Quality control sample for determination of impurity elements in silver and its preparation method

Abstract

The present application provides a quality control sample for the determination of impurity elements in silver and a preparation method thereof, and belongs to the technical field of chemical quality control sample preparation. The method of the present invention produces a stable and qualified quality control sample for the determination of impurity elements in silver by controlling the element transfer sequence and the segmented preparation method. Among them, the coexistence of impurity elements in the solution is guaranteed by controlling the element transfer sequence and the segmented preparation method. The quality control sample for the determination of impurity elements in silver in the present invention contains 15 elements (Bi, Cd, Cr, Cu, Fe, Mg, Mn, Ni, Pb, Pd, Sb, Se, Sn, Te, Zn), covering all the elements that must be tested for silver ingot products, and fully considering the coexistence conditions of different elements in the preparation process, ensuring the accuracy of the sample value, not only meeting the detection requirements of national standards and industry standards, but also suitable for the analysis of pure silver components in silver batch products.

Description

Technical Field

[0001] The invention relates to the technical field of chemical quality control sample preparation, and in particular to a quality control sample for determining impurity elements in silver and a preparation method thereof. Background Art

[0002] Silver is widely used and is an important raw material for the manufacture of jewelry, electronics, electroplating, alloys and other industries. Due to its excellent ductility, conductivity and heat transfer, it is widely used in the manufacture of highly sensitive instrument components, automation devices and communication systems. The contact points of these instruments and equipment work millions of times, and silver can meet the working requirements. However, impurity elements in silver will affect its electrical, thermal, mechanical properties and service life, so the requirements for trace elements in pure silver are very strict.

[0003] High-purity silver ingots are tested by impurity deduction method, and inductively coupled plasma optical emission spectrometry (ICP-OES) is commonly used for simultaneous determination of multiple elements. Because it has the advantages of simultaneous determination of multiple elements and the stability of solution injection, it is an ideal method for laboratory element analysis. This method uses the standard solution prepared with the reference material as the reference for determination. The national standard for silver ingots GB / T4135-2016 gives the upper limit requirements for the content of 8 impurity elements of Cu, Fe, Pb, Se, Te, Bi, Sb, and Pd for silver ingots of different grades, but the element types given in the standard are the minimum detection requirements. Due to different raw materials and production processes, some silver ingots also contain many other impurity elements, such as Sn, Cd, Zn, Mg, Mn, Ni, Cr, etc., but there are currently no very suitable quality control samples of this type in the market, and they all need to be configured by themselves. In addition, precipitation is very likely to occur during the configuration process, resulting in preparation failure, which greatly prolongs the detection time and reduces the detection efficiency. Applicable multi-element solution quality control samples can provide better support for obtaining accurate data for related tests.

[0004] In the prior art, a method for preparing a multi-element mixed standard solution for analytical testing is provided in the patent with publication number CN 118329559 A, and a method for preparing a standard solution for the determination of 22 elements in solid waste is provided in the patent with publication number CN 117990456 A. Both methods are performed by directly mixing the impurity elements after digestion, and precipitation is very likely to occur during the preparation process, resulting in preparation failure. Summary of the invention

[0005] In view of the technical problems existing in the background technology, the present application provides a quality control sample for the determination of impurity elements in silver and a preparation method thereof, aiming to solve the problems that the element types in the existing quality control samples for the determination of impurity elements in silver are not suitable and the performance of the prepared control samples is unstable.

[0006] In a first aspect, an embodiment of the present application provides a method for preparing a quality control sample for determining impurity elements in silver, comprising the following steps:

[0007] S1. Weigh 15 samples respectively; the 15 samples include bismuth, cadmium, chromium, copper, iron, magnesium, manganese, nickel, lead, palladium, antimony, selenium, tin, tellurium and zinc;

[0008] S2. digesting the 15 samples separately to obtain 15 single element solutions;

[0009] S3. The 15 single-element solutions are divided into three groups for preparation, and the single-element solutions in each group of solutions are mixed in order. After the preparation is completed, the mixed solutions are allowed to stand to obtain a first group of mixed solutions containing bismuth, copper, lead, chromium, and selenium, a second group of mixed solutions containing iron, nickel, manganese, magnesium, and zinc, and a third group of mixed solutions containing cadmium, palladium, antimony, tin, and tellurium;

[0010] S4. Mix the first group of mixed solutions with the second group of mixed solutions, shake well, let stand, then add the third group of mixed solutions, make up to volume with nitric acid solution, shake well, let stand, and thus obtain a quality control sample for the determination of impurity elements in silver.

[0011] In the technical scheme of the embodiment of the present application, the quality control sample for the determination of impurity elements in silver contains 15 elements (Bi, Cd, Cr, Cu, Fe, Mg, Mn, Ni, Pb, Pd, Sb, Se, Sn, Te, and Zn), covering all the required elements for silver ingot products. In addition, by controlling the order of element transfer and the segmented preparation method, the coexistence conditions of different elements are fully considered during the preparation process, thereby ensuring the accuracy of the sample value. It not only meets the testing requirements of national standards and industry standards, but is also suitable for the analysis of pure silver components in silver batch products.

