Method for measuring element content in silver anode plate
By using an X-fluorescence spectrometer in the silver anode plate for rapid detection, and using lathe to remove the surface layer and pre-determined standard sample correction coefficients, the problem of long analysis time and inability to synchronously determine high silver content in the prior art is solved, and the rapid and accurate determination of the element content in the silver anode plate is achieved.
Patent Information
- Application Number
- CN202411979929.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-31
- Publication Date
- 2025-04-25
AI Technical Summary
When determining the element content in silver anode plates, the analysis time is long, and the demand for rapid analysis in production cannot be met, and the high content of silver cannot be analyzed synchronously.
The surface of the silver anode plate was detected by an X-fluorescence spectrometer, and the surface layer was removed through the lathe was directly measured, and the pre-determined standard calibration coefficient was used for accurate measurement.
It realizes rapid and accurate determination of the element content in the silver anode plate, the sample pretreatment process is short, no chemical dissolution is required, and the hidden danger of acid and alkali burns is avoided, and multiple element contents can be measured at the same time.
Smart Images
Figure CN119880977A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the field of element chemical analysis, and in particular relates to a method for determining the element content in a silver anode plate. Background Art
[0002] The statements in this section are merely intended to provide background information related to the technical solution of the present application to aid understanding, and they do not necessarily constitute prior art for the technical solution of the present application.
[0003] Silver anode plate is an important alloy material in precious metal smelting and is the raw material for the next process of silver electrolysis. It has the characteristics of high gold and silver content (gold + silver ≥ 97%) and low impurity element content. In actual production, platinum and palladium will partially enter the electrolyte. If the electrolysis conditions are not properly controlled, palladium and silver will co-precipitate, affecting the quality of silver powder. If there is selenium in the silver anode mud, selenium and silver will also precipitate together in the weakly acidic electrolyte. When the silver ion concentration in the electrolyte drops sharply, copper will precipitate together with silver. Bismuth will also precipitate at the cathode after a long period of accumulation. Therefore, controlling the content of each element in the silver anode plate is a prerequisite for ensuring the quality of silver powder. The silver content in the silver anode plate is above 90%. The high content of silver is determined by potassium thiocyanate volumetric method, but other impurity elements such as gold, platinum, palladium, copper, selenium, tellurium, and bismuth need to be detected by other methods due to their low content. The silver anode plate can be dissolved by nitric acid, and iron solution and ammonia water are added to the solution. The tellurium in the silver anode plate is separated and enriched by co-precipitation with iron hydroxide. After eliminating the interference of the matrix, it is determined by atomic absorption method. However, this method has a complicated operation process and can only determine a single impurity element Te. The currently published papers introduce the method of ICP-AES determination of Se, Sb, Te, Bi, Pb, Au, Fe, Cu, and Pd impurity elements in silver anode plates. Tartaric acid solution is first added to the sample as a masking agent, and then nitric acid is added to dissolve the silver anode plate. Hydrochloric acid is added to the solution to precipitate the silver matrix, and the precipitate is filtered and washed. The washing solution and the filtrate are concentrated to a small volume and then fixed to volume with hydrochloric acid. The ICP-AES is determined according to the set instrument working conditions to obtain the content of each impurity element. This method is currently widely used and can measure multiple impurity elements simultaneously, but its measurement process requires chemical dissolution before measurement, and the analysis time is long. It cannot meet the needs of rapid analysis of silver anode plates in production, and cannot perform synchronous analysis of high-content silver. X-ray fluorescence spectroscopy has the advantages of simple spectral lines, no damage to samples, easy to overcome the absorption and enhancement effects of the matrix, simple operation, and rapid measurement. It is more suitable for on-site analysis. However, this method has low accuracy and is prone to large errors. Summary of the invention
[0004] In order to solve the problems existing in the prior art, a method for determining the element content in a silver anode plate is provided, which has obvious advantages in that the sample pretreatment process is short, the determination results are fast and accurate, and the span of element content is large.
