CN112284856A - Method for measuring contents of rare earth and trace elements in nickel-plated neodymium iron boron matrix by ICP-AES (inductively coupled plasma-atomic emission Spectrometry) - Google Patents

Method for measuring contents of rare earth and trace elements in nickel-plated neodymium iron boron matrix by ICP-AES (inductively coupled plasma-atomic emission Spectrometry) Download PDF

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CN112284856A
CN112284856A CN202011207238.3A CN202011207238A CN112284856A CN 112284856 A CN112284856 A CN 112284856A CN 202011207238 A CN202011207238 A CN 202011207238A CN 112284856 A CN112284856 A CN 112284856A
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rare earth
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刘晨
裴晓东
骆艳华
钱有军
佘世杰
张倩倩
鲍维东
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Sinosteel Nanjing New Material Research Institute Co Ltd
Sinosteel New Materials Co Ltd
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Abstract

The invention relates to the field of inspection and analysis methods, in particular to a method for measuring contents of rare earth and trace elements in a nickel-containing coating neodymium iron boron matrix by ICP-AES (inductively coupled plasma-atomic emission Spectrometry), which comprises the steps of preparing a deplating agent for surface treatment in advance; crushing the neodymium iron boron magnet containing the nickel plating layer; performing surface deplating treatment on the fragments; taking out the fragments of the neodymium iron boron matrix after deplating, cleaning and wiping the fragments to be used as a sample to be measured; accurately weighing a sample to be detected, dissolving the sample in nitric acid at low temperature, diluting the solution to a constant volume and continuously taking and diluting the solution to be detected to prepare a solution to be detected of trace elements and a solution to be detected of rare earth elements respectively; testing the intensity of the emitted light by using an inductively coupled plasma emission spectrometer, and calculating the percentage content of each element in the removed neodymium iron boron matrix by using a standard curve; the method completely avoids the interference of the nickel coating on the detection of each element in the matrix, and the obtained component content result is more accurate and closer to the actual formula of the neodymium iron boron matrix.

Description

Method for measuring contents of rare earth and trace elements in nickel-plated neodymium iron boron matrix by ICP-AES (inductively coupled plasma-atomic emission Spectrometry)
Technical Field
The invention relates to the technical field of chemical inspection and analysis methods for neodymium iron boron materials, in particular to a method for measuring contents of rare earth and trace elements in a nickel-containing coating neodymium iron boron matrix by ICP-AES.
Background
The neodymium iron boron magnetic material is called as the King magnet by virtue of excellent performance, and has been widely applied to high-tech fields such as electronics, machinery, traffic, national defense, medical treatment, aviation, aerospace and the like since the development of the 80 th century. Surface treatment techniques for neodymium iron boron materials have been widely used to resist surface oxidation and corrosion. In the conventional surface treatment mode at present, a nickel plating process becomes one of the mainstream processes due to excellent corrosion resistance and abrasion resistance, and the sintered neodymium iron boron magnet containing a nickel plating layer accounts for more than half of the market. For quality control and detection of neodymium iron boron material products, a method for rapidly and accurately measuring the constant and the trace elements is needed.
Compared with the widely-used analysis and detection method for the neodymium iron boron substrate before electroplating, the analysis of the components of the substrate material after nickel plating is difficult. With the increase of the recovery of inferior-quality products and waste products after nickel plating and the satisfaction of research and development requirements of neodymium iron boron materials, it is urgently needed to establish a component analysis method for rapidly and accurately determining an unknown component neodymium iron boron substrate after nickel plating.
Compared with an NdFeB base body which is not subjected to surface treatment, the difficulty in accurately measuring each element in the NdFeB base body containing the nickel coating is pre-treatment, firstly, the NdFeB base body containing the coating is treated by a common acid-soluble method, the coating cannot be completely dissolved, a small amount of NdFeB can be coated to form turbid liquid, and the accuracy of a detection result is influenced. Secondly, if the plating layer and the neodymium iron boron are not separated and are simultaneously dissolved and detected, the detection result of the content of each component of the neodymium iron boron substrate is low due to the existence of nickel-copper element, and the accurate neodymium iron boron formula cannot be obtained. At present, no test method and standard for the rare earth and the trace elements of the nickel-containing coating neodymium iron boron matrix exist.
In conclusion, the detection of rare earth and trace elements in the nickel-containing plated neodymium-iron-boron substrate is a difficult problem.
Disclosure of Invention
The method aims to solve the problems that the nickel-containing coating neodymium iron boron surface coating is difficult to dissolve and is difficult to separate from the matrix elements after dissolving, so that the accuracy of the detection result of rare earth and trace elements in the matrix is influenced, and the like. The invention adopts a step-by-step pretreatment mode, firstly, the nickel-containing coating is completely stripped by the prepared stripping solution, the corrosive agent and the complexing agent in the stripping solution can quickly and uniformly dissolve the coating, meanwhile, the internal matrix is basically not corroded, and the used reagent is simple and environment-friendly. And (3) performing two-step treatment on the treated neodymium iron boron substrate serving as a sample to be detected to prepare a solution to be detected, wherein the content of the detected rare earth and trace elements is closer to the formula of the neodymium iron boron substrate. The detection method completely avoids the interference of the coating on the detection of each element in the matrix, and simultaneously has simple and rapid treatment process and high result accuracy.