[0012] In some embodiments, the transfer order of each single element solution in the first group of mixed solutions in step S3 is: adding copper element solution, lead element solution, bismuth element solution, selenium element solution, and chromium element solution to the container in sequence; the transfer order of each single element solution in the second group of mixed solutions is: adding manganese element solution, magnesium element solution, nickel element solution, iron element solution, and zinc element solution to the container in sequence; the transfer order of each single element solution in the third group of mixed solutions is: adding tin element solution, antimony element solution, palladium element solution, cadmium element solution, and tellurium element solution to nitric acid in sequence.

[0013] In this embodiment, 15 impurity elements are divided into three groups to prepare three groups of solutions respectively, and the single element solutions in each group of solutions are also mixed in a specific order, fully considering the coexistence conditions of different elements, and effectively preventing precipitation when the single element solutions are mixed with each other.

[0014] In some embodiments, the digestion steps of the 15 samples in step S2 are as follows:

[0015] Bismuth solution: add nitric acid solution to the bismuth sample, cover, heat, and after the bismuth sample is completely dissolved, remove and cool to room temperature;

[0016] Cadmium solution: add nitric acid solution to the cadmium sample, cover, heat, and after the cadmium sample is completely dissolved, remove and cool to room temperature;

[0017] Chromium solution: add hydrochloric acid solution to the chromium sample, cover, heat, and after the chromium sample is completely dissolved, remove and cool to room temperature;

[0018] Copper solution: add nitric acid solution to the copper sample, cover, heat, and after the copper sample is completely dissolved, remove and cool to room temperature;

[0019] Iron solution: add nitric acid solution to the iron sample, cover, heat, and after the iron sample is completely dissolved, remove and cool to room temperature;

[0020] Magnesium solution: add nitric acid solution to the magnesium sample, cover, heat, and after the magnesium sample is completely dissolved, remove and cool to room temperature;

[0021] Manganese solution: add nitric acid solution to the manganese sample, cover, heat, and after the manganese sample is completely dissolved, remove and cool to room temperature;

[0022] Nickel solution: add nitric acid solution to the nickel sample, cover, heat, and after the nickel sample is completely dissolved, remove and cool to room temperature;

[0023] Lead solution: add nitric acid solution to the lead sample, cover, heat, and after the lead sample is completely dissolved, remove and cool to room temperature, wait for white lead nitrate solid to precipitate, add water, heat again, and after the lead nitrate solid is completely dissolved, remove and cool to room temperature;

[0024] Palladium solution: add aqua regia to the palladium sample, cover, heat, and after the palladium sample is completely dissolved, remove and cool to room temperature;

[0025] Antimony solution: add aqua regia to the antimony sample, cover, heat, and after the antimony sample is completely dissolved, remove and cool to room temperature;

[0026] Selenium solution: add nitric acid solution to the selenium sample, cover, heat, and add nitric acid until the selenium sample is completely dissolved, then remove and cool to room temperature;

[0027] Tin solution: add hydrochloric acid to the tin sample, cover, heat, and add more hydrochloric acid until the tin sample is completely dissolved, then remove and cool to room temperature;

[0028] Tellurium solution: add nitric acid to the tellurium sample, cover, heat, and after the antimony sample is completely dissolved, remove and cool to room temperature, wait for tellurium nitrate solid to precipitate, add water, heat again, and after the tellurium nitrate solid is completely dissolved, remove and cool to room temperature;

[0029] Zinc solution: add nitric acid solution to the zinc sample, cover, heat, and after the antimony sample is completely dissolved, remove and cool to room temperature.

[0030] In this embodiment, 15 single-element solutions are obtained by completely dissolving 15 impurity elements, wherein elements such as lead, selenium, and tellurium are dissolved by a multi-stage dissolution method to ensure that the insoluble elements are completely dissolved.

[0031] In some embodiments, the purity of the 15 samples described in step S1 is not less than 99.99%.

[0032] In this embodiment, high-purity samples can ensure the accuracy of quality control samples and reduce the impact of other impurity elements.

[0033] In some embodiments, the standing temperature in steps S3 and S4 is 18-22° C., and the standing time is 24 hours.

[0034] In this embodiment, the mixed solution is fully mixed by standing at a certain temperature to obtain a stable mixed solution.

[0035] In some embodiments, the volume percentage concentration of the nitric acid solution in step S4 is 18-22%.

[0036] In this embodiment, a quality control sample with a certain concentration of impurity elements is obtained by constant volume of nitric acid solution.

[0037] In some embodiments, the nitric acid solution is formed by mixing equal volumes of nitric acid and water; the hydrochloric acid solution is formed by mixing equal volumes of hydrochloric acid and water; the purity level of the hydrochloric acid and nitric acid is not less than super pure; and the water is distilled water or deionized water.

[0038] In this embodiment, the high-purity solvent can ensure the accuracy of the quality control sample and reduce the influence of other impurity elements.

[0039] In some embodiments, the heating temperature is 150-300°C.

[0040] In this embodiment, low temperature heating is adopted to ensure better digestion of various impurity elements.

[0041] In some embodiments, the quality control sample for the determination of impurity elements in silver includes 15 elements: bismuth, cadmium, chromium, copper, iron, magnesium, manganese, nickel, lead, palladium, antimony, selenium, tin, tellurium, and zinc, and the mass volume concentration of each element is 0.00 ~ 500 μg / mL.

