Method for determining tungsten element by atomic emission spectrometry and application

Abstract

The invention discloses a method for determining a tungsten element by atomic emission spectrometry and application, and relates to the technical field of tungsten element determination. The invention relates to a method for determining a tungsten element by atomic emission spectrometry. The method comprises the following steps: S1, establishing a standard curve according to a reference line and an analysis line; s2, measuring the iron content in the sample to obtain the iron content of the sample; s3, calculating the tungsten content in the sample according to the standard curve; the tungsten content in the sample is 0.8-10%. The determination method provided by the invention can be used for testing a sample with relatively high tungsten content, and the test method is simple. The determination method can be applied to metallurgy, metal materials, mineral exploration, mineral development and quality control.

Description

Technical Field

[0001] The invention belongs to the technical field of tungsten element determination, and specifically is a method and application for determining tungsten element by atomic emission spectrometry. Background Art

[0002] The national standard "GB / T11170-2008" stipulates the determination of tungsten content in stainless steel by spark atomic emission spectrometry, which is applicable to the analysis range of 0.05% to 0.8%. For tungsten content beyond this range, the following two chemical analysis methods can be used: "YB / T 4395-2014": Determination of molybdenum, niobium and tungsten in steel by inductively coupled plasma atomic emission spectrometry. The sample is decomposed by hydrochloric acid, nitric acid and hydrofluoric acid, and phosphoric acid and perchloric acid are used to eliminate interference. If necessary, add internal standard elements, dilute and introduce them into the analyzer through atomization, and calculate the element mass fraction through the calibration curve. "GB / T223.43-2008": Provides gravimetric and spectrophotometric methods for determining tungsten content. The gravimetric method includes the cinchonine gravimetric method, which removes impurities through oxidation, precipitation, filtration, burning and other steps to obtain the mass of pure tungsten trioxide. The spectrophotometric method determines the tungsten content by acid dissolution, reduction, precipitation, extraction and measurement of absorbance.

[0003] There are some challenges in analyzing high-content tungsten in stainless steel using the two chemical analysis methods of "YB / T4395-2014" and "GB / T223.43-2008", mainly because they not only have a long analysis cycle and cannot meet the needs of rapid on-site analysis, but also the accuracy of the results is highly dependent on the technical level of the operator and is easily affected by human factors. Nevertheless, achieving rapid and accurate analysis of high-content tungsten in stainless steel is crucial for the development of new products, but several key technical difficulties must be overcome: First, the analysis range of existing spectrometers usually does not exceed 0.8%, and for higher content of tungsten, it exceeds its analysis capability, resulting in difficulty in ensuring precision and accuracy; second, due to the high content of metal elements such as chromium (Cr) and nickel (Ni) in stainless steel, the mutual interference between elements is more obvious, so it is necessary to reset the excitation conditions to exclude interfering elements and refit the working curve; finally, in the preparation process of stainless steel samples, the use of conventional milling parameters is prone to tool adhesion, resulting in an uneven sample surface, which may also affect the accuracy of the analysis results. Summary of the invention

[0004] The present invention solves at least one of the above technical problems and thus provides a method and application of determining tungsten by atomic emission spectrometry. The method is simple and can determine stainless steel samples with a tungsten content of ≥0.8%, and the determination method has high accuracy.

[0005] The present invention provides a method for determining tungsten by atomic emission spectrometry, comprising the following steps:

[0006] S1. Establish a standard curve based on the reference line and analytical line;

[0007] S2. Determine the iron content in the sample to obtain the iron content of the sample;

[0008] S3. Calculate the tungsten content in the sample according to the standard curve;

[0009] The tungsten content in the sample is 0.8-10%.

[0010] In S1, the equation of the standard curve is y=9.5E-15x 2 +3.1E-08x-2.1E-03;

[0011] Wherein, x is the spectral line intensity of tungsten element, and y is the concentration ratio of tungsten element.

