Method for measuring content of components in zinc-nickel alloy

Abstract

The invention relates to a method for determining the content of components in a zinc-nickel alloy. The method comprises the following steps: (1) preparing a zinc-nickel alloy standard substance; (2) setting direct-reading spectrometer excitation parameters of each element, and setting an analysis line and a reference line of each element; (3) drawing a working curve; and (4) exciting a zinc-nickel alloy sample by using a direct-reading spectrometer, measuring the spectral intensity value of each element, and obtaining the content of each element according to the working curve. According to the scheme provided by the invention, the content of the components in the zinc-nickel alloy can be accurately and conveniently measured.

Description

Technical Field

[0001] The present application relates to the field of analytical technology, and in particular to a method for determining the content of components in a zinc-nickel alloy. Background Art

[0002] With the rapid development of zinc-nickel alloys in the fields of automobiles and home appliances, domestic enterprises have developed zinc-nickel alloys containing more than 0.03% nickel, but the national standard GB / T 26042-2010 "Analysis of zinc and zinc alloys - Photoelectric emission spectrometry" and the national standard GB-T 12689.12-2004 "Chemical analysis of zinc and zinc alloys" cannot analyze zinc-nickel alloys containing nickel. In addition, the direct reading spectrometer used in the relevant technology to measure the nickel element has inaccurate problems.

[0003] Therefore, it is necessary to provide an accurate and convenient method for determining the content of components in zinc-nickel alloys. Summary of the invention

[0004] In order to solve or partially solve the problems existing in the related art, the present application provides a method for determining the content of components in a zinc-nickel alloy, which can accurately and conveniently determine the content of components in a zinc-nickel alloy.

[0005] The present application provides a method for determining the content of components in a zinc-nickel alloy, comprising the following steps:

[0006] 1) Preparing zinc-nickel alloy standard products;

[0007] The content range of each element in the prepared zinc-nickel alloy standard is: Al element content is 0.0005%-0.3%, Fe element content is 0.0005%-0.035%, Pb element content is 0.0012%-0.035%, Cd element content is 0.0004%-0.031%, Sn element content is 0.0004%-0.031%, Cu element content is 0.0005%-0.035%, and Ni element content is 0.0005%-0.71%.

[0008] 2) Set the direct reading spectrometer excitation parameters of each element. The analysis line and reference line of each element are:

[0009] When the Al content is 0.0005%-0.03%, the wavelength of the analysis line is 396.2nm, and the reference line is the wavelength of the Zn element at 472.2nm; when the Al content is 0.03%-0.3%, the wavelength of the analysis line is 309.3nm, and the reference line is the wavelength of the Zn element at 303.6nm;

[0010] When the Ni content is 0.0005%-0.03%, the wavelength of the analysis line is 341.5nm, and the reference line is the Zn element wavelength of 303.6nm. When the Ni content is 0.03%-0.7%, the wavelength of the analysis line is 300.2nm, and the reference line is the Zn element wavelength of 303.6nm.

[0011] The wavelength of the Fe element analysis line is 372.2nm, and the reference line is the Zn element wavelength 303.6nm;

[0012] The wavelength of the Pb element analysis line is 405.8nm, and the reference line is the Zn element wavelength 472.2nm;

[0013] The wavelength of the Cd element analysis line is 228.8nm, and the reference line is the Zn element wavelength 196.9nm;

[0014] The wavelength of the Sn element analysis line is 317.5nm, and the reference line is the Zn element wavelength 472.2nm;

[0015] The wavelength of the Cu element analysis line is 223.0nm, and the reference line is the Zn element wavelength 196.9nm;

[0016] 3) Draw the working curve;

[0017] 4) Use a direct reading spectrometer to excite the zinc-nickel alloy sample, measure the spectral intensity value of each element, and obtain the content of each element according to the working curve in step 3).

[0018] Optionally, in step 2), the flushing time is 2 seconds, the pre-combustion time is 8 seconds, and the exposure time is 4 seconds.