[0042] In this embodiment, the quality control sample prepared for the determination of impurity elements in silver covers all the elements that must be tested for silver ingot products, and is suitable for the analysis of pure silver components in silver batch products.

[0043] The above description is only an overview of the technical solution of the present application. In order to more clearly understand the technical means of the present application, it can be implemented in accordance with the contents of the specification. In order to make the above and other purposes, features and advantages of the present application more obvious and easy to understand, the specific implementation methods of the present application are listed below. DETAILED DESCRIPTION

[0044] The following is a detailed description of the embodiments of the technical solution of the present application. The following embodiments are only used to more clearly illustrate the technical solution of the present application, and are therefore only used as examples, and cannot be used to limit the scope of protection of the present application.

[0045] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by technicians in the technical field to which this application belongs; the terms used herein are only for the purpose of describing specific embodiments and are not intended to limit this application; the terms "including" and "having" in the description and claims of this application and any variations thereof are intended to cover non-exclusive inclusions.

[0046] In the description of the embodiments of the present application, the technical terms "first", "second", etc. are only used to distinguish different objects, and cannot be understood as indicating or implying relative importance or implicitly indicating the number, specific order or primary and secondary relationship of the indicated technical features. In the description of the embodiments of the present application, the meaning of "multiple" is more than two, unless otherwise clearly and specifically defined.

[0047] Reference to "embodiments" herein means that a particular feature, structure, or characteristic described in conjunction with the embodiments may be included in at least one embodiment of the present application. The appearance of the phrase in various locations in the specification does not necessarily refer to the same embodiment, nor is it an independent or alternative embodiment that is mutually exclusive with other embodiments. It is explicitly and implicitly understood by those skilled in the art that the embodiments described herein may be combined with other embodiments.

[0048] In order to solve the problems of insufficient element content in the existing quality control samples for the determination of impurity elements in silver and unstable performance of the prepared control samples, the present application provides a quality control sample for the determination of impurity elements in silver and a preparation method thereof. The prepared quality control sample for the determination of impurity elements in silver contains 15 elements (Bi, Cd, Cr, Cu, Fe, Mg, Mn, Ni, Pb, Pd, Sb, Se, Sn, Te, Zn), covering all the elements that must be tested for silver ingot products, and by controlling the element transfer sequence and the segmented preparation method, the coexistence conditions of different elements are fully considered during the preparation process, ensuring the accuracy of the sample value, which not only meets the detection requirements of national standards and industry standards, but is also suitable for the analysis of pure silver components in silver batch products.

[0049] On the one hand, the present application provides a method for preparing a quality control sample for determining impurity elements in silver, comprising the following steps:

[0050] S1. Weigh 15 samples respectively; the 15 samples include bismuth, cadmium, chromium, copper, iron, magnesium, manganese, nickel, lead, palladium, antimony, selenium, tin, tellurium and zinc;

[0051] S2. digesting the 15 samples separately to obtain 15 single element solutions;

[0052] S3. The 15 single-element solutions are divided into three groups for preparation, and the single-element solutions in each group of solutions are mixed in order. After the preparation is completed, the mixed solutions are allowed to stand to obtain a first group of mixed solutions containing bismuth, copper, lead, chromium, and selenium, a second group of mixed solutions containing iron, nickel, manganese, magnesium, and zinc, and a third group of mixed solutions containing cadmium, palladium, antimony, tin, and tellurium;

[0053] S4. Mix the first group of mixed solutions with the second group of mixed solutions, shake well, let stand, then add the third group of mixed solutions, make up to volume with nitric acid solution, shake well, let stand, and thus obtain a quality control sample for the determination of impurity elements in silver.

[0054] In the technical scheme of the embodiment of the present application, the quality control sample for the determination of impurity elements in silver contains 15 elements (Bi, Cd, Cr, Cu, Fe, Mg, Mn, Ni, Pb, Pd, Sb, Se, Sn, Te, and Zn), covering all the required elements for silver ingot products. In addition, by controlling the order of element transfer and the segmented preparation method, the coexistence conditions of different elements are fully considered during the preparation process, thereby ensuring the accuracy of the sample value. It not only meets the testing requirements of national standards and industry standards, but is also suitable for the analysis of pure silver components in silver batch products.

[0055] Furthermore, in some embodiments, the transfer order of each single element solution in the first group of mixed solutions in step S3 is: adding copper element solution, lead element solution, bismuth element solution, selenium element solution, and chromium element solution to the container in sequence; the transfer order of each single element solution in the second group of mixed solutions is: adding manganese element solution, magnesium element solution, nickel element solution, iron element solution, and zinc element solution to the container in sequence; the transfer order of each single element solution in the third group of mixed solutions is: adding tin element solution, antimony element solution, palladium element solution, cadmium element solution, and tellurium element solution to nitric acid in sequence.

[0056] In the technical solution of the embodiment of the present application, 15 impurity elements are divided into three groups and three groups of solutions are prepared respectively, and the single element solutions in each group of solutions are also mixed in a specific order, fully considering the coexistence conditions of different elements, and effectively preventing precipitation when the single element solutions are mixed with each other.