[0012] In S3, the tungsten content = iron content * y * 100%.

[0013] In S1, the method for establishing a standard curve is to measure a sample with a known content, record and process the data, draw a curve, and then use a quadratic curve correction to eliminate interference from interfering elements to obtain a standard curve.

[0014] Further in S1, the data collection needs to collect data of at least 18 samples with known contents.

[0015] Further in S1, the interfering element includes at least one of Mo, Cr, Ti and V.

[0016] Further in S1, the content of the interfering element is ≤30%, preferably ≤25%.

[0017] Further in S1, the regression equation of the curve is y=1.0E-14x 2 +2.8E-08x-2.0E-03. In S1, the reference line selection method is to select different iron-based reference wavelengths to test standard substances, fix the iron content, measure the tungsten content, and select the iron-based reference wavelength when the standard deviation SD of the measurement result is ≤0.012%.

[0018] In S1, the reference line is an iron-based reference line, wherein the iron-based reference line includes 487.214nm, 390.648nm, 387.250nm, 383.633nm, 340.746nm and 339.933nm, preferably 390.648nm.

[0019] In S1, the analysis line is the analysis line wavelength of the tungsten element, wherein the analysis line wavelength is 400.875 nm.

[0020] In the present invention, the sample processing is obtained by grinding the sample to be tested with an abrasive belt.

[0021] Furthermore, the material of the abrasive belt is zirconium corundum.

[0022] Furthermore, the mesh number of the sanding belt is P60, P80 or P120.

[0023] Furthermore, the sample has a diameter of 20 to 80 mm and a thickness of 2 to 80 mm.

[0024] Furthermore, the upper and lower surfaces of the sample are parallel. Preferably, the sample can be a cylinder, a cuboid, or a cube.

[0025] Furthermore, the sample surface is clean, smooth and flat, has obvious and clear texture, and is free of pores and sand holes.

[0026] In S2, the method for determining the iron content in the sample is to use atomic emission spectroscopy to determine

[0027] In the present invention, an instrument preparation step is also included before the S1 step, and the instrument preparation step includes setting the spark source atomic emission spectrometry conditions and argon gas conditions, including:

[0028] (1) The flushing time of the analysis is 2.0 s;

[0029] (2) The pre-combustion time of the analysis is 8.0 s;

[0030] (3) The integration time of the analysis is 2.0 to 12.0 s;

[0031] (4) The excitation frequency of the spark source atomic emission spectrum is 400 to 500 Hz;

[0032] (5) The purity of the argon gas is ≥99.998%.

[0033] In the present invention, the method for determining tungsten by atomic emission spectrometry can also be used to determine the content of at least one element among C, Si, Mn, P, S, Ni, Cr, Cu, As, Sn, V, Ti, and Al in samples.

[0034] In the present invention, the sample analysis also includes a step of evaluating the accuracy of the tungsten content determination result; wherein the accuracy is evaluated using SD as the standard deviation, δ as the absolute deviation and r as the repeatability limit.

[0035] Furthermore, in the tungsten content determination result, 3SD≤r.

[0036] Furthermore, in the tungsten content measurement result, δ≤r.

[0037] Furthermore, |SD|=0.008-0.010%.

[0038] Furthermore, |δ|=0~0.03%.

[0039] The aforementioned atomic emission spectrometry method for determining tungsten is used in metallurgy, metal materials, mineral exploration, mineral development and quality control.

[0040] On the basis of being in accordance with the common sense in the art, the above-mentioned preferred conditions can be arbitrarily combined to obtain the preferred embodiments of the present invention.

[0041] Compared with the prior art, the present invention has the following beneficial effects:

[0042] 1. The sample preparation process of the present invention is concise and clear, and the determination method thereof is rapid and efficient, which is very suitable for the needs of rapid on-site analysis.