More specifically, the invention discloses a method for measuring contents of rare earth and trace elements in a nickel-plated neodymium iron boron matrix by ICP-AES, which is characterized by comprising the following steps:
(1) preparing a deplating solution for surface coating treatment in advance, quantitatively weighing a corrosive agent and a complexing agent, adding the corrosive agent and the complexing agent into deionized water, stirring, and fixing the volume for later use after complete dissolution;
(2) crushing the nickel-containing plated neodymium iron boron magnet with unknown matrix component content to obtain neodymium iron boron fragments with equivalent diameter less than or equal to 0.5 cm;
(3) weighing 5g of fragments containing the plating layer, soaking the fragments in a deplating solution preheated to 60-80 ℃, uniformly and quickly removing the plating layer on the surface of the magnet, and treating the plating layer on the surface of the fragments until the fragments are invisible to naked eyes after deplating is finished;
(4) taking out fragments of the neodymium iron boron matrix subjected to deplating, ultrasonically cleaning the fragments in distilled water to remove residual deplating agent, and quickly wiping the fragments with filter paper to be used as a sample to be detected; accurately weighing 2.5g (accurate to 0.0001g) of sample to be detected, heating the sample to be detected by using 20mL of analytically pure nitric acid at low temperature until the sample is completely dissolved, fixing the volume to a 100mL volumetric flask, continuously taking and diluting the solution by 20 times, and taking the solution as the solution to be detected of the trace elements; taking the solution diluted by 400 times as a to-be-detected solution of the rare earth element; simultaneously, performing a blank test;
(5) respectively preparing a mixed standard series solution of rare earth elements and a mixed standard series solution of trace elements: the rare earth elements comprise Nd, Pr, Dy, Ho, Gd, Tb and Ce, and the trace elements comprise Co, Al, Cu, Ga, Zr, Nb and B; respectively taking rare earth element mixed standard solutions with different volumes, and respectively adding the rare earth element mixed standard solutions into four 100mL volumetric flasks to prepare rare earth element mixed standard series solutions with different concentrations; then, mixing trace element mixed standard solutions with different volumes, and adding the mixed standard solutions into four 100mL volumetric flasks respectively to prepare trace mixed standard series solutions with different concentrations; wherein, iron matrix solution, neodymium matrix solution and praseodymium matrix solution with equivalent concentration are added into the mixed standard series solution of the trace elements;
(6) testing the emission light intensity of the mixed standard series solution of the rare earth elements and the mixed standard series solution of the trace elements by using an inductively coupled plasma emission spectrometer, and constructing a standard curve by taking the concentration of each element as an X axis and the analysis linear intensity as a Y axis;
(7) and (5) testing the emission light intensity of the liquid to be tested obtained in the step (4) by using an inductively coupled plasma emission spectrometer, and calculating the percentage content of each element in the removed neodymium iron boron substrate by using the standard curve in the step (6).
Preferably, the deplating agent in the step (1) comprises the following components in percentage by weight: the corrosive agent is sodium hydroxide or potassium hydroxide, and the content of the corrosive agent is 30-80 g/L, preferably 40-70 g/L; the complexing agent is disodium ethylene diamine tetraacetate, tetrasodium ethylene diamine tetraacetate, sodium ethylene diamine tetra-methylene phosphate or sodium citrate, and the content of the disodium ethylene diamine tetraacetate and the tetrasodium ethylene diamine tetraacetate is 5-20 g/L, preferably 5-10 g/L; the content of the ethylene diamine tetramethylene sodium phosphate is 10-30 g/L, preferably 10-20 g/L; the sodium citrate is 3-15 g/L, preferably 5-10 g/L.
Preferably, the volume-to-weight ratio of the deplating agent to the neodymium iron boron magnet containing the plating layer in the step (3) is 100 mL: 5g of the total weight.
Preferably, 5g of fragments containing the plating layer weighed in the step (3) are soaked in a deplating solution preheated to 60-80 ℃, the plating layer on the surface of the magnet is uniformly and quickly deplated, deplating can be completed within 10-15 min, and the plating layer on the surface of the fragments is processed until the fragments are invisible to naked eyes.
Preferably, in the step (4), the fragments of the neodymium iron boron matrix after deplating are taken out and cleaned in distilled water by ultrasonic cleaning for 1-2min, so that residual deplating agent can be removed, and the fragments are quickly wiped and dried by filter paper to be used as a sample to be detected.
Preferably, the concentrations of the mixed standard series solution of the rare earth elements in the step (5) are respectively as follows: : 1. mu.g/mL, 5. mu.g/mL, 10. mu.g/mL, 20. mu.g/mL; the concentrations of the mixed standard series solutions of the trace elements are respectively 1 mug/mL, 5 mug/mL, 10 mug/mL and 20 mug/mL, wherein the concentration of an iron matrix is 800 mug/mL, the concentration of a neodymium matrix is 350 mug/mL, and the concentration of a praseodymium matrix is 80 mug/mL.