[0005] In order to achieve the above object, the present invention adopts the following technical solutions:
[0006] A method for determining the element content in a silver anode plate comprises:
[0007] Using a lathe to remove the surface layer of the silver anode plate standard sample that has been cast into an ingot to obtain a smooth surface to be tested, wherein the element content in the silver anode plate standard sample has been determined in advance;
[0008] The surface layer of the silver anode plate sample which has been cast into an ingot is removed by lathe to obtain a smooth surface to be tested;
[0009] Using an X-ray fluorescence spectrometer to detect the test surface of the silver anode plate standard sample to obtain the test result of the content of each element in the element;
[0010] Comparing the detection result of the content of each element with the content of each element in the silver anode plate standard sample measured in advance, and determining the correction coefficient of each element;
[0011] Inputting a correction factor for each element into the X-ray fluorescence spectrometer;
[0012] The X-ray fluorescence spectrometer is used to detect the test surface of the silver anode plate sample to obtain the test result of the content of each element in the elements.
[0013] In one embodiment, determining the correction coefficient of each element includes: for each element, calculating the difference between the content detection result and the pre-determined content, calculating the ratio of the difference to the pre-determined content, and determining the correction coefficient according to the ratio.
[0014] In one embodiment, the step of removing the surface layer of the silver anode plate standard sample that has been cast into an ingot by using a lathe includes removing 2 mm of the surface layer of the silver anode plate standard sample that has been cast into an ingot by using a lathe, and the step of removing the surface layer of the silver anode plate sample that has been cast into an ingot by using a lathe includes removing 2 mm of the surface layer of the silver anode plate sample that has been cast into an ingot by using a lathe.
[0015] In one embodiment, the element includes one or more of silver, gold, platinum, palladium, copper, selenium, tellurium, and bismuth.
[0016] In one embodiment, when using an X-ray fluorescence spectrometer to detect the test surface of the silver anode plate standard or the silver anode plate sample, a suitable working mode of the X-ray fluorescence spectrometer is selected for different elements to be detected.
[0017] In one embodiment, the content of silver, gold, copper and palladium is detected by using the precious metal mode of the X-ray fluorescence spectrometer, and the content of platinum, selenium, tellurium and bismuth is detected by using the geochemical mode of the X-ray fluorescence spectrometer.
[0018] A method for determining the element content in a silver anode plate comprises:
[0019] Using a lathe to remove the surface layer of the silver anode plate standard sample that has been cast into an ingot to obtain a smooth surface to be tested, wherein the element content in the silver anode plate standard sample has been determined in advance;
[0020] The surface layer of the silver anode plate sample which has been cast into an ingot is removed by lathe to obtain a smooth surface to be tested;
[0021] Using an X-ray fluorescence spectrometer to detect the test surface of the silver anode plate standard sample to obtain the test result of the content of each element in the element;
[0022] Comparing the detection result of the content of each element with the content of each element in the silver anode plate standard sample measured in advance, and determining the correction coefficient of each element;
[0023] Using the X-ray fluorescence spectrometer to detect the test surface of the silver anode plate sample to obtain the test result of the content of each element in the elements;
[0024] Based on the detection result of the content of each element in the silver anode plate sample and the correction coefficient of each element, the content of each element in the silver anode plate sample is determined.
[0025] In one embodiment, determining the correction coefficient of each element includes: for each element, calculating the difference between the content detection result and the pre-determined content, calculating the ratio of the difference to the pre-determined content, and determining the correction coefficient according to the ratio.
[0026] In one embodiment, the step of removing the surface layer of the silver anode plate standard sample that has been cast into an ingot by using a lathe includes removing 2 mm of the surface layer of the silver anode plate standard sample that has been cast into an ingot by using a lathe, and the step of removing the surface layer of the silver anode plate sample that has been cast into an ingot by using a lathe includes removing 2 mm of the surface layer of the silver anode plate sample that has been cast into an ingot by using a lathe.