[0043] 2. The test range of the present invention is wide, and it can accurately measure samples with tungsten content reaching or exceeding 0.8wt%. At the same time, it also has the ability to measure elements such as C, Si, Mn, P, S, Ni, Cr, Cu, As, Sn, V, Ti and Al, ensuring the comprehensiveness and accuracy of the test.

[0044] 3. The test results of the present invention are highly accurate and repeatable. The standard deviation (|SD|) of the tungsten content determination results is within the range of 0.008-0.010%, and the relative deviation (|δ|) is within the range of 0-0.03%. In addition, all analysis results meet strict quality control standards, i.e., 3SD≤r and δ≤r, ensuring the reliability and consistency of the test results. BRIEF DESCRIPTION OF THE DRAWINGS

[0045] Figure 1 This is a diagram showing the effect of the processing method of the sample to be tested in Example 1 on the quality of the stainless steel sample.

[0046] Figure 2 This is a curve diagram before eliminating element interference in Example 4.

[0047] Figure 3 This is a curve chart after eliminating element interference in Example 4. DETAILED DESCRIPTION

[0048] In order to facilitate the understanding of the present invention, the present invention will be described more comprehensively and carefully in combination with preferred embodiments below, but the protection scope of the present invention is not limited to the following specific embodiments.

[0049] Unless otherwise defined, all professional terms used below have the same meanings as those generally understood by those skilled in the art. The professional terms used herein are only for the purpose of describing specific embodiments and are not intended to limit the scope of protection of the present invention.

[0050] The "range" disclosed in the present invention is defined in the form of a lower limit and an upper limit, and a given range is defined by selecting a lower limit and an upper limit, and the selected lower limit and upper limit define the boundaries of a particular range. The range defined in this way can be inclusive or exclusive of end values, and can be combined arbitrarily, that is, any lower limit can be combined with any upper limit to form a range. For example, if a range of 60-120 and 80-110 is listed for a specific parameter, it is understood that the range of 60-110 and 80-120 is also expected. In addition, if the minimum range values ​​1 and 2 are listed, and if the maximum range values ​​3, 4 and 5 are listed, the following ranges can all be expected: 1-3, 1-4, 1-5, 2-3, 2-4 and 2-5. In the present invention, unless otherwise specified, the numerical range "ab" represents an abbreviation of any real number combination between a and b, wherein a and b are real numbers. For example, the numerical range "0-5" represents that all real numbers between "0-5" have been fully listed herein, and "0-5" is just an abbreviation of these numerical combinations. In addition, when a parameter is expressed as an integer ≥ 2, it is equivalent to disclosing that the parameter is, for example, an integer of 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, etc.

[0051] If not otherwise specified, all embodiments and optional embodiments of the present invention can be combined with each other to form a new technical solution.

[0052] Unless otherwise specified, all technical features and optional technical features of the present invention can be combined with each other to form a new technical solution.

[0053] If not otherwise specified, all steps of the present invention may be performed sequentially or randomly, preferably sequentially. For example, the method includes steps (a) and (b), which means that the method may include steps (a) and (b) performed sequentially, or may include steps (b) and (a) performed sequentially. For example, the method may further include step (c), which means that step (c) may be added to the method in any order, for example, the method may include steps (a), (b) and (c), or may include steps (a), (c) and (b), or may include steps (c), (a) and (b), etc.

[0054] If there is no special explanation, the "include" and "comprising" mentioned in the present invention represent open-ended or closed-ended expressions. For example, the "include" and "comprising" may represent that other components not listed may also be included or only the listed components may be included or only the listed components may be included.

[0055] If not specifically stated, in the present invention, the term "or" is inclusive. For example, the phrase "A or B" means "A, B, or both A and B". More specifically, any of the following conditions satisfies the condition "A or B": A is true (or exists) and B is false (or does not exist); A is false (or does not exist) and B is true (or exists); or both A and B are true (or exist).