Preferably, the inductively coupled plasma emission spectrometer test conditions of step (6) and step (7):
Figure BDA0002757424400000031
preferably, the content of the rare earth elements including Nd, Pr, Dy, Ho, Gd, Tb, and Ce in the neodymium iron boron matrix in step (7) is w mass fractionreIn% by weight, the value is calculated according to formula (1):
Figure BDA0002757424400000032
in formula (1):
v is the volume of the solution of the rare earth element to be detected, and the unit is milliliter (mL);
c is the concentration of the analysis element of the rare earth element solution to be detected, and the unit is microgram per milliliter (mu g/mL);
C0-the blank solution is analyzed for the concentration of the element in micrograms per milliliter (μ g/mL);
m is the mass of the sample to be measured in grams (g);
400-rare earth element dilution factor.
Preferably, the microelements in the neodymium iron boron matrix in the step (7) comprise the contents of Co, Al, Cu, Ga, Zr, Nb and B
In terms of mass fraction wteIn% by weight, the value is calculated according to equation (2):
Figure BDA0002757424400000041
in formula (2):
v is the volume of the solution of the microelement to be detected, and the unit is milliliter (mL);
c' -concentration of trace element to be detected analysis element in microgram per milliliter (mug/mL);
C′0-the blank solution is analyzed for the concentration of the element in micrograms per milliliter (μ g/mL);
m is the mass of the sample to be measured in grams (g);
20-trace element dilution factor.
The invention firstly proposes a mode of carrying out step-by-step pretreatment on the neodymium iron boron substrate containing the nickel coating for sample dissolution, completely avoids the interference of the nickel coating on the detection of each element in the substrate, obtains more accurate component content results, and is closer to the actual formula of the neodymium iron boron substrate.
In addition, compared with the prior art, the invention has the beneficial effects that:
(1) the common alkali and the complexing agent are utilized for deplating, the dissolution is rapid and uniform, and the agent is simple and environment-friendly; the interference of the plating layer on the detection of the rare earth and the trace elements in the matrix is eliminated;
(2) after stripping the coating, taking the matrix as a sample to be detected for weighing, dissolving and detecting; the obtained component content result is more accurate, is closer to the actual formula of the neodymium iron boron matrix, and has greater guiding significance;
(3) the method has the advantages of multiple detection elements, wide linear range and simple and quick operation;
(4) the detection precision is good and the accuracy is high.
Detailed Description
The present invention will be further described with reference to the following examples. The described embodiments and their results are only intended to illustrate the invention and should not be taken as limiting the invention described in detail in the claims.
Example 1
(1) Preparing a deplating solution for surface coating treatment in advance, quantitatively weighing a corrosive agent and a complexing agent, adding the corrosive agent and the complexing agent into deionized water, stirring, and fixing the volume for later use after complete dissolution; wherein the corrosive agent is sodium hydroxide with the concentration of 30 g/L; the complexing agent is disodium ethylene diamine tetraacetate, and the concentration is 5 g/L;
(2) crushing the nickel-containing plating neodymium iron boron magnet with unknown matrix component content to obtain neodymium iron boron fragments with the equivalent diameter less than 0.5 cm;
(3) weighing about 5g of fragments containing the plating layer, soaking the fragments in 100mL of deplating solution, preheating to 80 ℃, uniformly and quickly deplating the plating layer on the surface of the magnet, and treating the plating layer on the surfaces of the fragments until the fragments are invisible to naked eyes after deplating for about 15 min;
(4) and taking out the fragments subjected to deplating, ultrasonically cleaning the fragments in distilled water for about 1min to remove residual deplating agent, and quickly wiping the fragments by using filter paper to serve as a sample to be detected. 2.5123g of sample to be detected is accurately weighed, 20mL of analytically pure nitric acid is used for completely dissolving the sample to be detected, the volume is determined to be 100mL, the solution diluted by 20 times is continuously divided and diluted to be used as the solution to be detected of the trace elements; taking the solution diluted by 400 times as a to-be-detected solution of the rare earth element; simultaneously, performing a blank test;
(5) respectively preparing a mixed standard series solution of rare earth elements and a mixed standard series solution of trace elements: the rare earth elements comprise Nd, Pr, Dy, Ho, Gd, Tb and Ce, and the trace elements comprise Co, Al, Cu, Ga, Zr, Nb and B. Respectively taking rare earth element mixed standard solutions with different volumes, respectively adding the rare earth element mixed standard solutions into four 100mL volumetric flasks to prepare rare earth element mixed standard series solutions with different concentrations, wherein the concentrations of the rare earth element mixed standard series solutions are respectively as follows: 1. mu.g/mL, 5. mu.g/mL, 10. mu.g/mL, 20. mu.g/mL. And then, taking the mixed trace element standard solutions with different volumes, and respectively adding the mixed trace element standard solutions into four 100mL volumetric flasks to prepare the mixed trace element standard solutions with different concentrations. The concentrations are respectively 1 mug/mL, 5 mug/mL, 10 mug/mL and 20 mug/mL, and an iron matrix solution, a neodymium matrix solution and a praseodymium matrix solution with equivalent concentrations are added, and the concentrations are respectively 800 mug/mL, 350 mug/mL and 80 mug/mL;
(6) testing the emission light intensity of the mixed standard series solution of the rare earth elements and the mixed standard series solution of the trace elements by using an inductively coupled plasma emission spectrometer, and constructing a standard curve by taking the concentration of each element as an X axis and the analysis linear intensity as a Y axis;