[0019] Optionally, the preparation method of the zinc-nickel alloy standard in step 1) is:

[0020] The zinc ingot is melted at 450-500°C, and after the zinc ingot is completely melted, the temperature is raised to 650-750°C, and a nickel ingot is added, stirred and melted, and then cast into a ZnNi10 master alloy; the mass ratio of the zinc ingot to the nickel ingot is 10:1;

[0021] The zinc ingot is melted at 450-500°C to obtain zinc liquid; the aluminum ingot, iron sheet, cathode copper and ZnNi10 master alloy are melted at 700°C, the molten liquid is directly added to the zinc liquid and stirred rapidly; the temperature is lowered to 500-550°C, lead ingot, cadmium ingot and tin ingot are added, stirred and melted, and a zinc-nickel alloy standard is obtained after 10-20 minutes.

[0022] The technical solution provided by this application may have the following beneficial effects:

[0023] The present application sets analysis lines and reference lines for Ni, Al, Fe, Pb, Cd, Sn and Cu elements, and can accurately determine the contents of each element in a zinc-nickel alloy standard product in the range of: Al content of 0.0005%-0.08%, Fe content of 0.0005%-0.035%, Pb content of 0.0012%-0.035%, Cd content of 0.0004%-0.031%, Sn content of 0.0004%-0.031%, Cu content of 0.0005%-0.035% and Ni content of 0.0005%-0.71%.

[0024] It should be understood that the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the present application. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] The above and other objects, features and advantages of the present application will become more apparent through a more detailed description of exemplary embodiments of the present application in conjunction with the accompanying drawings, wherein the same reference numerals generally represent the same components in the exemplary embodiments of the present application.

[0026] Figure 1 It is a schematic diagram of the working curve of the Al element shown in the present application;

[0027] Figure 2 This is a schematic diagram of the Ni element working curve shown in this application. DETAILED DESCRIPTION

[0028] The embodiments of the present application will be described in more detail below with reference to the accompanying drawings. Although the embodiments of the present application are shown in the accompanying drawings, it should be understood that the present application can be implemented in various forms and should not be limited by the embodiments described herein. On the contrary, these embodiments are provided to make the present application more thorough and complete, and to fully convey the scope of the present application to those skilled in the art.

[0029] A method for determining the content of components in a zinc-nickel alloy comprises the following steps:

[0030] 1) Preparation of zinc-nickel alloy standard

[0031] Add 2 kg of zinc ingot to a medium frequency induction furnace and melt it directly at a melting temperature of 450-500°C. After the zinc ingot is completely melted, heat it to 650-750°C, add 0.2 kg of nickel ingot, stir and melt it, and then cast it into a ZnNi10 master alloy.

[0032] Add the calculated weight of zinc ingots to the medium frequency induction furnace and melt them directly at a melting temperature of 450-500°C; melt the aluminum ingots, iron sheets, cathode copper, and ZnNi10 master alloy at 700°C in a high-precision automatic temperature control cabinet. Add the molten liquid directly to the zinc liquid and stir quickly to fuse the two liquids quickly. Cool down to 500-550°C, add the calculated weight of lead ingots, cadmium ingots, and tin ingots, stir and melt, and sample 8 standard samples after 10-20 minutes. The amount of each raw material added is shown in Table 1.

[0033] Table 1: Amount of each raw material added for zinc-nickel alloy standard

[0034]

[0035] According to the above zinc-nickel alloy standard preparation method, 8 zinc-nickel alloy standards with different contents were prepared, and the content of each element is shown in Table 2.