[0056] The testing method for iron content is: iron is the residual amount, 100% minus the content of other elements, the iron content is iteratively calculated, the first iron content is 100% to participate in the calculation to get the content of each element, after getting the content of each element, the iron content is calculated again, 100% minus the content of other elements is the iron content, and the accurate value of the content of each element is calculated again based on the iron content.

[0057] The testing method for other elements of the present invention is as follows: Atomic emission spectroscopy is used to test the content of other elements except iron, and other elements include: C, Si, Mn, P, S, Cr, Mo, Ni, Al, Co, Cu, Nb, Ti, V, W (reference content), Pb, Sn, As, Zr, Bi, Ca, Ce, Sb, B, Zn, La, and N.

[0058] The test spectra of other element contents are as follows:

[0059] C:193.091nm, Si:288.158nm, Mn:263.817nm, P:178.283nm, S:180.731nm, Cr:298.918nm, Mo:386.41 nm, Ni:218.55nm, Al:396.152nm, Co:288.615nm, Cu:324.753nm, Nb:313.079nm, Ti:337.28nm, V:310 .229nm, W:400.875nm, Pb:405.781nm, Sn:147.501nm, As:189.042nm, Zr:468.78nm, Bi:306.772nm, C a:393.366nm, Ce:456.236nm, Sb:217.518nm, B:182.64nm, Zn:206.2nm, La:433.374nm, N:149.263nm.

[0060] After measuring the content of each element according to the above spectrum, iron content = 100% - other element content.

[0061] The following examples and comparative examples use a SPECTROLAB S01 spectrometer CMOS detector, the selected spark source atomic emission spectrometry conditions are shown in Table 1, and the purity of argon gas is 99.999%.

[0062] Table 1 Light source conditions

[0063]

[0064] The standard substances or samples with known contents used in the following examples are specifically shown in Table 2.

[0065] Table 2 Content of each element in standard substances

[0066]

[0067] Example 1

[0068] This example explores the effect of the sample preparation method in S1 on the sample quality.

[0069] In this embodiment, YSBS11354a-2021 and YSBS11586-2018 are selected as samples, and the diameter of the samples is 35 mm and the height is 38 mm.

[0070] (1) The samples were processed using an automatic milling machine with a SANDVIK RCKT1204MO-PM 4220 blade. The blade is prone to becoming greasy during milling, resulting in many scratches and depressions on the surface of the sample. Figure 1 (a).

[0071] (2) Belt grinding: The belt material is zirconium corundum and the belt mesh is P60. The sample surface is clean, smooth, flat and has clear texture. Figure 1 (b).

[0072] Therefore, the following examples all selected the belt grinding method to prepare the samples.

[0073] Example 2

[0074] This example explores the influence of the abrasive belt material and mesh size on the measurement results.

[0075] (1) Selection of abrasive belt material: Standard materials YSBS11354a-2021 and YSBS11586-2018 were selected as the samples to be tested. The samples were prepared by abrasive belt grinding with abrasive belts made of silicon carbide, aluminum oxide, and zirconium corundum / P60, respectively. The samples were excited 10 times on the atomic emission spectrometer, and the test standard deviation SD results are shown in Table 3.

[0076] Table 3 Effect of abrasive belt material on standard deviation SD / % of test results

[0077] - Silicon Carbide Alumina Zirconia corundum YSBS11354a-2021 0.025 0.021 0.010 YSBS11586-2018 0.027 0.023 0.009

[0078] From the results in Table 3, it can be seen that when zirconium corundum is selected as the material of the abrasive belt, the test standard deviation is smaller and the precision is better, that is, the mesh size of the abrasive belt is selected when the standard deviation SD of the measurement result is ≤ 0.010%, so the abrasive belt made of zirconium corundum is selected.