(7) testing the emission light intensity of the liquid to be tested obtained in the step (4) by using an inductively coupled plasma emission spectrometer, and calculating the percentage content of each element in the deplated neodymium iron boron substrate by using the standard curve in the step (4);
(8) (6) and (7) the inductively coupled plasma emission spectrometer test conditions:
Figure BDA0002757424400000051
Figure BDA0002757424400000061
(9) the rare earth elements in the sample to be detected comprise Nd, Pr, Dy, Ho, Gd, Tb and Ce according to the mass fraction wreIn% by weight, the value is calculated according to formula (1):
Figure BDA0002757424400000062
in formula (1):
v is the volume of the solution of the rare earth element to be detected, and the unit is milliliter (mL);
c is the concentration of the analysis element of the rare earth element solution to be detected, and the unit is microgram per milliliter (mu g/mL);
C0-the concentration of the elements of the blank solution is analyzed in units ofMicrograms per milliliter (μ g/mL);
m is the mass of the sample to be measured in grams (g);
400-rare earth element dilution factor;
(10) the trace elements in the sample to be detected comprise Co, Al, Cu, Ga, Zr, Nb and B according to the mass fraction wteIn% by weight, the value is calculated according to equation (2):
Figure BDA0002757424400000063
in formula (2):
v is the volume of the solution of the trace element to be detected, and the unit is milliliter (mL);
c' -concentration of trace element in microgram per milliliter (mug/mL) of analytical element in the solution to be detected;
C′0-the blank solution is analyzed for the concentration of the element in micrograms per milliliter (μ g/mL);
m is the mass of the sample to be measured in grams (g);
20-trace element dilution times;
the contents of rare earth and trace elements in the sample to be tested of the neodymium iron boron matrix are shown in the following table:
table 1 content of rare earth and trace elements in the neodymium iron boron matrix:
Figure BDA0002757424400000064
(11) method detection limit of elements
The blank solution was measured 10 times using the established standard curve, and the standard deviation of the measurement results was 3 times as the detection limit of the method, and the results are shown in table 2.
Table 2 method detection limits:
Figure BDA0002757424400000071
(12) the method comprises the following steps:
prior to the determination of the sample results, a test of method precision was performed. The sample solution is repeatedly measured for 10 times according to the method, the precision of the method is verified, and the experimental result is shown in table 3; as can be seen from the results in Table 2, the RSD was within 3.0%, indicating that the precision of the method was high.
Table 3 method precision test data:
Figure BDA0002757424400000072
(13) and (3) standard addition recovery test:
the same sample is taken to carry out a standard addition recovery test according to the method, the test result is shown in table 4, the recovery rate is 98.2-101.8%, and the method is accurate and reliable.
Table 4 sample spiking recovery test:
Figure BDA0002757424400000073
example 2
(1) Preparing a deplating solution for surface coating treatment in advance, quantitatively weighing a corrosive agent and a complexing agent, adding the corrosive agent and the complexing agent into deionized water, stirring, and after complete dissolution, fixing the volume for later use; wherein the corrosive agent is sodium hydroxide with the concentration of 50 g/L; the complexing agent is tetrasodium ethylene diamine tetraacetate, and the concentration is 10 g/L;
(2) crushing the neodymium iron boron magnet with the same matrix component content as that in the embodiment 1 and the unknown nickel-containing coating, so as to obtain neodymium iron boron fragments with the equivalent diameter of less than 0.5 cm;
(3) weighing about 5g of fragments containing the plating layer, soaking the fragments in 100mL of deplating solution, preheating to 60 ℃, uniformly and quickly deplating the plating layer on the surface of the magnet, and treating the plating layer on the surfaces of the fragments until the fragments are invisible to naked eyes after deplating is finished for about 15 min;
(4) and taking out the fragments subjected to deplating, ultrasonically cleaning the fragments in distilled water for about 1min to remove residual deplating agent, and quickly wiping the fragments by using filter paper to serve as a sample to be detected. 2.5645g of sample to be detected is accurately weighed, 20mL of analytically pure nitric acid is used for completely dissolving the sample to be detected, the volume is determined to be 100mL, the solution diluted by 20 times is continuously divided and diluted to be used as the solution to be detected of the trace elements; and taking the solution diluted by 400 times as the solution to be detected of the rare earth element. Simultaneously, performing a blank test;
(5) respectively preparing a mixed standard series solution of rare earth elements and a mixed standard series solution of trace elements: the rare earth elements comprise Nd, Pr, Dy, Ho, Gd, Tb and Ce, and the trace elements comprise Co, Al, Cu, Ga, Zr, Nb and B; respectively taking rare earth element mixed standard solutions with different volumes, respectively adding the rare earth element mixed standard solutions into four 100mL volumetric flasks to prepare rare earth element mixed standard series solutions with different concentrations, wherein the concentrations of the rare earth element mixed standard series solutions are respectively as follows: 1. mu.g/mL, 5. mu.g/mL, 10. mu.g/mL, 20. mu.g/mL; and then, taking the mixed trace element standard solutions with different volumes, and respectively adding the mixed trace element standard solutions into four 100mL volumetric flasks to prepare the mixed trace element standard solutions with different concentrations. The concentrations are 1 mug/mL, 5 mug/mL, 10 mug/mL and 20 mug/mL respectively, and the iron matrix solution, the neodymium matrix solution and the praseodymium matrix solution with equivalent concentrations are added, and the concentrations are 800 mug/mL, 350 mug/mL and 80 mug/mL respectively.
