Method for detecting content of partial elements in diamond cutting wire

Abstract

The invention provides a method for detecting the content of part of elements in a diamond cutting wire, which comprises the following steps: sequentially dissolving a sample by adopting a nitric acid solution and a hydrochloric acid solution to prepare a to-be-detected sample solution; and testing the to-be-tested sample solution by adopting the inductively coupled plasma emission spectrometry, and calculating the content of partial elements in the to-be-tested sample solution according to the standard curve. The detection method provided by the invention is simple and rapid, has a wide determination range, can be suitable for determining the recovered nickel-containing diamond wire sample with the nickel content of 10.0%-35.0%, the silicon, manganese, chromium and copper content of 0.010%-1.00% and the phosphorus content of 0.010%-0.200%, realizes one-time sample dissolution synchronous determination of main elements and secondary elements, and has the advantages of high detection accuracy and high detection precision. And the requirement of accurate element analysis when the recycled material is applied in ferrous metallurgy can be met.

Description

Technical Field

[0001] This application relates to the technical field of metallurgical chemical analysis and detection, and particularly to a method for detecting the content of some elements in diamond cutting wire. Background Art

[0002] Nickel-containing diamond cutting wire is a metal product with high strength, wear resistance and corrosion resistance, and is used for the recycled materials after slicing solar polysilicon and monocrystalline silicon. Its nickel content is 20%-30%. Nickel element is commonly used as an alloying element in steel smelting, which can improve the strength, toughness, corrosion resistance, high-temperature performance, etc. of steel. Especially, the usage amount of stainless steel and high-nickel steel grades is relatively high. Usually, alloying is carried out by adding nickel-containing materials such as ferronickel and metallic nickel, but the cost is very high.

[0003] Using recycled nickel-containing diamond cutting wire instead of ferronickel and metallic nickel can effectively reduce the production cost. Therefore, understanding and accurately detecting the content of nickel element and main impurity elements such as silicon, manganese, chromium, copper, zinc, and phosphorus in recycled nickel-containing diamond cutting wire has important guiding significance for the correct application of diamond wire in steel smelting. At present, there is no test method and standard for the content of nickel, silicon, manganese, chromium, copper, zinc, and phosphorus in recycled nickel-containing diamond cutting wire. Summary of the Invention

[0004] This application is made in view of the above problems, and its purpose is to provide a method for detecting the content of some elements in diamond cutting wire.

[0005] Specifically, the first aspect of this application provides a method for detecting the content of some elements in diamond cutting wire, including the following steps:

[0006] Dissolve the sample successively with nitric acid solution and hydrochloric acid solution to prepare a sample solution to be measured;

[0007] After testing the sample solution to be measured by inductively coupled plasma optical emission spectrometry, calculate the content of some elements in the sample solution to be measured according to the standard curve.

[0008] Further, when adding the nitric acid solution to the sample, it is in a slightly boiling state, the temperature is 100-110°C. After adding the nitric acid solution and hydrochloric acid solution, heat to keep the temperature within 100-200°C to completely dissolve the sample.

[0009] Further, the mass concentration of the nitric acid solution is 30%-50%.

[0010] Further, the mass of the nitric acid solution is 120-200 times the mass of the sample.

[0011] Further, the nitric acid solution is pre-heated to the boiling state before adding it to the sample.

[0012] Further, the mass concentration of the hydrochloric acid solution is 36%-38%.

[0013] Further, the mass of the hydrochloric acid solution is 40-60 times the mass of the sample.

[0014] Further, when using inductively coupled plasma optical emission spectrometry for testing, the characteristic ICP analysis lines for determining nickel, silicon, manganese, chromium, copper, zinc, and phosphorus elements are selected. The characteristic ICP analysis line for nickel element is 231.604nm and 341.476nm, the characteristic ICP analysis line for silicon element is 251.611nm; the characteristic ICP analysis line for manganese element is 257.610nm; the characteristic ICP analysis line for chromium element is 267.716nm; the characteristic ICP analysis line for copper is 324.754nm; the characteristic ICP analysis line for zinc element is 206.200nm; the characteristic ICP analysis line for phosphorus element is 178.284nm.