[0027] In one embodiment, the element includes one or more of silver, gold, platinum, palladium, copper, selenium, tellurium, and bismuth.
[0028] In one embodiment, when using an X-ray fluorescence spectrometer to detect the test surface of the silver anode plate standard or the silver anode plate sample, a suitable working mode of the X-ray fluorescence spectrometer is selected for different elements to be detected.
[0029] In one embodiment, the content of silver, gold, copper and palladium is detected by using the precious metal mode of the X-ray fluorescence spectrometer, and the content of platinum, selenium, tellurium and bismuth is detected by using the geochemical mode of the X-ray fluorescence spectrometer.
[0030] Compared with the prior art, the present invention has the following beneficial technical effects: after treating the surface of the silver anode plate to be tested, the present invention uses an X-ray fluorescence spectrometer to measure the content of each element in the silver anode plate to be tested, and obtains the test result. Compared with the original sample pretreatment process of "nitric acid dissolution-chlorination silver precipitation", the present invention has the characteristics of short sample pretreatment process, no need to chemically dissolve the sample, and eliminate the hidden danger of acid and alkali burns during the operation; compared with the potassium thiocyanate volumetric method for determining the amount of high-grade silver, and the inductively coupled plasma emission spectrometry method for determining the content of low-grade gold, platinum, palladium, copper, selenium, tellurium, and bismuth, the present invention has the characteristics of fast determination speed, small interference, no pollution to the environment, and can achieve simultaneous determination of multiple elements with large content differences. The present invention can be extended to the determination of element content in other alloy materials in the field of metallurgy. BRIEF DESCRIPTION OF THE DRAWINGS
[0031] The embodiments of the present invention are further described below with reference to the accompanying drawings, in which:
[0032] Figure 1 The figure is a schematic flow chart of a method for determining the element content in a silver anode plate according to one embodiment. DETAILED DESCRIPTION
[0033] In order to make the purpose, technical solution and advantages of the present invention more clearly understood, the present invention is further described in detail below through specific embodiments in conjunction with the accompanying drawings. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.
[0034] Figure 1 The figure is a flow chart of a method for determining the element content in a silver anode plate according to one embodiment. The method comprises:
[0035] The surface layer of the silver anode plate standard sample that has been cast into an ingot is removed by lathe to obtain a smooth surface to be tested, wherein the element content in the silver anode plate standard sample has been pre-determined. Various element determination methods in the art can be used to pre-determine the element content in the silver anode plate standard sample. Generally, these determination methods have high accuracy, but may be cumbersome, take a long time, or may be costly. In one embodiment, a portion of the standard sample can be taken and chemically dissolved, and divided into two portions, one of which can be titrated to determine the silver content therein, and the other portion can be determined using an inductively coupled plasma emission spectrometer (ICP spectrometer) to determine the content of other elements.
[0036] In one embodiment, the element includes one or more of silver, gold, platinum, palladium, copper, selenium, tellurium, and bismuth. In one embodiment, a lathe can be used to remove 2 mm of the surface layer of the silver anode plate standard sample that has been cast into an ingot.
[0037] The silver anode plate samples that have been cast into ingots are turned away from the surface by a lathe to obtain a smooth surface to be tested. In one embodiment, the silver anode plate samples that have been cast into ingots can be turned away from the surface by 2 mm by a lathe.
[0038] The test surface of the silver anode plate standard sample is tested using an X-ray fluorescence spectrometer to obtain the test result of the content of each element in the element.
[0039] The detection result of the content of each element is compared with the content of each element in the silver anode plate standard sample measured in advance to determine the correction coefficient of each element. In one embodiment, the difference between the detection result of the content of each element and the pre-determined content can be calculated, and the proportional relationship between the difference and the pre-determined content can be calculated to determine the correction coefficient.