[0079] (2) Selection of abrasive belt material: Standard materials YSBS11354a-2021 and YSBS11586-2018 were selected as the stainless steel samples to be tested, and zirconium corundum abrasive belts with mesh sizes of P40, P60, P80, and P120 were used for abrasive belt grinding. The prepared samples were excited 10 times on the atomic emission spectrometer (the test results were taken as the average of 10 times), and the standard deviation SD results of the tungsten content test were referred to Table 4.

[0080] Table 4 Effect of abrasive belt mesh on standard deviation SD / % of tungsten content test results

[0081] - P40 P60 P80 P120 YSBS11354a-2021 0.023 0.0096 0.011 0.012 YSBS11586-2018 0.025 0.01 0.0105 0.012

[0082] From the results in Table 4, it can be seen that when the abrasive belt is coarser, the analysis accuracy is poor. When it reaches P60 or above, the accuracy tends to be stable. Considering that further thinning will make the sample difficult to grind, a P60 abrasive belt is selected; that is, the mesh size of the abrasive belt is selected when the standard deviation SD of the measurement results is ≤0.010%.

[0083] The samples in the following examples were prepared by belt grinding using a zirconium corundum abrasive belt with a mesh size of P60 to obtain the samples.

[0084] Example 3

[0085] This example explores the effect of iron reference wavelength selection on the measurement results.

[0086] The iron-based reference wavelengths of 487.214 nm, 390.648 nm, 387.250 nm, 383.633 nm, 340.746 nm and 339.933 nm were selected for the samples of standard substances YSBS11354a-2021 and YSBS11586-2018, respectively. The samples were excited 10 times on the atomic emission spectrometer to determine the tungsten content (the tungsten element analysis line was 400.875 nm). The standard deviation SD of the tungsten content was shown in Table 5.

[0087] Table 5 Effect of iron reference wavelength on standard deviation SD / % of tungsten content test results

[0088]

[0089] From the results in Table 5, it can be seen that when the iron reference wavelength is selected as 390.648 nm, the tungsten content test results have good repeatability.

[0090] In the following examples, the tungsten element analysis line is selected to be 400.875 nm, and the iron reference wavelength is selected to be 390.648 nm.

[0091] Example 4

[0092] This example explores the effect of interference from interfering elements on the accuracy of the determination, and uses a quadratic curve correction to eliminate the interference from interfering elements to obtain a standard curve.

[0093] The upper limit of tungsten element analysis in GB / T 11170-2008 is 0.8%, and it is impossible to analyze high tungsten above 0.8%. This embodiment uses the full spectrum scanning and online real-time drift correction function of the CMOS detector of the SPECTROLAB S01 spectrometer. First, the air light chamber, ultraviolet light chamber lens and spark stand of the spectrometer are fully maintained. After the normal data of the excitation spot is stable, iCAL intelligent standardization and global standardization are performed to confirm that the parameters and element linearity of the instrument are normal.

[0094] The samples with known contents in Table 6 were selected as the samples to be tested and processed with zirconium corundum P60 abrasive belt to obtain their samples.