[0015] Further, during the test using inductively coupled plasma optical emission spectrometry, the analysis pump speed is 45-55 / rpm, and the flushing pump speed is 90-110 / rpm.

[0016] Further, during the test using inductively coupled plasma optical emission spectrometry, the auxiliary gas flow rate is 0.3-0.5 / L / min, and the nebulizer gas flow rate is 0.6-0.8 / L / min.

[0017] Further, in step S1, the size of the diamond cutting wire sample is less than 1 cm.

[0018] The present invention has the following beneficial effects:

[0019] (1) The present invention uses a nitric acid solution to quickly dissolve the sample to prevent the passivation of nickel, and then adds a hydrochloric acid solution. By using the reducibility and acidity of hydrochloric acid, the generation of manganese precipitation is reduced, and the polymerization of silicic acid is prevented, so that nickel, silicon, manganese, chromium, copper, zinc, and phosphorus in the sample can be quickly and completely dissolved into the solution, diluted to a certain volume, analyzed and detected by ICP-OES, measure the spectral intensity of each element, and calculate the mass fraction of each element to be measured through a series of standard curves prepared from iron matrix and standard solutions. The detection results have high accuracy.

[0020] (2) This application solves the problem that there is no suitable method for detecting nickel, silicon, manganese, chromium, copper, zinc, and phosphorus in recycled nickel-containing diamond cutting wires. The analysis process is simple and fast, the measurement range is wide, and it can be applied to samples with nickel content in recycled nickel-containing diamond wires ranging from 10.0% to 35.0%, silicon, manganese, chromium, and copper content ranging from 0.010% to 1.00%, and phosphorus content ranging from 0.010% to 0.200%. It realizes the simultaneous determination of major and minor elements in one sample dissolution, and can meet the requirements of accurate element analysis when the recycled material is used in iron and steel metallurgy. Brief Description of the Drawings

[0021] To more clearly illustrate the technical solutions in the embodiments of the present drawings or the prior art, the following will briefly introduce the drawings required for use in the description of the embodiments or the prior art. Obviously, the drawings in the following description are only some embodiments of the present drawings. For those of ordinary skill in the art, without creative efforts, other drawings can be obtained based on the structures shown in these drawings.

[0022] Figure 1 It is a schematic diagram of the sample processing of the present invention;

[0023] Figure 2 It is a standard curve graph of the nickel analysis line 231.604nm;

[0024] Figure 3 It is a standard curve graph of the nickel analysis line 341.476nm;

[0025] Figure 4 It is a standard curve graph of the silicon analysis line 251.611nm;

[0026] Figure 5 It is a standard curve graph of the manganese analysis line 257.610nm

[0027] Figure 6 It is a standard curve graph of the chromium analysis line 267.716nm;

[0028] Figure 7 It is a standard curve graph of the copper analysis line 324.754nm;

[0029] Figure 8 It is a standard curve graph of the zinc analysis line 206.200nm;

[0030] Figure 9 It is a standard curve graph of the phosphorus analysis line 178.284nm.

[0031] The realization, functional features and advantages of the purpose of the present drawings will be further described with reference to the embodiments and the drawings. Detailed Embodiments

[0032] In order to make the purpose, technical solutions and advantages of the present application more clear and understandable, the following will describe and explain the present application in combination with embodiments. It should be understood that the specific embodiments described herein are only used to explain the present application and are not used to limit the present application. Based on the embodiments provided in the present application, all other embodiments obtained by those of ordinary skill in the art without creative efforts belong to the scope of protection of the present application.

[0033] Obviously, the following description is only some examples or embodiments of the present application. For those of ordinary skill in the art, without creative efforts, the present application can also be applied to other similar scenarios. In addition, it can also be understood that although the efforts made in such a development process may be complex and lengthy, for those of ordinary skill in the art related to the content disclosed in the present application, some design, manufacturing, or production changes based on the technical content disclosed in the present application are only conventional technical means and should not be understood as the content disclosed in the present application being insufficient.

[0034] A method for detecting the content of some elements in a diamond cutting wire, comprising the following steps:

[0035] Dissolve the sample successively with nitric acid solution and hydrochloric acid solution to obtain a sample solution to be tested;

[0036] After testing the sample solution to be tested by inductively coupled plasma emission spectrometry, calculate the content of some elements in the sample solution to be tested according to the standard curve.