[0057] Further, in some embodiments, the digestion steps of the 15 samples in step S2 are as follows:

[0058] Bismuth solution: add nitric acid solution to the bismuth sample, cover, heat, and after the bismuth sample is completely dissolved, remove and cool to room temperature;

[0059] Cadmium solution: add nitric acid solution to the cadmium sample, cover, heat, and after the cadmium sample is completely dissolved, remove and cool to room temperature;

[0060] Chromium solution: add hydrochloric acid solution to the chromium sample, cover, heat, and after the chromium sample is completely dissolved, remove and cool to room temperature;

[0061] Copper solution: add nitric acid solution to the copper sample, cover, heat, and after the copper sample is completely dissolved, remove and cool to room temperature;

[0062] Iron solution: add nitric acid solution to the iron sample, cover, heat, and after the iron sample is completely dissolved, remove and cool to room temperature;

[0063] Magnesium solution: add nitric acid solution to the magnesium sample, cover, heat, and after the magnesium sample is completely dissolved, remove and cool to room temperature;

[0064] Manganese solution: add nitric acid solution to the manganese sample, cover, heat, and after the manganese sample is completely dissolved, remove and cool to room temperature;

[0065] Nickel solution: add nitric acid solution to the nickel sample, cover, heat, and after the nickel sample is completely dissolved, remove and cool to room temperature;

[0066] Lead solution: add nitric acid solution to the lead sample, cover, heat, and after the lead sample is completely dissolved, remove and cool to room temperature, wait for white lead nitrate solid to precipitate, add water, heat again, and after the lead nitrate solid is completely dissolved, remove and cool to room temperature;

[0067] Palladium solution: add aqua regia to the palladium sample, cover, heat, and after the palladium sample is completely dissolved, remove and cool to room temperature;

[0068] Antimony solution: add aqua regia to the antimony sample, cover, heat, and after the antimony sample is completely dissolved, remove and cool to room temperature;

[0069] Selenium solution: add nitric acid solution to the selenium sample, cover, heat, and add nitric acid until the selenium sample is completely dissolved, then remove and cool to room temperature;

[0070] Tin solution: add hydrochloric acid to the tin sample, cover, heat, and add more hydrochloric acid until the tin sample is completely dissolved, then remove and cool to room temperature;

[0071] Tellurium solution: add nitric acid to the tellurium sample, cover, heat, and after the antimony sample is completely dissolved, remove and cool to room temperature, wait for tellurium nitrate solid to precipitate, add water, heat again, and after the tellurium nitrate solid is completely dissolved, remove and cool to room temperature;

[0072] Zinc solution: add nitric acid solution to the zinc sample, cover, heat, and after the antimony sample is completely dissolved, remove and cool to room temperature.

[0073] In the technical solution of the embodiment of the present application, 15 single-element solutions are obtained by completely digesting 15 impurity elements, among which elements such as lead, selenium, and tellurium are digested by a multi-stage dissolution method to ensure that the insoluble elements are completely digested.

[0074] Furthermore, in some embodiments, the purity of the 15 samples in step S1 is not less than 99.99%.

[0075] In the technical solution of the embodiment of the present application, high-purity samples can ensure the accuracy of quality control samples and reduce the influence of other impurity elements.

[0076] Furthermore, in some embodiments, the standing temperature in steps S3 and S4 is 18-22° C., and the standing time is 24 hours.

[0077] In the technical solution of the embodiment of the present application, the mixed solution is fully mixed by standing at a certain temperature to obtain a stable mixed solution.

[0078] Furthermore, in some embodiments, the volume percentage concentration of the nitric acid solution in step S4 is 18-22%.

[0079] In the technical solution of the embodiment of the present application, a mixed solution of impurity elements of a certain concentration is obtained by constant volume of nitric acid solution.

[0080] Furthermore, in some embodiments, the nitric acid solution is formed by mixing equal volumes of nitric acid and water; the hydrochloric acid solution is formed by mixing equal volumes of hydrochloric acid and water; the purity grade of the hydrochloric acid and nitric acid is not less than premium purity; and the water is distilled water or deionized water.

[0081] In the technical solution of the embodiment of the present application, the high-purity solvent can ensure the accuracy of the quality control sample and reduce the influence of other impurity elements.

[0082] Furthermore, in some embodiments, the heating temperature is 150-300°C.

[0083] In the technical solution of the embodiment of the present application, a low-temperature heating method is adopted to ensure better digestion of various impurity elements.

[0084] Furthermore, in some embodiments, the quality control sample for the determination of impurity elements in silver includes 15 elements: bismuth, cadmium, chromium, copper, iron, magnesium, manganese, nickel, lead, palladium, antimony, selenium, tin, tellurium, and zinc, and the mass volume concentration of each element is 0.00 ~500μg / mL.

[0085] In the technical solution of the embodiment of the present application, the quality control sample prepared for the determination of impurity elements in silver covers all the elements that must be tested for silver ingot products, and is suitable for the analysis of pure silver components in silver batch products.

[0086] Some specific embodiments are listed below. It should be noted that the embodiments described below are exemplary and are only used to explain the present application, and should not be construed as limiting the present application. If specific techniques or conditions are not specified in the embodiments, the techniques or conditions described in the literature in this area or the product specifications are used. The reagents or instruments used without specifying the manufacturer are all conventional products that can be obtained commercially.