[0036] Table 2 Content of each element in zinc-nickel alloy standard

[0037] Standard sample number Al content (%) Fe content (%) Pb content (%) Cd content (%) Sn content (%) Cu content (%) Ni content (%) 1 0.0005 0.0005 0.0012 0.0004 0.0004 0.0005 0.0005 2 0.0067 0.0022 0.0018 0.0008 0.0007 0.0008 0.0035 3 0.015 0.0047 0.0022 0.0012 0.0013 0.0028 0.0089 4 0.020 0.0071 0.0065 0.0039 0.0037 0.0042 0.016 5 0.052 0.0089 0.0073 0.0056 0.0058 0.0085 0.038 6 0.08 0.012 0.0157 0.0153 0.0149 0.0132 0.092 7 0.10 0.023 0.021 0.0185 0.0195 0.022 0.25 8 0.30 0.035 0.035 0.031 0.031 0.035 0.71

[0038] 8 zinc-nickel alloy standard products were processed into smooth surfaces using a lathe;

[0039] 2) Set the direct reading spectrometer excitation parameters for each element

[0040] Direct reading spectrometer excitation parameter effect experiment:

[0041] Select spectral lines according to the range of elements with different contents: select highly sensitive analytical lines for low-content elements, select sub-sensitive lines for higher-content elements, and select spectral lines close to the analytical lines for reference lines.

[0042] In the present application, when the Al content is 0.0005%-0.03%, the wavelength of the analysis line is 396.2nm, and the reference line is the wavelength of the Zn element 472.2nm; when the Al content is 0.03%-0.3%, the wavelength of the analysis line is 309.3nm, and the reference line is the wavelength of the Zn element 303.6nm;

[0043] When the Ni content is 0.0005%-0.03%, the wavelength of the analysis line is 341.5nm, and the reference line is the Zn element wavelength of 303.6nm. When the Ni content is 0.03%-0.7%, the wavelength of the analysis line is 300.2nm, and the reference line is the Zn element wavelength of 303.6nm.

[0044] The pre-combustion time was set to 10S and the exposure time to 4S. Only the flushing time was changed. The 1M GLV-4B zinc-nickel alloy standard was excited. The results (Table 3) showed that when the flushing time was >2S, the RSD value of the light intensity ratio of Al and Ni was <2%, and the data was stable. In order to save analysis time, the flushing time was selected as 2S.

[0045] Table 3 Light intensity ratio data at different flushing times

[0046]

[0047] The flushing time was set to 2S, the exposure time was set to 4S, and only the pre-combustion time was changed. The 1M GLV-4B zinc-nickel alloy standard was excited. The results (Table 4) showed that when the pre-combustion time was >8S, the RSD value of the light intensity ratio of Al and Ni was <2%, and the data was stable. In order to save analysis time, the pre-combustion time was selected as 8S.

[0048] Table 4 Light intensity ratio data for different pre-combustion time

[0049]

[0050] The flushing time was set to 2S, the pre-combustion time was set to 8S, and only the exposure time was changed to excite the 1M GLV-4B zinc-nickel alloy standard. The results (Table 5) showed that when the exposure time was >4S, the RSD value of the light intensity ratio of Al and Ni was <2%, and the data was stable. In order to save analysis time, the exposure time was selected as 4S.

[0051] Table 5 Light intensity ratio data for different pre-combustion time

[0052]

[0053] The direct reading spectrometer excitation parameters of each element are shown in Table 6.

[0054] Table 6 Direct reading spectrometer excitation parameter settings for each element

[0055]

[0056]

[0057] 3) Draw the working curve

[0058] Use a direct reading spectrometer to excite the zinc-nickel alloy standard, and draw the working curve of each element with the spectral intensity value of each element as the horizontal axis and the content of each element in the standard sample as the vertical axis. Figure 1 shown.

[0059] 4) Use a direct reading spectrometer to excite the zinc-nickel alloy sample, measure the spectral intensity value of each element, and obtain the content of each element according to the working curve in step 3).

[0060] Zinc-nickel alloy samples with low and high nickel contents were selected to carry out precision tests, and the results were read on the established working curves, as shown in Tables 7 and 8 below.

[0061] Table 7 Precision test results of low-content nickel-zinc-nickel alloy samples

[0062]

[0063] Table 8 Precision test results of high content nickel-zinc-nickel alloy samples

[0064]

[0065]

[0066] It can be seen from the above table that the method of the present invention has good repeatability and can meet the analysis requirements.