[0037] Furthermore, the method for detecting the content of some elements in the diamond cutting wire comprises the following steps:

[0038] Step S1: Take samples from different parts of the diamond cutting wire and mix them for standby;

[0039] Step S2: Weigh a quantitative sample, add nitric acid solution preheated to slight boiling to the sample for rapid heating and decomposition. After the sample is basically dissolved, add hydrochloric acid solution and continue heating until the sample is completely dissolved to obtain a sample solution to be tested;

[0040] Step S3: Weigh high-purity iron, a reference substance with the same mass as the sample to be tested, and prepare a blank solution according to the treatment method in Step S2;

[0041] Step S4: Weigh a quantitative amount of high-purity iron, add a quantitative amount of nitric acid solution and hydrochloric acid solution to the high-purity iron, heat and dissolve it completely, transfer it to a volumetric flask, and successively add nickel, silicon, manganese, chromium, copper, zinc, and phosphorus standard solutions to it until the content of each element covers the sample analysis range, with points evenly distributed during this period, and dilute to the scale to prepare a series of standard solutions;

[0042] Step S5: Measure the emission light intensity of the series of standard solutions by inductively coupled plasma emission spectrometry to construct a standard curve;

[0043] Step S6: Measure the blank solution and the sample solution to be tested successively by inductively coupled plasma emission spectrometry, and calculate the content of nickel, silicon, manganese, chromium, copper, zinc, and phosphorus elements in the sample solution according to the standard curve in Step S5.

[0044] The nitric acid solution is pre-heated to the boiling state and then added to the sample. In the present invention, a slightly boiling nitric acid solution is used to rapidly dissolve the sample, preventing the passivation of nickel. A hydrochloric acid solution is added to utilize the reducing property and acidity of hydrochloric acid to reduce the generation of manganese precipitation and prevent the polymerization of silicic acid, enabling nickel, silicon, manganese, chromium, copper, zinc, and phosphorus in the sample to be rapidly and completely dissolved into the solution. It is diluted to a certain volume and analyzed and detected by ICP-OES to measure the spectral intensities of various elements. The mass fractions of the elements to be measured are calculated through a series of standard curves prepared from an iron matrix and a standard solution, and the detection results are highly accurate.

[0045] In an embodiment of the present application, the step S1 further includes cutting the recycled nickel-containing diamond cutting wire from different parts under latex protective gloves and mixing it into a sample bag. Before weighing the sample, the analyst cleans and wipes the scissors with ethanol, and cuts different cross-sections into fine chips less than 1 cm under the premise of laying a clean white paper below to obtain no less than 5 g of the sample for analysis and mixing.

[0046] In an embodiment of the present application, the mass concentration of the nitric acid solution is 30%-50%. The nitric acid solution can be prepared from concentrated nitric acid and water. For example, it is prepared by mixing concentrated nitric acid with a mass fraction of about 65% and a density of 1.42 g / mL and water in a volume ratio of 1:1. The mass of the nitric acid solution is 120-200 times the mass of the sample. The mass concentration of the hydrochloric acid solution is 36%-38%, and the dosage of the hydrochloric acid solution is 40-60 times the dosage of the sample.

[0047] Specifically, 0.09-0.11 g of the fine chip sample is quantitatively weighed into a 250 mL beaker, and 15 mL of the nitric acid solution pre-heated to slightly boiling is added for rapid decomposition by heating to prevent the passivation of nickel. The nitric acid is of analytical purity, with a mass fraction of about 69% and a density of 1.42 g / mL. The nitric acid solution is prepared by mixing concentrated nitric acid and water in a volume ratio of 1:1, and the dosage is 120-200 times the amount of the sample. After the sample is basically dissolved, 5 mL of the hydrochloric acid solution is added to utilize the reducing property and acidity of hydrochloric acid to reduce the generation of manganese precipitation and prevent the polymerization of silicic acid. The hydrochloric acid is of analytical purity, with a mass fraction of 37% and a density of 1.19 g / mL, and the dosage is 40-60 times the amount of the sample. Continue to heat until nickel, silicon, manganese, chromium, copper, zinc, and phosphorus in the sample can be rapidly and completely dissolved into the solution. During this period, water is added to rinse the inner wall of the beaker to prevent the sample from sticking to the cup wall and keep the solution volume constant. Then it is transferred to a 200 mL volumetric flask and diluted to the mark, and mixed evenly for measurement.