(6) Testing the emission light intensity of the mixed standard series solution of the rare earth elements and the mixed standard series solution of the trace elements by using an inductively coupled plasma emission spectrometer, and constructing a standard curve by taking the concentration of each element as an X axis and the analysis linear intensity as a Y axis;
(7) testing the emission light intensity of the liquid to be tested obtained in the step (4) by using an inductively coupled plasma emission spectrometer, and calculating the percentage content of each element in the deplated neodymium iron boron substrate by using the standard curve in the step (4);
(8) (6) and (7) the inductively coupled plasma emission spectrometer test conditions:
parameter(s) Set value Parameter(s) Set value
High frequency transmitter power (W) 1300 Plasma gas flow (L/min) 12
Auxiliary gas flow (L/min) 0.4 Atomizer gas flow (L/min) 0.7
Observation mode Vertical observation Analysis Pump speed (mL/min) 1.5
Characteristic analysis line (nm) of Nd 406.109 Characteristic analysis line (nm) of Pr 390.844
Characteristic analysis line (nm) of Dy 353.175 Characteristic analysis spectral line (nm) of Ho 345.600
Characteristic analysis line (nm) of Gd 376.844 Characteristic analysis line (nm) of Tb 350.917
Characteristic analysis line (nm) of Co 413.764 Characteristic analysis line (nm) of Al 273.313
Characteristic analysis line (nm) of Cu 324.755 Characteristic analysis line (nm) of Ga 294.364
Characteristic analysis line (nm) of Zr 343.823 Characteristic analytical line (nm) of Nb 316.340
Characteristic analysis line (nm) of B 208.889
(9) The rare earth elements in the sample to be detected comprise Nd, Pr, Dy, Ho, Gd, Tb and Ce according to the mass fraction wreIn% by weight, the value is calculated according to formula (1):
Figure BDA0002757424400000091
in formula (1):
v is the volume of the solution of the rare earth element to be detected, and the unit is milliliter (mL);
c is the concentration of the analysis element of the rare earth element solution to be detected, and the unit is microgram per milliliter (mu g/mL);
C0-the blank solution is analyzed for the concentration of the element in micrograms per milliliter (μ g/mL);
m is the mass of the sample to be measured in grams (g);
400-rare earth element dilution factor;
(10) the trace elements in the sample to be detected comprise Co, Al, Cu, Ga, Zr, Nb and B according to the mass fraction wteIn% by weight, the value is calculated according to equation (2):
Figure BDA0002757424400000092
in formula (2):
v is the volume of the solution of the trace element to be detected, and the unit is milliliter (mL);
c' -concentration of trace element in microgram per milliliter (mug/mL) of analytical element in the solution to be detected;
C′0-the blank solution is analyzed for the concentration of the element in micrograms per milliliter (μ g/mL);
m is the mass of the sample to be measured in grams (g);
20-trace element dilution times;
the contents of rare earth and trace elements in the sample to be tested of the neodymium iron boron matrix are shown in the following table:
table 5 content of rare earth and trace elements in the neodymium iron boron matrix:
Figure BDA0002757424400000093
the same unknown sample is used for detection, and compared with the result of the embodiment 1, the difference value is small, the detection result is accurate, and the reproducibility is good.