[0040] The correction factor for each element is input into the X-ray fluorescence spectrometer.
[0041] The X-ray fluorescence spectrometer is used to detect the test surface of the silver anode plate sample to obtain the test result of the content of each element in the elements.
[0042] In one embodiment, when using an X-ray fluorescence spectrometer to detect the surface to be tested of the silver anode plate standard or the silver anode plate sample, for different elements to be detected, a suitable working mode of the X-ray fluorescence spectrometer can be selected, and then the surface to be tested is placed above the detection window of the X-ray fluorescence spectrometer, and the detection is started to obtain the detection result of the element content. In one embodiment, the precious metal mode of the X-ray fluorescence spectrometer can be used to determine the content of Ag, Au, Cu, and Pd elements, and the geochemical mode of the X-ray fluorescence spectrometer can be used to determine the content of Pt, Se, Te, and Bi elements.
[0043] Example 1
[0044] After the silver anode plate sample (silver anode plate No. 1) and the silver anode plate standard were cast into ingots in a graphite crucible, the surface was removed by lathe about 2mm to obtain a smooth surface to be tested. The built-in precious metal mode of the X-ray fluorescence spectrometer was selected, and the smooth surface to be tested of the silver anode plate standard was placed above the detection window of the X-ray fluorescence spectrometer to determine the content of Ag, Au, Cu, and Pd elements in the silver anode plate standard. Then, the built-in geochemical mode of the X-ray fluorescence spectrometer was selected to determine the content of Pt, Se, Te, and Bi elements in the silver anode plate standard, and compared with the previously determined fixed values of the content of each element of the silver anode plate standard to obtain the correction coefficient of each element. Input the correction coefficient of each element into the X-ray fluorescence spectrometer, then place the smooth surface of the silver anode plate No. 1 to be tested above the detection window of the X-ray fluorescence spectrometer, select the precious metal mode of the X-ray fluorescence spectrometer to determine the content of Ag, Au, Cu, and Pd elements, and then select the geochemical mode of the X-ray fluorescence spectrometer to determine the content of Pt, Se, Te, and Bi elements, and obtain the detection results of the content of each element in the silver anode plate No. 1.
[0045] Table 1 Test results of silver anode plate standard sample
[0046]
[0047] Table 2 Correction coefficients of each element
[0048]
[0049] Table 3 Test results of silver anode plate No. 1
[0050]
[0051] Example 2
[0052] After the silver anode plate sample (silver anode plate No. 2) is cast into an ingot in a graphite crucible, the surface is turned away by a lathe to remove about 2 mm to obtain a smooth surface to be tested. After the X-ray fluorescence spectrometer is calibrated using the silver anode plate standard sample (see above for the specific calibration method), the correction coefficients of each element are input into the X-ray fluorescence spectrometer. Select the built-in precious metal mode of the X-ray fluorescence spectrometer, place the smooth surface of the silver anode plate No. 2 to be tested above the detection window of the X-ray fluorescence spectrometer, and measure the content of Ag, Au, Cu, and Pd elements in the silver anode plate. Then select the built-in geochemical mode of the X-ray fluorescence spectrometer to measure the content of Pt, Se, Te, and Bi elements in the silver anode plate, and obtain the test results of the content of each element in the silver anode plate No. 2.
[0053] Table 4 Test results of silver anode plate No. 2
[0054]
[0055] Example 3
[0056] After the silver anode plate sample (silver anode plate No. 3) is cast into an ingot in a graphite crucible, the surface is turned by a lathe to remove about 2 mm to obtain a smooth surface to be tested. After the X-ray fluorescence spectrometer is calibrated using the silver anode plate standard sample (the specific calibration method is as above), the correction coefficients of each element are input into the X-ray fluorescence spectrometer. The built-in precious metal mode of the X-ray fluorescence spectrometer is selected, and the smooth surface of the silver anode plate No. 3 to be tested is placed above the detection window of the X-ray fluorescence spectrometer to determine the content of Ag, Au, Cu, and Pd elements in the silver anode plate. Then, the built-in geochemical mode of the X-ray fluorescence spectrometer is selected to determine the content of Pt, Se, Te, and Bi elements in the silver anode plate, and the detection results of the content of each element in the silver anode plate No. 3 are obtained.