[0048] In the embodiments of the present application, the preparation of the series of standard curve solutions in step S4 is specifically as follows: Weigh 5 portions of high-purity iron, each portion being 0.070 g, and place them in 5 beakers respectively. Add 15 mL of nitric acid solution (concentrated nitric acid and water in a ratio of 1:1) and 5.0 mL of hydrochloric acid solution to each beaker to completely dissolve the high-purity iron. Then transfer the solution to a 200 mL volumetric flask, which is equivalent to a 70% iron content based on a 0.10 g sample, so that the iron content in the standard solution matches the iron content in the sample solution. The high-purity iron used is high-purity iron as a reference material, numbered GBW01402-f, with an iron content of 99.98%. The amount of acid used to prepare the matrix is also the same as that of the sample to ensure that the acidity of the calibration curve solution is consistent with that of the sample.

[0049] It should be noted that all reagents used in the present invention are of analytical purity or prepared from analytical purity reagents, and all standard solutions used for preparing the standard curve are national standard solutions.

[0050] In the embodiments of the present application, the standard curve contains 5 points. The preparation of the series of standard curve solutions in step S4 further includes adding 0.0, 10.0, 20.0, 25.0, 35.00 mL of 1000 μg / mL nickel standard solution, 0.0, 0.40, 0.60, 1.20, 2.00 mL of 500 μg / mL silicon standard solution, 0.0, 0.20, 0.40, 0.60, 1.00 mL of 1000 μg / mL manganese, chromium, copper, zinc standard solution, and 0.0, 0.40, 1.0, 2.0, 4.0 mL of 50 μg / mL phosphorus standard solution to the 5 beakers respectively.

[0051] The nickel mass contents calculated based on a 0.1000 g sample are 0.00, 10.00, 20.00, 25.00, 35.00% in sequence; the silicon mass contents calculated based on a 0.1000 g sample are 0.00, 0.20, 0.40, 0.60, 1.00% in sequence; the manganese, chromium, copper, zinc mass contents calculated based on a 0.1000 g sample are 0.00, 0.20, 0.40, 0.60, 1.00% in sequence; the phosphorus mass contents calculated based on a 0.1000 g sample are 0.00, 0.020, 0.050, 0.100, 0.200% in sequence.

[0052] The nickel standard solution is a national standard solution with the number GBW(E)080603, a concentration of 1000 μg / mL, and a medium of 5% (v / v) HNO3 solution; the silicon standard solution is a national standard solution with the number GBW(E)080577, a concentration of 500 μg / mL, and a medium of 0.5% (m / v) Na2CO3 solution; the manganese standard solution is a national standard solution with the number GBW(E)080600, a concentration of 1000 μg / mL, and a medium of 10% (v / v) HNO3; the chromium standard solution is a national standard solution with the number GSB G62017-90, a concentration of 1000 μg / mL, and a medium of 10% (v / v) HCl; the copper standard solution is a national standard solution with the number GSB(E)080605, a concentration of 1000 μg / mL, and a medium of 10% (v / v) HCl; the zinc standard solution is a national standard solution with the number GBW(E)080607, a concentration of 1000 μg / mL, and a medium of 10% (v / v) HCl; the 50 μg / mL phosphorus standard solution is obtained by pipetting 5.00 mL of the national phosphorus standard solution with the number GBW(E)080584, a concentration of 1000 μg / mL, and a medium of H2O into a 100 mL volumetric flask and diluting to the mark with water and mixing well.