[0067] Two zinc-nickel alloy samples were randomly selected from the site, and the zinc-nickel alloy samples were processed into smooth planes using a lathe. They were excited on a direct reading spectrometer with set excitation parameters to obtain the spectral intensity values ​​of each element, and the content of each element was calculated based on the working curves of each element.

[0068] The two samples were analyzed for composition using the determination method of the present application and the ICP method. The comparison results of the two methods are shown in Table 9 below.

[0069] Table 9 Comparison results of the applied determination method and ICP component analysis

[0070]

[0071] As can be seen from the above table, the sample results measured by the determination method of the present application are in good agreement with the results measured by the ICP method. The present invention has high accuracy and reliability.

[0072] The embodiments of the present application have been described above, and the above description is exemplary, not exhaustive, and is not limited to the disclosed embodiments. Many modifications and changes will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments. The selection of terms used herein is intended to best explain the principles of the embodiments, practical applications, or improvements to the technology in the market, or to enable other persons of ordinary skill in the art to understand the embodiments disclosed herein.

Claims

1. A method for determining the content of components in a zinc-nickel alloy, characterized in that: The following steps are involved: 1) Preparing zinc-nickel alloy standard products; The content range of each element in the prepared zinc-nickel alloy standard is: Al element content is 0.0005%-0.3%, Fe element content is 0.0005%-0.035%, Pb element content is 0.0012%-0.035%, Cd element content is 0.0004%-0.031%, Sn element content is 0.0004%-0.031%, Cu element content is 0.0005%-0.035%, and Ni element content is 0.0005%-0.71%. 2) Set the direct reading spectrometer excitation parameters of each element. The analysis line and reference line of each element are: When the Al content is 0.0005%-0.03%, the wavelength of the analysis line is 396.2nm, and the reference line is the wavelength of the Zn element at 472.2nm; when the Al content is 0.03%-0.3%, the wavelength of the analysis line is 309.3nm, and the reference line is the wavelength of the Zn element at 303.6nm; When the Ni content is 0.0005%-0.03%, the wavelength of the analysis line is 341.5nm, and the reference line is the Zn element wavelength of 303.6nm. When the Ni content is 0.03%-0.7%, the wavelength of the analysis line is 300.2.6nm, and the reference line is the Zn element wavelength of 303.6nm. The wavelength of the Fe element analysis line is 372.2nm, and the reference line is the Zn element wavelength 303.6nm; The wavelength of the Pb element analysis line is 405.8nm, and the reference line is the Zn element wavelength 472.2nm; The wavelength of the Cd element analysis line is 228.8nm, and the reference line is the Zn element wavelength 196.9nm; The wavelength of the Sn element analysis line is 317.5nm, and the reference line is the Zn element wavelength 472.2nm; The wavelength of the Cu element analysis line is 223.0nm, and the reference line is the Zn element wavelength 196.9nm; 3) Draw the working curve; 4) Using a direct reading spectrometer to excite the zinc-nickel alloy sample, measuring the spectral intensity value of each element, and obtaining the content of each element according to the working curve described in step 3).

2. The method according to claim 1, characterized in that: In the step 2), the flushing time is 2 seconds, the pre-combustion time is 8 seconds, and the exposure time is 4 seconds.

3. The method according to claim 1, characterized in that: The preparation method of the zinc-nickel alloy standard in step 1) is: The zinc ingot is melted at 450-500°C, and after the zinc ingot is completely melted, the temperature is raised to 650-750°C, and a nickel ingot is added, stirred and melted, and then cast into a ZnNi10 master alloy; the mass ratio of the zinc ingot to the nickel ingot is 10:1; The zinc ingot is melted at 450-500°C to obtain zinc liquid; the aluminum ingot, iron sheet, cathode copper and ZnNi10 master alloy are melted at 700°C, the molten liquid is directly added to the zinc liquid and stirred rapidly; the temperature is lowered to 500-550°C, lead ingot, cadmium ingot and tin ingot are added, stirred and melted, and a zinc-nickel alloy standard is obtained after 10-20 minutes.

Images