[0087] Example 1

[0088] This embodiment provides a method for preparing a quality control sample for determination of impurity elements in silver, which specifically comprises the following steps:

[0089] S1. Weigh 2.00 mg of bismuth, cadmium, chromium, copper, iron, magnesium, manganese, nickel, lead, palladium, antimony, selenium, tin, tellurium and zinc element samples with a purity of 99.99% respectively.

[0090] S2. Digest the weighed samples separately, the steps are as follows:

[0091] Bismuth solution: Place the weighed bismuth into a beaker, add 20 ml of high-purity (1+1) nitric acid solution, cover with a watch glass, place the beaker on an electric stove and heat at 200°C. After the raw materials are completely dissolved, remove and cool to room temperature.

[0092] Cadmium solution: Place the weighed cadmium into a beaker, add 20 ml of high-purity (1+1) nitric acid solution, cover with a watch glass, place the beaker on an electric stove and heat at 200°C. After the raw materials are completely dissolved, remove and cool to room temperature.

[0093] Chromium solution: Place the weighed chromium into a beaker, add 20 ml of high-purity (1+1) hydrochloric acid solution, cover with a watch glass, place the beaker on an electric stove and heat at 200°C. After the raw materials are completely dissolved, remove and cool to room temperature.

[0094] Copper solution: Place the weighed copper into a beaker, add 20 ml of high-purity (1+1) nitric acid solution, cover with a watch glass, place the beaker on an electric stove and heat at 200°C. After the raw materials are completely dissolved, remove and cool to room temperature.

[0095] Iron solution: Place the weighed iron into a beaker, add 20 ml of high-purity (1+1) nitric acid solution, cover with a watch glass, place the beaker on an electric stove and heat at 200°C. After the raw materials are completely dissolved, remove and cool to room temperature.

[0096] Magnesium solution: Place the weighed magnesium into a beaker, add 20 ml of high-purity (1+1) nitric acid solution, cover with a watch glass, place the beaker on an electric stove and heat at 200°C. After the raw materials are completely dissolved, remove and cool to room temperature.

[0097] Manganese solution: Place the weighed manganese into a beaker, add 20 ml of high-purity (1+1) nitric acid solution, cover with a watch glass, place the beaker on an electric stove and heat at 200°C. After the raw materials are completely dissolved, remove and cool to room temperature.

[0098] Nickel solution: Place the weighed nickel into a beaker, add 20 ml of high-purity (1+1) nitric acid solution, cover with a watch glass, place the beaker on an electric stove and heat at 200°C. After the raw materials are completely dissolved, remove and cool to room temperature.

[0099] Lead solution: Place the weighed lead into a beaker, add 20 ml of high-purity (1+1) nitric acid solution, cover with a watch glass, place the beaker on an electric stove and heat at 200°C. After the raw materials are completely dissolved, remove and cool to room temperature. After the white lead nitrate solid is precipitated, add 30 ml of deionized water, heat again at 200°C, and after the salts are completely dissolved, remove and cool to room temperature.

[0100] Palladium solution: Place the weighed palladium into a beaker, add 20 ml of aqua regia, cover with a watch glass, place the beaker on an electric stove and heat at 200°C. After the raw materials are completely dissolved, remove and cool to room temperature.

[0101] Antimony solution: Put the weighed antimony into a beaker, add 20 ml of aqua regia, cover with a watch glass, place the beaker on an electric stove and heat at 200°C. After the raw materials are completely dissolved, remove and cool to room temperature.

[0102] Selenium solution: Place the weighed selenium into a beaker, add 20 ml of high-purity (1+1) nitric acid solution, cover with a watch glass, place the beaker on an electric stove and heat at 200°C. Add 10 ml of nitric acid during digestion. After the raw material is completely digested, remove and cool to room temperature.

[0103] Tin solution: Place the weighed tin into a beaker, add 20 ml of high-purity (1+1) hydrochloric acid, cover with a watch glass, place the beaker on an electric stove and heat at 200°C. Add high-purity hydrochloric acid in small amounts and multiple times during digestion. After the raw material is completely digested, remove and cool to room temperature.

[0104] Tellurium solution: Place the weighed tellurium into a beaker, add 20 ml of high-purity (1+1) nitric acid, cover with a watch glass, place the beaker on an electric stove and heat at 200°C. After the raw materials are completely dissolved, remove and cool to room temperature. After the tellurium nitrate solid is precipitated, add 30 ml of deionized water, heat again at 200°C, and after the salts are completely dissolved, remove and cool to room temperature.

[0105] Zinc solution: Place the weighed zinc into a beaker, add 20 ml of high-purity (1+1) nitric acid solution, cover with a watch glass, place the beaker on an electric stove and heat at 200°C. After the raw materials are completely dissolved, remove and cool to room temperature.