[0095] Table 6 The content of each element in samples with known content

[0096] Samples with known content content 1A-422 W 1.28%, Mo 0.033%, Fe 90.00% 1A-423 W 2.06%, Mo 0.027, Fe 90.50% 1A-424 W 3.02%, Mo 0.036%, Fe 90.50% 1J-C 700-1 W 1.3%, Mo 1.02%, Cr 0.72%, Ti 0.144%, V 0.3%, Fe 93.50% 1J-C 700-2 W 0.9%, Mo 0.266%, Cr 0.35%, Ti 0.483%, V 0.446%, Fe 89.40% 1I-BS-TM1 W 1.7%, Mo 8.4%, Cr 3.72%, V 1.05%, Fe 78.00% 1-MAW6 W 1.04%, Mo 0.16%, Cr 0.22%, V 0.043%, Fe 91.54% 1N-CRM 189A W 1.3%, Mo 0.837%, Cr 1.065%, Ti 0.326%, V 0.054%, Fe 87.00% 1U-SUS-1R W 0.7%, Mo 0.9%, Cr 1.7%, V 0.5%, Fe 92.20% 3I-C 810-1 W 2.46%, Mo 1.44%, Cr 18.23%, Ti 2.79%, V 0.01%, Fe 38.10% 3I-C 810-2 W 2.24%, Mo 1.66%, Cr 16.61%, Ti 2.624%, Fe 37.90% 3G-C 800-1 W 6.02%, Cr 24.01%, Ti 0.46%, Fe 31.85% 3G-C 800-2 W 4.65%, Cr 22.84%, Ti 0.70%, Fe 32.30% 3G-C 800-3 W 3.21%, Cr 21.09%, Ti 0.97%, Fe 32.80% 3G-C 800-4 W 2.37%, Cr 19.42%, Ti 1.23%, Fe 32.80% 3G-C 800-5 W 1.69%, Cr 18%, Ti 1.61%, Fe 31.30% 3N-MBH 162 W 2.38%, Mo 2.83%, Cr 21.60%, Ti 0.023%, Fe 42.61% 3J-C 820-3 W 0.71%, Mo 0.69%, Cr 9.32%, Ti 0.51%, Fe 84.50%

[0097] According to the measured tungsten element spectral line intensity (x) and the tungsten content in the sample with known content (y = tungsten content / iron content / 100%), a xy relationship curve is drawn, and the regression equation of the curve is obtained by the least squares method: y = 1.0E-14x 2 +2.8E-08x-2.0E-03, the curve has a large dispersion, see Figure 2 .

[0098] After eliminating the interference of Mo / Cr / Ti / V using the quadratic curve equation, the standard curve equation y=9.5E is obtained. - 15x 2 +3.1E-08x-2.1E-03, the dispersion of the standard curve is reduced, see Figure 3 .

[0099] Example 5

[0100] This embodiment is based on y=9.5E-15x obtained in embodiment 4 2+3.1E-08x-2.1E-03 standard curve is used to measure the tungsten content in various substances with known contents. To explore the absolute deviation δ of the analysis results, the measured tungsten element spectral line intensity x is substituted into the standard curve equation to calculate y, tungsten content (%) = iron content * y * 100%, and the calculation results are shown in Table 7.

[0101] Table 7 Calculation of tungsten content

[0102]

[0103] Example 6

[0104] This embodiment is based on y=9.5E-15x obtained in embodiment 4 2 The +3.1E-08x-2.1E-03 standard curve was used to measure the tungsten content in the standard substances YSBS11354a-2021 and YSBS11586-2018 to explore the accuracy of the analysis results, see Table 8. Among them, the r value is derived from GB / T20124-2006.

[0105] Table 8 Accuracy of analysis results

[0106]

[0107]

[0108] Example 7

[0109] In this example, the tungsten content in any sample is measured according to the standard curve obtained in Example 4 to explore the reproducibility of the analysis results.

[0110] The iron content test process is shown in Table 9 below.

[0111] Table 9 Content of each element in the sample / %

[0112]

[0113]

[0114] Equipment and instruments in Lian Tempering Room 3: SPECTROLAB S01 spectrometer;

[0115] Equipment and instruments in Hengguan Laboratory: OBLF QSG750-II spectrometer.

[0116] Five rackets (numbered 23107956, 23107958, 23107959, 23107960, 23107961) and one blank sample (marked as blank sample A) were selected as the test objects. The six samples were measured by spark source atomic emission spectrometry in the Lianhua Tempering Room 3 and Hengguan Laboratory. Each sample was tested three times independently, and the average value was taken to ensure the accuracy of the results. The specific test results are shown in Table 10.