[0053] In the embodiments of the present application, when using inductively coupled plasma emission spectrometry for testing, the characteristic ICP analysis lines of nickel, silicon, manganese, chromium, copper, zinc, and phosphorus elements are selected and determined. The characteristic ICP analysis lines of nickel element are 231.604 nm and 341.476 nm, the characteristic ICP analysis line of silicon element is 251.611 nm; the characteristic ICP analysis line of manganese element is 257.610 nm; the characteristic ICP analysis line of chromium element is 267.716 nm; the characteristic ICP analysis line of copper is 324.754 nm; the characteristic ICP analysis line of zinc element is 206.200 nm; the characteristic ICP analysis line of phosphorus element is 178.284 nm.

[0054] In the embodiments of the present application, step S5 further includes sequentially analyzing the 0-4 point standards of the standard curve solution to obtain the spectral intensities of nickel, silicon, manganese, chromium, copper, zinc, and phosphorus elements, and drawing a standard curve through the concentrations and intensities of each element. Further, step S5 also includes checking the linear correlation of the standard curve. The correlation coefficient r of nickel element is >0.9995, and the correlation coefficients r of silicon, manganese, chromium, copper, zinc, and phosphorus elements are >0.999.

[0055] Select and optimize the characteristic ICP analysis lines and instrument parameters for nickel, silicon, manganese, chromium, copper, zinc, and phosphorus elements by selecting the midpoint of the prepared standard working curve. Analyze the standard solution in sequence to obtain the spectral intensities of nickel, silicon, manganese, chromium, copper, zinc, and phosphorus elements, and draw a calibration curve through the concentration and intensity of each element. Check the linearity of the calibration curve through the linear correlation of the calibration curve. The correlation coefficient r of nickel element is required to be >0.9995, and the correlation coefficient r of silicon, manganese, chromium, copper, zinc, and phosphorus elements is required to be >0.999.

[0056] In the embodiments of the present application, the test conditions for inductively coupled plasma emission spectrometry in steps S5 and S6 are: the analysis pump speed is 45 - 55 / rpm, and the flushing pump speed is 90 - 110 / rpm; the auxiliary gas flow rate is 0.3 - 0.5 / L / min, and the nebulizer gas flow rate is 0.6 - 0.8 / L / min.

[0057] The reagents used in the following examples:

[0058] a) Nitric acid solution: Nitric acid 1 + 1, density about 1.42 g / mL, analytical pure, mass fraction of 65% concentrated nitric acid and water are mixed in a volume ratio of 1:1 and mixed before use;

[0059] b) Hydrochloric acid: Density about 1.19 g / mL, analytical pure, mass fraction of 37%;

[0060] c) High-purity iron GBW01402-f, iron mass content 99.98%;

[0061] d) Nickel standard solution, numbered GBW(E)080603, concentration 1000 ug / mL, medium is 5% HNO3 solution by volume concentration;

[0062] e) Silicon standard solution, numbered GBW(E)080577, concentration 500 ug / mL, medium is 0.5% Na2CO3 solution by mass-volume concentration;

[0063] f) Manganese standard solution, numbered GBW(E)080600, concentration 1000 ug / mL, medium is 10% HNO3 solution by volume concentration;

[0064] g) Chromium standard solution, numbered GSB G62017-90, concentration 1000 ug / mL, medium is 10% HCl solution by volume concentration;

[0065] h) Copper standard solution, numbered GSB(E)080605, concentration 1000 ug / mL, medium is 10% HCl solution by volume concentration;

[0066] i) Zinc standard solution, numbered GBW(E)080607, concentration 1000 ug / mL, medium is 10% HCl solution by volume;

[0067] j) Phosphorus standard solution, concentration 50 ug / mL. Pipette 5.00 mL of phosphorus national standard solution, numbered GBW(E)080584, concentration 1000 ug / mL, medium H2O solution into a 100 mL volumetric flask and dilute to the mark with water and mix well to obtain;

[0068] k) Standard substance: High-purity metallic nickel, Central Iron and Steel Research Institute, nickel purity 99.99%.

[0069] l) Low-alloy steel (all mass fractions): GSBH40080-94, nickel 0.121%, silicon 0.520%, manganese 0.75%, chromium 0.202%, copper 0.243%, phosphorus 0.034%;

[0070] m) Low-alloy steel (all mass fractions): GSBH40031-93, nickel 0.026%, silicon 0.228%, manganese 0.55%, chromium 0.035%, copper 0.034%, phosphorus 0.017%;

[0071] n) Low-alloy steel (all mass fractions): GSB03-2454-2008, nickel 0.409%, silicon 0.109%, manganese 0.151%, chromium 0.164%, copper 0.154%, phosphorus 0.039%;

[0072] o) Standard sample: Ferronickel, numbered GBW(E)010423, nickel 10.70%, manganese 0.053%, copper 0.021%, phosphorus 0.032%.

