Matrix matching method in beryllium chemical analysis wet analysis

Abstract

The invention discloses a matrix matching method in beryllium chemical analysis and wet analysis, and belongs to the technical field of beryllium chemical analysis. The method comprises the following steps: determining a beryllium chemical analysis wet analysis method; extracting elements associated with the preparation of the standard working solution in the beryllium chemical analysis wet analysis method; beryllium hydroxide or beryllium hydroxide and a coexisting matrix are equivalently placed in a plurality of beakers, the beakers are wetted with secondary water, then dissolving acids of the same type and the same volume are added, and after the heating reaction is finished, a first mixed solution series is obtained; adding to-be-detected elements with corresponding content gradients into each first mixed solution in the first mixed solution series to obtain a second mixed solution series; respectively transferring each second mixed solution in the second mixed solution series into a corresponding volumetric flask and fixing the volume to obtain a third mixed solution series as a standard working solution series; and drawing a standard curve. High-purity beryllium is replaced with high-purity beryllium hydroxide, and the problem that high-purity beryllium is difficult to obtain is solved.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of beryllium chemical analysis, and particularly relates to a matrix matching method in beryllium chemical analysis wet analysis. BACKGROUND

[0002] Beryllium is a rare light metal with excellent performance, and is known for its low density, high specific stiffness, high specific strength and excellent thermal performance. It is widely used as a functional and structural material in many key fields, and its alloy is also an indispensable key material in the high-tech field due to its unique mechanical properties, physical characteristics and excellent processing characteristics, and shows important application value in many fields. The analysis and detection of beryllium resources is a key link to ensure product quality and performance, which not only helps to accurately evaluate product composition, structure, performance and the like, so as to ensure that the product meets the standard requirements, but also helps to improve product quality, optimize production process, reduce cost, promote new material research and development and the like.

[0003] With the progress of analysis technology, traditional volumetric method, gravimetric method and colorimetric method and the like are gradually replaced by inductively coupled plasma optical emission spectrometry (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS) with higher efficiency. Both ICP-OES and ICP-MS are instrumental methods, and belong to relative analysis method. The key is to control the true consistency of the analysis conditions, eliminate the adverse effects, and adjust the measurement environment and equipment parameters to obtain a more accurate measurement system. At the same time, it also belongs to "wet analysis", that is, the analysis object is required to be in a solution state. Therefore, the sample generally needs to be decomposed and treated first to convert the measured component into a soluble form to prepare a test solution.

[0004] In relative analysis and wet analysis, effectively eliminating matrix effect, matching the viscosity difference between test solution and standard solution, and changing the aerosol generation efficiency of each solution to improve the accuracy and reliability of the analysis results are key links in measurement. It is the most simple and efficient to eliminate matrix effect by using matrix matching method. In the national standards for copper, steel, aluminum and other metal analysis, high-purity metal is dissolved to meet the matrix matching in wet analysis. However, in the field of beryllium chemical analysis, high-purity beryllium is difficult to obtain, expensive and difficult to meet the application requirements of beryllium chemical analysis, so it is difficult to realize a simple and efficient matrix matching method as in the copper, steel, aluminum and other industries. SUMMARY

[0005] To solve the above technical problems, the application provides a method for matrix matching in beryllium chemical analysis wet analysis, which is based on the principle of acid-base neutralization, uses high-purity beryllium hydroxide to replace high-purity beryllium, avoids the problem that high-purity beryllium is difficult to obtain, and realizes the same matrix matching effect as high-purity beryllium dissolution in the chemical behavior and state of the standard series solution by using high-purity beryllium hydroxide and corresponding dissolving acid to generate matrix beryllium salt and water in the configuration of the series standard solution required for ICP-OES and ICP-MS analysis.