Example 3
(1) Preparing a deplating solution for surface coating treatment in advance, quantitatively weighing a corrosive agent and a complexing agent, adding the corrosive agent and the complexing agent into deionized water, stirring, and after complete dissolution, fixing the volume for later use; wherein the corrosive agent is sodium hydroxide with the concentration of 70 g/L; the complexing agent is ethylene diamine tetra methylene sodium phosphate with the concentration of 20 g/L;
(2) crushing the neodymium iron boron magnet with the same matrix component content as that in the embodiment 1 and the unknown nickel-containing coating, so as to obtain neodymium iron boron fragments with the equivalent diameter of less than 0.5 cm;
(3) weighing about 5g of fragments containing the plating layer, soaking the fragments in 100mL of deplating solution, preheating to 60 ℃, uniformly and quickly deplating the plating layer on the surface of the magnet, and treating the plating layer on the surfaces of the fragments until the fragments are invisible to naked eyes after deplating is finished for about 15 min;
(4) taking out the fragments subjected to deplating, ultrasonically cleaning the fragments in distilled water for about 1min to remove residual deplating agent, and quickly wiping the fragments by using filter paper to serve as a sample to be detected; 2.5057g of sample to be detected is accurately weighed, 20mL of analytically pure nitric acid is used for completely dissolving the sample to be detected, the volume is determined to be 100mL, the solution diluted by 20 times is continuously divided and diluted to be used as the solution to be detected of the trace elements; taking the solution diluted by 400 times as a to-be-detected solution of the rare earth element; simultaneously, performing a blank test;
(5) respectively preparing a mixed standard series solution of rare earth elements and a mixed standard series solution of trace elements: the rare earth elements comprise Nd, Pr, Dy, Ho, Gd, Tb and Ce, and the trace elements comprise Co, Al, Cu, Ga, Zr, Nb and B. Respectively taking rare earth element mixed standard solutions with different volumes, respectively adding the rare earth element mixed standard solutions into four 100mL volumetric flasks to prepare rare earth element mixed standard series solutions with different concentrations, wherein the concentrations of the rare earth element mixed standard series solutions are respectively as follows: 1. mu.g/mL, 5. mu.g/mL, 10. mu.g/mL, 20. mu.g/mL. And then, taking the mixed trace element standard solutions with different volumes, and respectively adding the mixed trace element standard solutions into four 100mL volumetric flasks to prepare the mixed trace element standard solutions with different concentrations. The concentrations are respectively 1 mug/mL, 5 mug/mL, 10 mug/mL and 20 mug/mL, and an iron matrix solution, a neodymium matrix solution and a praseodymium matrix solution with equivalent concentrations are added, and the concentrations are respectively 800 mug/mL, 350 mug/mL and 80 mug/mL;
(6) testing the emission light intensity of the mixed standard series solution of the rare earth elements and the mixed standard series solution of the trace elements by using an inductively coupled plasma emission spectrometer, and constructing a standard curve by taking the concentration of each element as an X axis and the analysis linear intensity as a Y axis;
(7) testing the emission light intensity of the liquid to be tested obtained in the step (4) by using an inductively coupled plasma emission spectrometer, and calculating the percentage content of each element in the deplated neodymium iron boron substrate by using the standard curve in the step (4);
(8) (6) and (7) the inductively coupled plasma emission spectrometer test conditions:
Figure BDA0002757424400000101
Figure BDA0002757424400000111
(9) the rare earth elements in the sample to be detected comprise Nd, Pr, Dy, Ho, Gd, Tb and Ce according to the mass fraction wreIn% by weight, the value is calculated according to formula (1):
Figure BDA0002757424400000112
in formula (1):
v is the volume of the solution of the rare earth element to be detected, and the unit is milliliter (mL);
c is the concentration of the analysis element of the rare earth element solution to be detected, and the unit is microgram per milliliter (mu g/mL);
C0-the blank solution is analyzed for the concentration of the element in micrograms per milliliter (μ g/mL);
m is the mass of the sample to be measured in grams (g);
400-rare earth element dilution factor;
(10) the trace elements in the sample to be detected comprise Co, Al, Cu, Ga, Zr, Nb and B according to the mass fraction wteIn% by weight, the value is calculated according to equation (2):
Figure BDA0002757424400000113
in formula (2):
v is the volume of the solution of the trace element to be detected, and the unit is milliliter (mL);
c' -concentration of trace element in microgram per milliliter (mug/mL) of analytical element in the solution to be detected;
C′0-the blank solution is analyzed for the concentration of the element in micrograms per milliliter (μ g/mL);
m is the mass of the sample to be measured in grams (g);
20-trace element dilution times;
the contents of rare earth and trace elements in the sample to be tested of the neodymium iron boron matrix are shown in the following table:
table 6 contents of rare earth and trace elements in the neodymium iron boron matrix:
Figure BDA0002757424400000114
Figure BDA0002757424400000121
the same unknown sample is used for detection, and compared with the result of the embodiment 1, the difference value is small, the detection result is accurate, and the reproducibility is good.