[0073] Instrumentation equipment:

[0074] Inductively coupled plasma emission spectrometer. The minimum experimental resolution of the spectrometer: Calculate the spectral bandwidth for the selected analysis line, and this bandwidth must be less than 0.03 nm; The minimum short-term precision: The standard deviation of the average value of the absolute intensity or relative intensity does not exceed 0.4%.

[0075] Testing instrument: Thermo Scientific ICAP 6300 full-spectrum direct-reading scanning type inductively coupled plasma atomic emission spectrometer, detector CID, quartz injection system. The testing working parameters are shown in Table 1.

[0076] Table 1 Testing working parameters

[0077]

[0078] Medium-temperature electric furnace, 1000 W, temperature adjustable;

[0079] Sampling equipment: balance, precision 0.01 g; electronic balance, precision 0.1 mg;

[0080] Apparatus materials: 250 mL beaker, 200 mL volumetric flask, 10 mL, 5 mL, 2 mL, 1 mL pipettes, 10 mL measuring cylinder;

[0081] Others: Common tool materials for chemical wet experiments such as sampling tools.

[0082] Example 1

[0083] A method for detecting the content of some elements in diamond cutting wire, comprising the following steps:

[0084] Step S1: Sample processing

[0085] Refer to Figure 1 , while wearing latex protective gloves, cut the recycled nickel-containing diamond cutting wire from different parts and mix it into a sample bag. Before sampling, the analyst cleans and wipes the scissors with ethanol, and cuts different cross-sections into appropriate-sized fine chips on a clean white paper pad to obtain 5 g of sample for analysis and mix;

[0086] Step S2: Dissolve the sample to prepare a solution

[0087] Weigh 0.1000 g of the fine chip sample, place the sample in a 250 mL beaker, add 15 mL of nitric acid solution (volume ratio of concentrated nitric acid (mass fraction 65%) to water is 1:1) preheated to 105°C ± 5°C and slightly boiling, and heat it to 120°C - 150°C with a 200°C low-temperature electric furnace to quickly dissolve the sample. During this period, shake continuously to prevent the sample from adhering to the cup wall, and make up water to keep the solution volume unchanged. After the sample is basically decomposed, add 5 mL of hydrochloric acid (mass fraction 37%), continue to heat to maintain the temperature at 120°C - 150°C until the sample is completely dissolved, take it off and cool it, transfer it to a 200 mL volumetric flask, dilute it to the mark, and shake well. Synchronously weigh 0.0700 g of high-purity iron powder to prepare a blank test solution (high-purity iron powder is high-purity iron GBW01402-f, iron mass content 99.98%);

[0088] Step S3: Drawing of the standard curve

[0089] Weigh 5 portions of high-purity iron powder, each portion being 0.070 g, and place them in 5 250-mL beakers. Add 15 mL of nitric acid 1+1 solution (the volume ratio of concentrated nitric acid (mass fraction 65%) to water is 1:1), and add 5.0 mL of hydrochloric acid (mass fraction 37%). Heat to completely dissolve, transfer to a 200-mL volumetric flask. According to the content of the elements to be measured in the sample, successively add nickel, silicon, manganese, chromium, copper, zinc, and phosphorus standard solutions until the nickel content range calculated based on 0.1000 g of the sample is 0.00% - 35.00%, the silicon, manganese, chromium, copper, and zinc content ranges are 0.00% - 1.00%, and the phosphorus content range is 0.000% - 0.200%. Distribute the points evenly during this period, dilute to the mark, and shake well. See Table 2 below for details;

[0090] Table 2 Standard Curve Preparation Table

[0091]