[0057] Table 5 Test results of silver anode plate No. 3
[0058]
[0059] In one embodiment, a method for determining the element content in a silver anode plate comprises:
[0060] The surface layer of the silver anode plate standard sample cast into an ingot is removed by lathe to obtain a smooth surface to be tested, wherein the element content in the silver anode plate standard sample has been determined in advance. In one embodiment, the element includes one or more of silver, gold, platinum, palladium, copper, selenium, tellurium, and bismuth.
[0061] The surface layer of the silver anode plate sample which has been cast into an ingot is removed by lathe to obtain a smooth surface to be tested.
[0062] The test surface of the silver anode plate standard sample is tested using an X-ray fluorescence spectrometer to obtain the test result of the content of each element in the element.
[0063] The detection result of the content of each element is compared with the content of each element in the silver anode plate standard sample measured in advance to determine the correction coefficient of each element.
[0064] The X-ray fluorescence spectrometer is used to detect the test surface of the silver anode plate sample to obtain the test result of the content of each element in the elements.
[0065] Based on the detection result of the content of each element in the silver anode plate sample and the correction coefficient of each element, the content of each element in the silver anode plate sample is determined.
[0066] In this embodiment, after determining the correction coefficient of each element, it is not necessary to input the correction coefficient of each element into the X-ray fluorescence spectrometer. Instead, the accurate content of each element can be determined based on the test results of the content of each element in the silver anode plate sample and the correction coefficient of each element (that is, the test results are adjusted using the correction coefficient).
[0067] References herein to "various embodiments", "some embodiments", "one embodiment" or "an embodiment" etc. refer to that a particular feature, structure or property described in conjunction with the embodiment is included in at least one embodiment. Therefore, the phrases "in various embodiments", "in some embodiments", "in one embodiment" or "in an embodiment" etc. appearing throughout this document do not necessarily refer to the same embodiment. In addition, particular features, structures or properties may be combined in any suitable manner in one or more embodiments. Therefore, the particular features, structures or properties shown or described in conjunction with one embodiment may be combined in whole or in part with features, structures or properties of one or more other embodiments without restriction, as long as the combination is not illogical or inoperable. Expressions similar to "according to A", "based on A", "through A" or "using A" appearing herein are intended to be non-exclusive, that is, "according to A" may cover "according to A only" or "according to A and B", unless it is specifically stated that its meaning is "according to A only". In this application, for the sake of clarity, some exemplary operating steps are described in a certain order, but those skilled in the art will understand that each of these operating steps is not essential, and some of the steps may be omitted or replaced by other steps. These operation steps do not have to be executed sequentially in the manner shown; on the contrary, some of these operation steps can be executed in different orders or in parallel according to actual needs, as long as the new execution manner is not illogical or inoperable.
[0068] Some exemplary embodiments of the present invention are described above. It can be understood that the above embodiments are only used to explain the present invention and do not constitute a limitation on the protection scope of the present invention. The features in these embodiments can be recombined in a suitable manner, and the scheme obtained thereby is still within the protection scope required by the present invention. Based on the above embodiments, all other embodiments obtained by those skilled in the art without making creative work, that is, all modifications, equivalent substitutions and improvements made within the spirit and principles of this application, fall within the protection scope required by the present invention.