Example 4
(1) Preparing a deplating solution for surface coating treatment in advance, quantitatively weighing a corrosive agent and a complexing agent, adding the corrosive agent and the complexing agent into deionized water, stirring, and after complete dissolution, fixing the volume for later use; wherein the corrosive agent is sodium hydroxide with the concentration of 80 g/L; the complexing agent is sodium citrate with the concentration of 10 g/L;
(2) crushing the neodymium iron boron magnet with the same matrix component content as that in the embodiment 1 and the unknown nickel-containing coating, so as to obtain neodymium iron boron fragments with the equivalent diameter of less than 0.5 cm;
(3) weighing about 5g of fragments containing the plating layer, soaking the fragments in 100mL of deplating solution, preheating to 60 ℃, uniformly and quickly deplating the plating layer on the surface of the magnet, and treating the plating layer on the surfaces of the fragments until the fragments are invisible to naked eyes after deplating is finished for about 15 min;
(4) taking out the fragments subjected to deplating, ultrasonically cleaning the fragments in distilled water for about 1min to remove residual deplating agent, and quickly wiping the fragments by using filter paper to serve as a sample to be detected; 2.5057g of sample to be detected is accurately weighed, 20mL of analytically pure nitric acid is used for completely dissolving the sample to be detected, the volume is determined to be 100mL, the solution diluted by 20 times is continuously divided and diluted to be used as the solution to be detected of the trace elements; taking the solution diluted by 400 times as a to-be-detected solution of the rare earth element; simultaneously, performing a blank test;
(5) respectively preparing a mixed standard series solution of rare earth elements and a mixed standard series solution of trace elements: the rare earth elements comprise Nd, Pr, Dy, Ho, Gd, Tb and Ce, and the trace elements comprise Co, Al, Cu, Ga, Zr, Nb and B. Respectively taking rare earth element mixed standard solutions with different volumes, respectively adding the rare earth element mixed standard solutions into four 100mL volumetric flasks to prepare rare earth element mixed standard series solutions with different concentrations, wherein the concentrations of the rare earth element mixed standard series solutions are respectively as follows: 1. mu.g/mL, 5. mu.g/mL, 10. mu.g/mL, 20. mu.g/mL. And then, taking the mixed trace element standard solutions with different volumes, and respectively adding the mixed trace element standard solutions into four 100mL volumetric flasks to prepare the mixed trace element standard solutions with different concentrations. The concentrations are respectively 1 mug/mL, 5 mug/mL, 10 mug/mL and 20 mug/mL, and an iron matrix solution, a neodymium matrix solution and a praseodymium matrix solution with equivalent concentrations are added, and the concentrations are respectively 800 mug/mL, 350 mug/mL and 80 mug/mL;
(6) testing the emission light intensity of the mixed standard series solution of the rare earth elements and the mixed standard series solution of the trace elements by using an inductively coupled plasma emission spectrometer, and constructing a standard curve by taking the concentration of each element as an X axis and the analysis linear intensity as a Y axis;
(7) testing the emission light intensity of the liquid to be tested obtained in the step (4) by using an inductively coupled plasma emission spectrometer, and calculating the percentage content of each element in the deplated neodymium iron boron substrate by using the standard curve in the step (4);
(8) (6) and (7) the inductively coupled plasma emission spectrometer test conditions:
parameter(s) Set value Parameter(s) Set value
High frequency transmitter power (w) 1300 Plasma gas flow (L/min) 12
Auxiliary gas flow (L/min) 0.4 Atomizer gas flow (L/min) 0.7
Observation mode Vertical observation Analysis Pump speed (mL/min) 1.5
Characteristic analysis line (nm) of Nd 406.109 Characteristic analysis line (nm) of Pr 390.844
Characteristic analysis line (nm) of Dy 353.175 Characteristic analysis spectral line (nm) of Ho 345.600
Characteristic analysis line (nm) of Gd 376.844 Characteristic analysis spectral line of Tb(nm) 350.917
Characteristic analysis line (nm) of Co 413.764 Characteristic analysis line (nm) of Al 273.313
Characteristic analysis line (nm) of Cu 324.755 Characteristic analysis line (nm) of Ga 294.364
Characteristic analysis line (nm) of Zr 343.823 Characteristic analytical line (nm) of Nb 316.340
Characteristic analysis line (nm) of B 208.889
(9) The rare earth elements in the sample to be detected comprise Nd, Pr, Dy, Ho, Gd, Tb and Ce according to the mass fraction wreIn% by weight, the value is calculated according to formula (1):
Figure BDA0002757424400000131
in formula (1):
v is the volume of the solution of the rare earth element to be detected, and the unit is milliliter (mL);
c is the concentration of the analysis element of the rare earth element solution to be detected, and the unit is microgram per milliliter (mu g/mL);
C0-the blank solution is analyzed for the concentration of the element in micrograms per milliliter (μ g/mL);
m is the mass of the sample to be measured in grams (g);
400-rare earth element dilution factor;
(10) the trace elements in the sample to be detected comprise Co, Al, Cu, Ga, Zr, Nb and B according to the mass fraction wteIn% by weight, the value is calculated according to equation (2):
Figure BDA0002757424400000132
in formula (2):
v is the volume of the solution of the trace element to be detected, and the unit is milliliter (mL);
c' -concentration of trace element in microgram per milliliter (mug/mL) of analytical element in the solution to be detected;
C′0-the blank solution is analyzed for the concentration of the element in micrograms per milliliter (μ g/mL);
m is the mass of the sample to be measured in grams (g);
20-trace element dilution times;
the contents of rare earth and trace elements in the sample to be tested of the neodymium iron boron matrix are shown in the following table:
table 7 contents of rare earth and trace elements in the neodymium iron boron matrix:
Figure BDA0002757424400000141
the same unknown sample is used for detection, and compared with the result of the embodiment 1, the difference value is small, the detection result is accurate, and the reproducibility is good.