[0092] See Figures 2 to 9 , use an inductively coupled plasma emission spectrometer to detect the above standard solutions and draw a standard curve. Select and optimize the characteristic ICP analysis lines and instrument parameters of nickel, silicon, manganese, chromium, copper, zinc, and phosphorus elements by introducing the third point of the prepared standard curve. After testing, finally confirm that the characteristic ICP analysis lines of nickel element are 231.604 nm and 341.476 nm, the characteristic ICP analysis line of silicon element is 251.611 nm; the characteristic ICP analysis line of manganese element is 257.610 nm; the characteristic ICP analysis line of chromium element is 267.716 nm; the characteristic ICP analysis line of copper is 324.754 nm; the characteristic ICP analysis line of zinc element is 206.200 nm; the characteristic ICP analysis line of phosphorus element is 178.284 nm. The optimized analysis conditions are shown in "Test Working Parameters" in Table 1. Analyze the standards at points 0 - 4 of the calibration curve in sequence to obtain the spectral intensities of nickel, silicon, manganese, chromium, copper, zinc, and phosphorus elements, and check the linear correlation of the calibration curve. The correlation coefficient r of nickel element satisfies > 0.9995, and the correlation coefficients r of silicon, manganese, chromium, copper, zinc, and phosphorus elements satisfy > 0.999.

[0093] Step S4: Sample Determination

[0094] Successively measure the blank solution and the sample solution to be measured, and directly read out the analysis results of nickel, silicon, manganese, chromium, copper, zinc, and phosphorus elements. The correlation table of the standard curve for the experiment is shown in Table 3:

[0095] Table 3 Standard Curve Correlation

[0096] Element analysis line Calibration curve correlation Element analysis line Calibration curve correlation Ni 231.604 nm r＝0.99989 Ni 341.476 nm r＝0.99992 Si 251.611 nm r＝0.99964 Mn 257.610 nm r＝0.99949 Cr 267.716 nm r＝0.99978 Cu 324.754 nm r＝0.99952 Zn 206.200 nm r＝0.99992 P 178.284 nm r＝0.99943

[0097] Precision Experiment

[0098] According to the method of Example 1, the nickel-containing diamond cutting wire samples were independently determined for recovery, and each was determined 6 times to obtain the SD and RSD. The results are shown in Table 4.

[0099] Table 4 Precision test data (%)

[0100]

[0101] As can be seen from Table 4, the precision of the detection method of the present invention meets the requirements for the expected precision of the analytes in the content range in "GB / T 32465-2015 Chemical Analysis Method Verification, Validation and Internal Quality Control" (when the target component content is 100%, the expected RSD < 1.3%; when the target component content is 10%, the expected RSD < 1.9%; when the target component content is 1%, the expected RSD < 2.7%; when the target component content is 0.1%, the expected RSD < 3.7%; when the target component content is 0.01%, the expected RSD < 5.3%); in addition, it should be noted that according to the requirements for the expected precision in GB / T 32465-2015 "Chemical Analysis Method Verification, Validation and Internal Quality Control Requirements", for the case where the target component content is 0.16%, the expected RSD should be less than 3.7%. Because 0.16% is between 0.1% and 1%, and the standard stipulates that when the target component content is 0.1%, the expected RSD < 3.7%, and when the target component content is 0.01%, the expected RSD < 5.3%.

[0102] Accuracy experiment

[0103] a) Nickel-iron GBW(E)010423 and steel standard samples with compositions and contents similar to those of the samples in Example 1 were selected, and metal nickel was added to simulate Samples 1#, 2#, and 3#. The contents of each element were determined by this method, and the results are shown in Tables 5 and 6.

[0104] Table 5 Test data for the determination of standard samples (%)

[0105]

[0106] Table 6 Reference values of steel standard samples (%)

[0107] Name Number Ni Si Mn Cr Cu P Low alloy steel GSBH40080-94 0.121 0.520 0.75 0.202 0.243 0.034 Low alloy steel GSBH40031-93 0.026 0.228 0.55 0.035 0.034 0.017 Low alloy steel GSB03-2454-2008 0.409 0.109 0.151 0.164 0.154 0.039

[0108] Note: 1. No Zn was determined in the nickel-iron and steel standard samples, so no test was conducted.