[0106] S3. Prepare three groups of mixed solutions by adding the single element solutions obtained by digestion in the following order: in a clean room at 20°C, transfer the copper single element solution to a beaker of appropriate volume, then transfer the lead single element solution to a beaker containing the copper single element solution, then transfer the bismuth single element solution to a beaker containing a copper-lead mixed solution, then transfer the selenium single element solution to a beaker containing a copper, lead, and bismuth mixed solution, and finally transfer the chromium single element solution to a beaker containing a copper, lead, bismuth, and selenium mixed solution to obtain the first group of mixed solutions, which are allowed to stand for 24 hours; transfer the manganese single element solution to a beaker of appropriate volume, then transfer the magnesium single element solution to a beaker containing a manganese single element solution, then transfer the nickel single element solution to a beaker containing a manganese and magnesium mixed solution, then transfer the iron single element solution to a beaker containing a manganese, magnesium, and nickel mixed solution. liquid, and finally transfer the zinc single element solution to a beaker containing a mixed solution of manganese, magnesium, nickel and zinc to obtain a second group of mixed solutions, which are allowed to stand for 24 hours; add 20 ml of ultra-pure (1+1) nitric acid to the beaker, and then transfer the tin single element solution to the beaker containing ultra-pure (1+1) nitric acid, and then transfer the antimony single element solution to the beaker containing ultra-pure (1+1) nitric acid and tin single element solution, and then transfer the palladium single element solution to the beaker containing ultra-pure (1+1) nitric acid, tin and antimony mixed solution, then transfer the cadmium single element solution to the beaker containing ultra-pure (1+1) nitric acid, tin, antimony and palladium mixed solution, and finally transfer the tellurium single element solution to a beaker containing ultra-pure (1+1) nitric acid, tin, antimony, palladium and cadmium mixed solution to obtain a third group of mixed solutions, which are allowed to stand for 24 hours. The three groups of mixed solutions after standing were mixed in the following order of addition: in a clean room at 20°C, the first group of mixed solutions was first transferred to a volumetric flask, and then the second group of mixed solutions was transferred to the volumetric flask containing the first group of mixed solutions. After shaking, the mixture was allowed to stand for 24 hours. The third group of mixed solutions was then transferred to the volumetric flask containing the first and second groups of mixed solutions, and the volume was adjusted to 1000 ml with 20% nitric acid solution. After shaking, the mixture was allowed to stand for 24 hours to obtain quality control samples for the determination of impurity elements in silver.

[0107] Example 2

[0108] The present embodiment provides a quality control sample for the determination of impurity elements in silver and a preparation method thereof. Compared with Example 1, the difference is that in step S1, 5.00 mg of bismuth, cadmium, chromium, copper, iron, magnesium, manganese, nickel, lead, palladium, antimony, selenium, tin, tellurium, and zinc element samples are weighed, and the other steps are substantially the same as those in Example 1 and are not described again herein.

[0109] Example 3

[0110] The present embodiment provides a quality control sample for the determination of impurity elements in silver and a preparation method thereof. Compared with Example 1, the difference is that in step S1, 10.00 mg of bismuth, cadmium, chromium, copper, iron, magnesium, manganese, nickel, lead, palladium, antimony, selenium, tin, tellurium, and zinc element samples are weighed, and the other steps are substantially the same as those in Example 1 and are not repeated here.

[0111] The target concentrations of the impurity elements in the quality control samples prepared in Examples 1 to 3 are shown in Table 1.

[0112] Table 1 Target concentration of each impurity element in the quality control sample for determination of impurity elements in silver in Examples 1 to 3

[0113]

[0114] According to YS / T 958-2014 “Silver Chemical Analysis Method”, the impurity element content in the quality control samples prepared in Examples 1 to 3 was detected by inductively coupled plasma atomic emission spectrometry, and the quality control samples prepared in each example were tested 9 times. The test results are shown in Tables 2 to 16.

[0115] Table 2 Detection results of bismuth in quality control samples prepared in Examples 1 to 3

[0116]

[0117] Table 3 Detection results of cadmium in the quality control samples prepared in Examples 1 to 3

[0118]

[0119] Table 4 Detection results of chromium in the quality control samples prepared in Examples 1 to 3

[0120]

[0121] Table 5 Detection results of copper in the quality control samples prepared in Examples 1 to 3

[0122]

[0123] Table 6 Iron detection results in the quality control samples prepared in Examples 1 to 3

[0124]

[0125] Table 7 Magnesium detection results in quality control samples prepared in Examples 1 to 3

[0126]

[0127] Table 8 Detection results of manganese in quality control samples prepared in Examples 1 to 3

[0128]

[0129] Table 9 Nickel detection results in the quality control samples prepared in Examples 1 to 3

[0130]

[0131] Table 10 Detection results of lead in quality control samples prepared in Examples 1 to 3

[0132]

[0133] Table 11 Detection results of palladium in quality control samples prepared in Examples 1 to 3

[0134]

[0135] Table 12 Antimony element detection results in the quality control samples prepared in Examples 1 to 3

[0136]

[0137] Table 13 Detection results of selenium in quality control samples prepared in Examples 1 to 3

[0138]

[0139] Table 14 Detection results of tin in the quality control samples prepared in Examples 1 to 3

[0140]

[0141] Table 15 Detection results of tellurium in quality control samples prepared in Examples 1 to 3

[0142]

[0143] Table 16 Detection results of zinc in quality control samples prepared in Examples 1 to 3

[0144]

[0145] The test results of the concentrations of 15 elements in the quality control samples prepared in Examples 1 to 3 in Tables 2 to 16 show that the values ​​of the 15 elements are consistent with the target values.

