury standard solutions of 0, 5, 10, 20, 30, 40, and 50 ug / mL.
10. The method for detecting mercury content according to claim 9, characterized in that: The process of using inductively coupled plasma atomic emission spectrometry to plot a standard curve and measuring the mercury content of the sample specifically includes: Using an inductively coupled plasma atomic emission spectrometer (ICP-AES), the mercury standard solution was measured sequentially at selected wavelengths, and a standard curve was plotted under set conditions. Finally, the sample to be tested was measured using an ICP-AES.