[0117] Table 10 Accuracy of analysis results

[0118] Sample No. Lian Tempered Glass Room 3 Laboratory Deviation δ δ≤r Sample A 1.73 1.73 0 satisfy 23107956 1.72 1.7 -0.02 satisfy 23107958 1.67 1.68 0.01 satisfy 23107959 1.71 1.71 0 satisfy 23107960 1.71 1.69 -0.02 satisfy 23107961 1.74 1.74 0 satisfy

[0119] Unless otherwise specified, various raw materials, reagents, instruments and equipment used in the present invention can be purchased from the market or prepared by existing methods. The specific embodiments described above further describe the purpose, technical solutions and beneficial effects of the present invention in detail. It should be understood that the above description is only a specific embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for determining tungsten by atomic emission spectrometry. It is characterized in that The following steps are involved: S1. Establish a standard curve based on the reference line and analytical line; S2. Determine the iron content in the sample to obtain the iron content of the sample; S3. Calculate the tungsten content in the sample according to the standard curve; The tungsten content in the sample is 0.8-10%.

2. The method for determining tungsten by atomic emission spectrometry according to claim 1, It is characterized in that The equation of the standard curve is y=9.5E-15x 2 +3.1E-08x-2.1E-03; where x is the spectral line intensity of tungsten element and y is the concentration ratio of tungsten element.

3. The method for determining tungsten by atomic emission spectrometry according to claim 2, It is characterized in that The tungsten content=iron content*y*100%.

4. The method for determining tungsten by atomic emission spectrometry according to claim 1, It is characterized in that The method for establishing a standard curve is to measure samples with known contents, record and process data, draw a curve, and then use a quadratic curve to correct and eliminate interference from interfering elements to obtain a standard curve.

5. The method for determining tungsten by atomic emission spectrometry according to claim 4, It is characterized in that Satisfy at least one of the following conditions (1) to (4): (1) The data collection requires collecting data from at least 18 samples with known contents; (2) The interfering element includes at least one of Mo, Cr, Ti and V; (3) The content of the interfering element is ≤30%; (4) The regression equation of the curve is y = 1.0E-14x 2 +2.8E-08x-2.0E-03.

6. The method for determining tungsten by atomic emission spectrometry according to claim 1, It is characterized in that Satisfy at least one of the following conditions (1) to (3): (1) The method for selecting the reference line is to select different iron-based reference wavelengths to test standard substances, fix the iron content, measure the tungsten content, and select the iron-based reference wavelength when the standard deviation SD of the measurement results is ≤0.012%; (2) The reference line is an iron-based reference line, wherein the iron-based reference line includes 487.214 nm, 390.648 nm, 387.250 nm, 383.633 nm, 340.746 nm and 339.933 nm; (3) The analysis line is the analysis line wavelength of tungsten element, wherein the analysis line wavelength is 400.875 nm.

7. The method for determining tungsten by atomic emission spectrometry according to claim 1, It is characterized in that The sample processing is obtained by grinding the sample to be tested with an abrasive belt.

8. The method for determining tungsten by atomic emission spectrometry according to claim 7, It is characterized in that Satisfy at least one of the following conditions (1) to (4): (1) The material of the abrasive belt is zirconium corundum; (2) The mesh number of the abrasive belt is P60, P80 or P120; (3) The sample has a diameter of 20 to 80 mm and a thickness of 2 to 80 mm; (4) The upper and lower surfaces of the sample are parallel.

9. The method for determining tungsten by atomic emission spectrometry according to claim 1, It is characterized in that Before the step S1, an instrument preparation step is also included, and the instrument preparation step includes setting the spark source atomic emission spectrometry conditions and argon gas conditions, including: (1) The flushing time of the analysis is 2.0 s; (2) The pre-combustion time of the analysis is 8.0 s; (3) The integration time of the analysis is 2.0 to 12.0 s; (4) The excitation frequency of the spark source atomic emission spectrum is 400 to 500 Hz; (5) The purity of the argon gas is ≥99.998%.

10. Application of the method for determining tungsten by atomic emission spectrometry according to any one of claims 1 to 9 in metallurgy, metal materials, mineral exploration, mineral development and quality control.

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