[0146] Comparative Example 1

[0147] The present comparative example provides a quality control sample for determination of impurity elements in silver and a preparation method thereof. Compared with Example 1, the difference is that in step S3, the order of adding each single element solution is: adding cadmium single element solution, zinc single element solution, magnesium single element solution, selenium single element solution, tellurium single element solution, antimony single element solution, manganese single element solution, iron single element solution, bismuth single element solution, copper single element solution, lead single element solution, nickel single element solution, chromium single element solution, tin single element solution, and palladium single element solution into a beaker in sequence, and mixing all 15 single element solutions at one time. The other steps are substantially the same as those in Example 1 and will not be repeated here.

[0148] Comparative Example 2

[0149] The present comparative example provides a quality control sample for determination of impurity elements in silver and a preparation method thereof. Compared with Example 1, the difference is that in step S3, the order of adding each single element solution is: adding copper single element solution, lead single element solution, bismuth single element solution, selenium single element solution, chromium single element solution, manganese single element solution, magnesium single element solution, nickel single element solution, iron single element solution, zinc single element solution, tin single element solution, antimony single element solution, palladium single element solution, cadmium single element solution, and tellurium single element solution into a beaker in turn, and mixing all 15 single element solutions at one time. The other steps are substantially the same as those in Example 1 and will not be repeated here.

[0150] Comparative Example 3

[0151] This comparative example provides a quality control sample for the determination of impurity elements in silver and a preparation method thereof. Compared with Example 1, the difference is that in step S3, the mixing order of the single element solutions is different, that is, the first group of mixed solutions is transferred to a volumetric flask, and then the third group of mixed solutions is transferred to the volumetric flask containing the first group of mixed solutions, and then the second group of mixed solutions is transferred to the volumetric flask containing the first and third groups of mixed solutions. The other steps are roughly the same as in Example 1 and will not be repeated here.

[0152] The target concentrations of the impurity elements in the quality control samples prepared in Comparative Examples 1 to 3 are shown in Table 17.

[0153] Table 17 Target concentration of each impurity element in the quality control samples for determination of impurity elements in silver in comparative examples 1 to 3

[0154]

[0155] According to the requirements of YS / T 958-2014 “Silver Chemical Analysis Method”, the impurity element content in the quality control sample prepared from this comparative ratio was tested by inductively coupled plasma atomic emission spectrometry. The test results are shown in Table 18.

[0156] Table 18 Detection results of 15 elements in the quality control samples prepared in Comparative Examples 1 to 3

[0157]

[0158] From the test results in Table 18, it can be seen that the detection results of 15 impurity elements in the quality control sample prepared in Comparative Example 1 are seriously inconsistent with the target concentration, and the prepared quality control sample solution has precipitation, and the element values ​​are inaccurate; although the quality control samples prepared in Comparative Example 2 and Comparative Example 3 did not have precipitation, the detection results of some elements in the samples were significantly different from the target concentration and could not be used to guide production, indicating that the preparation methods of Comparative Examples 1 to 3 are inappropriate.

[0159] In summary, the present application provides a quality control sample for the determination of impurity elements in silver and a preparation method thereof, which belongs to the technical field of chemical quality control sample preparation. The quality control sample for the determination of impurity elements in silver contains 15 elements (Bi, Cd, Cr, Cu, Fe, Mg, Mn, Ni, Pb, Pd, Sb, Se, Sn, Te, Zn), covering all the elements that must be tested for silver ingot products, and by controlling the element transfer sequence and the segmented preparation method, the coexistence conditions of different elements are fully considered during the preparation process, ensuring the accuracy of the sample value, which not only meets the detection requirements of national standards and industry standards, but is also suitable for the analysis of pure silver components in silver batch products. It solves the problems of insufficient element content in the existing quality control samples for the determination of impurity elements in silver, and unstable performance of the prepared control samples.

[0160] It should be noted that the present application is not limited to the above-mentioned embodiments. The above-mentioned embodiments are only examples, and the embodiments having the same structure as the technical idea and exerting the same effect within the scope of the technical solution of the present application are all included in the technical scope of the present application. In addition, without departing from the scope of the main purpose of the present application, various modifications that can be thought of by those skilled in the art to the embodiments and other methods of combining some of the constituent elements in the embodiments are also included in the scope of the present application.