[0006] The application provides a method for matrix matching in beryllium chemical analysis wet analysis, which comprises the following steps:

[0007] Step S1, determining a beryllium chemical analysis wet analysis method;

[0008] Step S2, extracting elements associated with the preparation of a standard working solution in the beryllium chemical analysis wet analysis method;

[0009] Step S3, putting an equal amount of beryllium hydroxide or beryllium hydroxide and coexisting matrix into a plurality of beakers, respectively adding the same kind and volume of dissolving acid after wetting with secondary water, and obtaining a first mixed solution series after heating and reaction;

[0010] Step S4, adding corresponding content gradients of to-be-measured elements into each first mixed solution in the first mixed solution series, respectively, to obtain a second mixed solution series;

[0011] Step S5, transferring each second mixed solution in the second mixed solution series into a corresponding volumetric flask and constant volume to obtain a third mixed solution series as a standard working solution series;

[0012] Step S6, using the standard working solution series to draw a standard curve.

[0013] According to the method for matrix matching in beryllium chemical analysis wet analysis, the elements in step S2 include the amount of beryllium, the amount of coexisting matrix, the type of dissolving acid, the amount of dissolving acid, the type of to-be-measured element, the content gradient of to-be-measured element, the number of standard points of the standard working solution series, and the constant volume of a single standard point.

[0014] According to the method for matrix matching in beryllium chemical analysis wet analysis, the type of to-be-measured element includes at least one of iron, aluminum, chromium, silicon, magnesium, zinc, copper, manganese, nickel, lead, calcium, molybdenum, titanium, zirconium, silver, cadmium, lithium, cobalt, boron, samarium, europium, gadolinium, dysprosium, and uranium.

[0015] According to the method for matrix matching in beryllium chemical analysis wet analysis, the upper limit of the content gradient of to-be-measured element is 100 mu g / mL.

[0016] According to the method for matrix matching in beryllium chemical analysis wet analysis provided in the application, in the step S5, the number of the volumetric flasks is equal to the number of the standard points; the nominal capacity of the plurality of volumetric flasks is equal, and the nominal capacity of the volumetric flasks is equal to the constant volume of the single standard point.

[0017] According to the method for matrix matching in beryllium chemical analysis wet analysis provided in the application, in the step S3, the amount of beryllium hydroxide in each beaker is 4.78 times of the amount of beryllium.

[0018] According to the method for matrix matching in beryllium chemical analysis wet analysis provided in the application, in the step S1, the application object of the beryllium chemical analysis wet analysis method includes metal beryllium and beryllium alloy.

[0019] According to the method for matrix matching in beryllium chemical analysis wet analysis provided in the application, in the step S1, the type of the beryllium chemical analysis wet analysis method includes a standard method or a non-standard method.

[0020] According to the method for matrix matching in beryllium chemical analysis wet analysis provided in the application, in the step S1, the principle of the beryllium chemical analysis wet analysis method includes ICP-OES method and ICP-MS method.

[0021] The scheme provided in the application has the following technical effects:

[0022] According to the acid-base neutralization principle, the high-purity beryllium hydroxide is used to replace the high-purity beryllium, the problem of difficult to obtain the high-purity beryllium is avoided, in the configuration of the series of standard solutions required in ICP-OES and ICP-MS analysis, the high-purity beryllium hydroxide and the corresponding dissolving acid are used to generate the matrix beryllium salt and water, and the same matrix matching effect as the high-purity metal beryllium dissolution is realized in the chemical behavior and state of the standard series solution.

[0023] In addition, since the high-purity beryllium hydroxide is more easily obtained than the high-purity metal beryllium, the application solves the key problem of impurity analysis in metal beryllium chemical analysis in production practice, and also solves similar problems in related beryllium alloy chemical analysis, and promotes the technical progress of beryllium and beryllium alloy chemical analysis.

[0024] In addition, the application solves the problem of matrix matching in domestic beryllium chemical analysis wet analysis, improves the work efficiency, reduces the difficulty of daily analysis work, improves the adaptability of analysis, is conducive to establishing the traceability of material metrology, meets the related method matching requirements of the further promotion of beryllium chemical analysis standardization work and equipment localization substitution work. Specific embodiments

[0025] In order to make the purposes, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below. Obviously, the described embodiments are only some of the embodiments of the present application but not all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative efforts belong to the scope of protection of the present application.