Claims
1. A method for determining the element content in a silver anode plate, characterized in that: include: Using a lathe to remove the surface layer of the silver anode plate standard sample that has been cast into an ingot to obtain a smooth surface to be tested, wherein the element content in the silver anode plate standard sample has been determined in advance; The surface layer of the silver anode plate sample which has been cast into an ingot is removed by lathe to obtain a smooth surface to be tested; Using an X-ray fluorescence spectrometer to detect the test surface of the silver anode plate standard sample to obtain the test result of the content of each element in the element; Comparing the detection result of the content of each element with the content of each element in the silver anode plate standard sample measured in advance, and determining the correction coefficient of each element; Inputting a correction factor for each element into the X-ray fluorescence spectrometer; The X-ray fluorescence spectrometer is used to detect the test surface of the silver anode plate sample to obtain the test result of the content of each element in the elements.
2. The method for determining the element content in a silver anode plate according to claim 1, wherein: The element includes one or more of silver, gold, platinum, palladium, copper, selenium, tellurium, and bismuth.
3. The method for determining the element content in a silver anode plate according to claim 1, wherein: Determining the correction coefficient of each element includes: for each element, calculating the difference between the content detection result and the pre-determined content, calculating the ratio of the difference to the pre-determined content, and determining the correction coefficient according to the ratio.
4. The method for determining the element content in a silver anode plate according to claim 1, wherein: The precious metal mode of the X-ray fluorescence spectrometer was used to detect the contents of silver, gold, copper and palladium, and the geochemical mode of the X-ray fluorescence spectrometer was used to detect the contents of platinum, selenium, tellurium and bismuth.
5. The method for determining the element content in a silver anode plate according to claim 1, wherein: The method of removing the surface layer of the silver anode plate standard sample that has been cast into an ingot by lathe includes removing 2 mm of the surface layer of the silver anode plate standard sample that has been cast into an ingot by lathe, and the method of removing the surface layer of the silver anode plate sample that has been cast into an ingot by lathe includes removing 2 mm of the surface layer of the silver anode plate sample that has been cast into an ingot by lathe.
6. A method for determining the element content in a silver anode plate, characterized in that: include: Using a lathe to remove the surface layer of the silver anode plate standard sample that has been cast into an ingot to obtain a smooth surface to be tested, wherein the element content in the silver anode plate standard sample has been determined in advance; The surface layer of the silver anode plate sample which has been cast into an ingot is removed by lathe to obtain a smooth surface to be tested; Using an X-ray fluorescence spectrometer to detect the test surface of the silver anode plate standard sample to obtain the test result of the content of each element in the element; Comparing the detection result of the content of each element with the content of each element in the silver anode plate standard sample measured in advance, and determining the correction coefficient of each element; Using the X-ray fluorescence spectrometer to detect the test surface of the silver anode plate sample to obtain the test result of the content of each element in the elements; Based on the detection result of the content of each element in the silver anode plate sample and the correction coefficient of each element, the content of each element in the silver anode plate sample is determined.
7. The method for determining the element content in a silver anode plate according to claim 6, wherein: The element includes one or more of silver, gold, platinum, palladium, copper, selenium, tellurium, and bismuth.
8. The method for determining the element content in a silver anode plate according to claim 6, wherein: Determining the correction coefficient of each element includes: for each element, calculating the difference between the content detection result and the pre-determined content, calculating the ratio of the difference to the pre-determined content, and determining the correction coefficient according to the ratio.
9. The method for determining the element content in a silver anode plate according to claim 6, wherein: The precious metal mode of the X-ray fluorescence spectrometer was used to detect the contents of silver, gold, copper and palladium, and the geochemical mode of the X-ray fluorescence spectrometer was used to detect the contents of platinum, selenium, tellurium and bismuth.
10. The method for determining the element content in a silver anode plate according to claim 6, wherein: The method of removing the surface layer of the silver anode plate standard sample that has been cast into an ingot by lathe includes removing 2 mm of the surface layer of the silver anode plate standard sample that has been cast into an ingot by lathe, and the method of removing the surface layer of the silver anode plate sample that has been cast into an ingot by lathe includes removing 2 mm of the surface layer of the silver anode plate sample that has been cast into an ingot by lathe.