[0109] 2. The theoretical conversion value of sample No. 1# Ni in the test data of standard sample determination in Table 5 (%) is calculated as (0.121% × 0.1000 g + 99.99% × 0.0199 g) / 0.1000 g = 20.02%; the theoretical conversion value of sample No. 2# Ni is calculated as (0.026% × 0.1000 g + 99.99% × 0.0169 g) / 0.1000 g = 16.92%; the theoretical conversion value of sample No. 3# Ni is calculated as (0.409% × 0.1000 g + 99.99% × 0.0259 g) / 0.1000 g = 26.31%.

[0110] As can be seen from Table 5 and Table 6, the measured values of nickel, silicon, manganese, chromium, copper, and phosphorus are in agreement with the standard values (or theoretical conversion values), indicating that the detection method for the content of some elements in the metal cutting wire of the present invention has high accuracy. b) The standard addition recovery test was carried out, and the results are shown in Table 7.

[0111] Table 7 Results of the standard addition recovery test

[0112]

[0113] As can be seen from Table 7, the recovery rates of nickel, silicon, manganese, chromium, copper, zinc, and phosphorus elements in the present invention are 101.20%, 96.00%, 98.00%, 98.00%, 105.0%, 102.00%, and 96.00% respectively, further indicating that the detection method of the present invention has high accuracy.

[0114] It should be noted that this application is not limited to the above embodiments. The above embodiments are only examples, and embodiments with the same composition and the same function and effect as the technical idea within the technical solution scope of this application are all included in the technical scope of this application. In addition, within the scope of not departing from the main idea of this application, various modifications that can be thought of by those skilled in the art to the embodiments, and other ways constructed by combining some constituent elements in the embodiments are also included in the scope of this application.

Claims

1. A method for detecting the content of some elements in diamond cutting wire, characterized in that: The following steps are involved: Dissolving the sample in nitric acid solution and hydrochloric acid solution in turn to prepare a sample solution to be tested; After the sample solution to be tested is tested by inductively coupled plasma emission spectrometry, the contents of some elements in the sample solution to be tested are calculated based on the standard curve.

2. The method for detecting the content of some elements in diamond cutting wire according to claim 1, characterized in that: The mass concentration of the nitric acid solution is 30%-50%.

3. The method for detecting the content of some elements in diamond cutting wire according to claim 2, characterized in that: The mass of the nitric acid solution is 120-200 times the mass of the sample.

4. The method for detecting the content of some elements in diamond cutting wire according to claim 1, characterized in that: The nitric acid solution is heated to boiling state in advance and then added to the sample.

5. The method for detecting the content of some elements in diamond cutting wire according to claim 1, characterized in that: The mass concentration of the hydrochloric acid solution is 36%-38%.

6. The method for detecting the content of some elements in diamond cutting wire according to claim 1, characterized in that: The mass of the hydrochloric acid solution is 40-60 times the mass of the sample.

7. The method for detecting the content of some elements in diamond cutting wire according to claim 1, characterized in that: When using inductively coupled plasma emission spectrometry for testing, the characteristic ICP analysis lines of nickel, silicon, manganese, chromium, copper, zinc and phosphorus were selected and determined. The characteristic ICP analysis line of nickel is 231.604nm and 341.476nm, the characteristic ICP analysis line of silicon is 251.611nm; the characteristic ICP analysis line of manganese is 257.610nm; the characteristic ICP analysis line of chromium is 267.716nm; the characteristic ICP analysis line of copper is 324.754nm; the characteristic ICP analysis line of zinc is 206.200nm; and the characteristic ICP analysis line of phosphorus is 178.284nm.

8. The method for detecting the content of some elements in diamond cutting wire according to claim 1, characterized in that: The analysis pump speed for the experiments using inductively coupled plasma optical emission spectrometry was 45-55 / rpm, and the flushing pump speed was 90-110 / rpm.

9. The method for detecting the content of some elements in diamond cutting wire according to claim 1, characterized in that: In the experiment using inductively coupled plasma emission spectrometry, the auxiliary gas flow rate was 0.3-0.5 / L / min, and the nebulizer gas flow rate was 0.6-0.8 / L / min.

10. The method for detecting the content of some elements in diamond cutting wire according to claim 1, characterized in that: The size of the sample was less than 1 cm.

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