[0026] The abbreviations and key terms involved in the embodiments are defined as follows:

[0027] Standard method: a detection method formulated and published by an authoritative organization or a standardization organization.

[0028] Non-standard method: a detection method not approved by an international, regional or national standard organization, including a laboratory self-built method, an improved standard method or a method published by a recognized technical organization.

[0029] The embodiments provide a method for matrix matching in beryllium chemical analysis wet analysis, and the method comprises the following steps:

[0030] In step S1, a beryllium chemical analysis wet analysis method is determined. The application objects of the beryllium chemical analysis wet analysis method include metal beryllium and beryllium alloys. The types of the beryllium chemical analysis wet analysis method include standard methods or non-standard methods. The principles of the beryllium chemical analysis wet analysis method include ICP-OES method and ICP-MS method.

[0031] In step S2, elements associated with the preparation of a standard working solution in the beryllium chemical analysis wet analysis method are extracted.

[0032] In some embodiments, in the step S2, the elements include the amount of beryllium, the amount of coexisting matrix, the type of dissolving acid, the amount of dissolving acid, the type of measured element, the content gradient of measured element, the number of standard points of a standard working solution series and the constant volume of a single standard point.

[0033] Preferably, the type of measured element can be extended and includes but is not limited to at least one of iron, aluminum, chromium, silicon, magnesium, zinc, copper, manganese, nickel, lead, calcium, molybdenum, titanium, zirconium, silver, cadmium, lithium, cobalt, boron, samarium, europium, gadolinium, dysprosium and uranium.

[0034] Preferably, the content gradient range of the measured element can be extended, and the upper limit is 100 μg / mL.

[0035] Step S3, according to the procedure requirements of the beryllium chemical analysis wet analysis method, the same amount of beryllium hydroxide or beryllium hydroxide and coexisting matrix is placed in multiple beakers, and after being wetted with secondary water, the same kind and volume of dissolved acid is added, and after heating reaction, a first mixed solution series is obtained. The amount of beryllium hydroxide in each beaker is 4.78 times the amount of beryllium.

[0036] Preferably, when the dissolved acid is added, the beaker with beryllium hydroxide or beryllium hydroxide and coexisting matrix is semi-sealed with a watch glass; after the dissolved acid is added, the inner wall of the beaker and the watch glass is washed with secondary water.

[0037] Specifically, the mass fraction of beryllium hydroxide is not less than 99.99%; when applied to ICP-OES method analysis, the mass fraction of the measured element in beryllium hydroxide is not more than 0.0010%, and when applied to ICP-MS method analysis, the mass fraction of the measured element in beryllium hydroxide is not more than 0.0001%.

[0038] Specifically, when the application object of the beryllium chemical analysis wet analysis method is metallic beryllium, the coexisting matrix addition amount is 0; when the application object of the beryllium chemical analysis wet analysis method is beryllium alloy, the coexisting matrix addition amount is not 0.

[0039] Step S4, a corresponding content gradient of the measured element is added to each first mixed solution in the first mixed solution series to obtain a second mixed solution series.

[0040] Step S5, each second mixed solution in the second mixed solution series is transferred to a corresponding volumetric flask and is constant volume to obtain a third mixed solution series as a standard working solution series. The number of volumetric flasks is equal to the number of standard points. The nominal capacity of the plurality of volumetric flasks is equal, and the nominal capacity of the volumetric flask is equal to the constant volume of a single standard point.

[0041] Step S6, the standard working solution series is used for standard curve drawing.

[0042] In summary, the scheme proposed by the present application has the following technical effects:

[0043] According to the acid-base neutralization principle, high-purity beryllium hydroxide is used to replace high-purity beryllium, which avoids the difficulty of obtaining high-purity beryllium. In the configuration of the series of standard solutions required for ICP-OES and ICP-MS analysis, high-purity beryllium hydroxide and corresponding dissolved acid are used to generate matrix beryllium salt and water, and the chemical behavior and state of the standard series solution are realized to achieve the same matrix matching effect as high-purity metallic beryllium dissolution.