Claims

1. A method for preparing a quality control sample for determination of impurity elements in silver, characterized in that: The steps include: S1. Weigh 15 metal samples respectively; the 15 metal samples include bismuth, cadmium, chromium, copper, iron, magnesium, manganese, nickel, lead, palladium, antimony, selenium, tin, tellurium and zinc; S2. digesting the 15 metal samples separately to obtain 15 single element solutions; S3. The 15 single-element solutions are divided into three groups for preparation, and the single-element solutions in each group of solutions are mixed in order. After preparation, the solutions are allowed to stand to obtain a first group of mixed solutions containing bismuth, copper, lead, chromium and selenium, a second group of mixed solutions containing iron, nickel, manganese, magnesium and zinc, and a third group of mixed solutions containing cadmium, palladium, antimony, tin and tellurium; wherein, the transfer order of the single-element solutions in the first group of mixed solutions is: copper element solution, lead element solution, bismuth element solution, selenium element solution and chromium element solution are added to the container in sequence; the transfer order of the single-element solutions in the second group of mixed solutions is: manganese element solution, magnesium element solution, nickel element solution, iron element solution and zinc element solution are added to the container in sequence; the transfer order of the single-element solutions in the third group of mixed solutions is: tin element solution, antimony element solution, palladium element solution, cadmium element solution and tellurium element solution are added to nitric acid in sequence; S4. Mix the first group of mixed solutions with the second group of mixed solutions, shake well, let stand, then add the third group of mixed solutions, make up to volume with nitric acid solution, shake well, let stand, and thus obtain a quality control sample for the determination of impurity elements in silver.

2. The method for preparing a quality control sample for determination of impurity elements in silver according to claim 1, characterized in that: The digestion steps of the 15 metal samples in step S2 are as follows: Bismuth solution: add nitric acid solution to the bismuth sample, cover, heat, and after the bismuth sample is completely dissolved, remove and cool to room temperature; Cadmium solution: add nitric acid solution to the cadmium sample, cover, heat, and after the cadmium sample is completely dissolved, remove and cool to room temperature; Chromium solution: add hydrochloric acid solution to the chromium sample, cover, heat, and after the chromium sample is completely dissolved, remove and cool to room temperature; Copper solution: add nitric acid solution to the copper sample, cover, heat, and after the copper sample is completely dissolved, remove and cool to room temperature; Iron solution: add nitric acid solution to the iron sample, cover, heat, and after the iron sample is completely dissolved, remove and cool to room temperature; Magnesium solution: add nitric acid solution to the magnesium sample, cover, heat, and after the magnesium sample is completely dissolved, remove and cool to room temperature; Manganese solution: add nitric acid solution to the manganese sample, cover, heat, and after the manganese sample is completely dissolved, remove and cool to room temperature; Nickel solution: add nitric acid solution to the nickel sample, cover, heat, and after the nickel sample is completely dissolved, remove and cool to room temperature; Lead solution: add nitric acid solution to the lead sample, cover, heat, and after the lead sample is completely dissolved, remove and cool to room temperature, wait for white lead nitrate solid to precipitate, add water, heat again, and after the lead nitrate solid is completely dissolved, remove and cool to room temperature; Palladium solution: add aqua regia to the palladium sample, cover, heat, and after the palladium sample is completely dissolved, remove and cool to room temperature; Antimony solution: add aqua regia to the antimony sample, cover, heat, and after the antimony sample is completely dissolved, remove and cool to room temperature; Selenium solution: add nitric acid solution to the selenium sample, cover, heat, and add nitric acid until the selenium sample is completely dissolved, then remove and cool to room temperature; Tin solution: add hydrochloric acid to the tin sample, cover, heat, and add more hydrochloric acid until the tin sample is completely dissolved, then remove and cool to room temperature; Tellurium solution: add nitric acid to the tellurium sample, cover, heat, and after the antimony sample is completely dissolved, remove and cool to room temperature, wait for tellurium nitrate solid to precipitate, add water, heat again, and after the tellurium nitrate solid is completely dissolved, remove and cool to room temperature; Zinc solution: add nitric acid solution to the zinc sample, cover, heat, and after the antimony sample is completely dissolved, remove and cool to room temperature.

3. The method for preparing a quality control sample for determination of impurity elements in silver according to claim 1, characterized in that: The purity of the 15 metal samples in step S1 is not less than 99.99%.

4. The method for preparing a quality control sample for determination of impurity elements in silver according to claim 1, characterized in that: The standing temperature in step S3 is 18-22° C., and the standing time is 24 hours.

5. The method for preparing a quality control sample for determination of impurity elements in silver according to claim 1, characterized in that: The standing temperature in step S4 is 18-22° C., and the standing time is 24 hours.

6. The method for preparing a quality control sample for determination of impurity elements in silver according to claim 1, characterized in that: The volume percentage concentration of the nitric acid solution in step S4 is 18-22%.

7. The method for preparing a quality control sample for determination of impurity elements in silver according to claim 1, characterized in that: In step S3, the purity level of the nitric acid is not lower than premium purity.

8. The method for preparing a quality control sample for determination of impurity elements in silver according to claim 2, characterized in that: The nitric acid solution is formed by mixing equal volumes of nitric acid and water; the hydrochloric acid solution is formed by mixing equal volumes of hydrochloric acid and water; the purity level of the hydrochloric acid and the nitric acid is not less than premium purity; the water is distilled water or deionized water; and the heating temperature is 150-300°C.

9. A quality control sample for determination of impurity elements in silver, characterized in that: The quality control sample for determining impurity elements in silver and the preparation method thereof as described in any one of claims 1 to 8 are prepared, comprising 15 metal elements: bismuth, cadmium, chromium, copper, iron, magnesium, manganese, nickel, lead, palladium, antimony, selenium, tin, tellurium and zinc, and the mass volume concentration of each metal element is greater than 0 μg / mL and less than or equal to 500 μg / mL.

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