[0044] In addition, since high-purity beryllium hydroxide is more easily obtained than high-purity beryllium metal, the present application solves the key problem of impurity analysis in beryllium metal chemical analysis in production practice, and can also solve similar problems in related beryllium alloy chemical analysis, thereby effectively promoting the technical progress of beryllium and beryllium alloy chemical analysis.

[0045] In addition, the present application solves the problem of matrix matching in domestic beryllium chemical analysis wet analysis, improves work efficiency, reduces the difficulty of daily analysis work, improves the adaptability of analysis, is conducive to establishing the traceability of material metrology, meets the related method matching requirements of the further promotion of beryllium chemical analysis standardization work and equipment domestic substitution work.

[0046] The above examples only express several embodiments of the present application, and the description is more specific and detailed, but it cannot be understood as a limitation on the scope of the patent. It should be noted that for ordinary skilled persons in the art, without departing from the concept of the present application, a number of modifications and improvements can be made, which are within the scope of the present application. Therefore, the protection scope of the patent of the present application should be subject to the appended claims.

Claims

1. A method for matrix matching in wet analysis of beryllium chemical analysis, characterized in that: The method comprises: Step S1, determining a wet analysis method for beryllium chemical analysis; Step S2, extracting elements associated with the preparation of a standard working solution in the beryllium chemical analysis wet analysis method; Step S3, placing equal amounts of beryllium hydroxide or beryllium hydroxide and a coexisting matrix in multiple beakers, wetting them with secondary water, and then adding the same type and volume of dissolving acid respectively. After the heating reaction is completed, a first mixed solution series is obtained; Step S4, adding the element to be tested with a corresponding content gradient to each first mixed solution in the first mixed solution series to obtain a second mixed solution series; Step S5, transferring each second mixed solution in the second mixed solution series to a corresponding volumetric flask and fixing the volume to obtain a third mixed solution series as a standard working solution series; Step S6: draw a standard curve using the standard working solution series.

2. The method for matrix matching in wet analysis of beryllium chemical analysis according to claim 1, characterized in that: In step S2, the factors include: beryllium amount, coexisting matrix amount, dissolving acid type, dissolving acid dosage, analyte type, analyte content gradient, number of standard points in the standard working solution series, and constant volume of a single standard point.

3. The method for matrix matching in wet analysis of beryllium chemical analysis according to claim 2, characterized in that: The types of elements to be detected include: at least one of iron, aluminum, chromium, silicon, magnesium, zinc, copper, manganese, nickel, lead, calcium, molybdenum, titanium, zirconium, silver, cadmium, lithium, cobalt, boron, samarium, europium, gadolinium, dysprosium and uranium.

4. The method for matrix matching in wet analysis of beryllium chemical analysis according to claim 2, characterized in that: The upper limit of the gradient of the element content to be measured is 100 μg / mL.

5. The method for matrix matching in wet analysis of beryllium chemical analysis according to claim 2, characterized in that: In step S5, the number of volumetric flasks is equal to the number of standard points; the nominal capacities of the multiple volumetric flasks are equal, and the nominal capacities of the volumetric flasks are equal to the fixed volume of a single standard point.

6. The method for matrix matching in wet analysis of beryllium chemical analysis according to claim 1, characterized in that: In step S3, the amount of beryllium hydroxide in each beaker is 4.78 times the amount of beryllium.

7. The method for matrix matching in wet analysis of beryllium chemical analysis according to claim 1, characterized in that: In the step S1, the application objects of the beryllium chemical analysis wet analysis method include: metallic beryllium and beryllium alloys.

8. The method for matrix matching in wet analysis of beryllium chemical analysis according to claim 1, characterized in that: In the step S1, the beryllium chemical analysis wet analysis method includes: a standard method or a non-standard method.

9. The method for matrix matching in wet analysis of beryllium chemical analysis according to claim 1, characterized in that: In the step S1, the principles of the beryllium chemical analysis wet analysis method include: ICP-OES method and ICP-MS method.