Example 5
(1) Preparing a deplating solution for surface coating treatment in advance, quantitatively weighing a corrosive agent and a complexing agent, adding the corrosive agent and the complexing agent into deionized water, stirring, and after complete dissolution, fixing the volume for later use; wherein the corrosive agent is potassium hydroxide with the concentration of 40 g/L; the complexing agent is disodium ethylene diamine tetraacetate, and the concentration is 15 g/L;
(2) crushing the neodymium iron boron magnet with the same matrix component content as that in the embodiment 1 and the unknown nickel-containing coating, so as to obtain neodymium iron boron fragments with the equivalent diameter of less than 0.5 cm;
(3) weighing about 5g of fragments containing the plating layer, soaking the fragments in 100mL of deplating solution, preheating to 60 ℃, uniformly and quickly deplating the plating layer on the surface of the magnet, and treating the plating layer on the surfaces of the fragments until the fragments are invisible to naked eyes after deplating is finished for about 15 min;
(4) taking out the fragments subjected to deplating, ultrasonically cleaning the fragments in distilled water for about 1min to remove residual deplating agent, and quickly wiping the fragments by using filter paper to serve as a sample to be detected; 2.5057g of sample to be detected is accurately weighed, 20mL of analytically pure nitric acid is used for completely dissolving the sample to be detected, the volume is determined to be 100mL, the solution diluted by 20 times is continuously divided and diluted to be used as the solution to be detected of the trace elements; taking the solution diluted by 400 times as a to-be-detected solution of the rare earth element; simultaneously, performing a blank test;
(5) respectively preparing a mixed standard series solution of rare earth elements and a mixed standard series solution of trace elements: the rare earth elements comprise Nd, Pr, Dy, Ho, Gd, Tb and Ce, and the trace elements comprise Co, Al, Cu, Ga, Zr, Nb and B. Respectively taking rare earth element mixed standard solutions with different volumes, respectively adding the rare earth element mixed standard solutions into four 100mL volumetric flasks to prepare rare earth element mixed standard series solutions with different concentrations, wherein the concentrations of the rare earth element mixed standard series solutions are respectively as follows: 1. mu.g/mL, 5. mu.g/mL, 10. mu.g/mL, 20. mu.g/mL. And then, taking the mixed trace element standard solutions with different volumes, and respectively adding the mixed trace element standard solutions into four 100mL volumetric flasks to prepare the mixed trace element standard solutions with different concentrations. The concentrations are respectively 1 mug/mL, 5 mug/mL, 10 mug/mL and 20 mug/mL, and an iron matrix solution, a neodymium matrix solution and a praseodymium matrix solution with equivalent concentrations are added, and the concentrations are respectively 800 mug/mL, 350 mug/mL and 80 mug/mL;
(6) testing the emission light intensity of the mixed standard series solution of the rare earth elements and the mixed standard series solution of the trace elements by using an inductively coupled plasma emission spectrometer, and constructing a standard curve by taking the concentration of each element as an X axis and the analysis linear intensity as a Y axis;
(7) testing the emission light intensity of the liquid to be tested obtained in the step (4) by using an inductively coupled plasma emission spectrometer, and calculating the percentage content of each element in the deplated neodymium iron boron substrate by using the standard curve in the step (4);
(8) (6) and (7) the inductively coupled plasma emission spectrometer test conditions:
parameter(s) Set value Parameter(s) Set value
High frequency transmitter power (W) 1300 Plasma gas flow (L/min) 12
Auxiliary gas flow (L/min) 0.4 Atomizer gas flow (L/min) 0.7
Observation mode Vertical observation Analysis Pump speed (mL/min) 1.5
Characteristic analysis line (nm) of Nd 406.109 Characteristic analysis line (nm) of Pr 390.844
Characteristic analysis line (nm) of Dy 353.175 Characteristic analysis spectral line (nm) of Ho 345.600
Characteristic analysis line (nm) of Gd 376.844 Characteristic analysis line (nm) of Tb 350.917
Characteristic analysis line (nm) of Co 413.764 Characteristic analysis line (nm) of Al 273.313
Characteristic analysis line (nm) of Cu 324.755 Characteristic analysis line (nm) of Ga 294.364
Characteristic analysis line (nm) of Zr 343.823 Characteristic analytical line (nm) of Nb 316.340
Characteristic analysis line (nm) of B 208.889
(9) The rare earth elements in the sample to be detected comprise Nd, Pr, Dy, Ho, Gd, Tb and Ce according to the mass fraction wreIn% by weight, the value is calculated according to formula (1):
Figure BDA0002757424400000151
in formula (1):
v is the volume of the solution of the rare earth element to be detected, and the unit is milliliter (mL);
c is the concentration of the analysis element of the rare earth element solution to be detected, and the unit is microgram per milliliter (mu g/mL);
C0-the blank solution is analyzed for the concentration of the element in micrograms per milliliter (μ g/mL);
m is the mass of the sample to be measured in grams (g);
400-rare earth element dilution factor;
(10) the trace elements in the sample to be detected comprise Co, Al, Cu, Ga, Zr, Nb and B according to the mass fraction wteIn% by weight, the value is calculated according to equation (2):
Figure BDA0002757424400000152
in formula (2):
v is the volume of the solution of the trace element to be detected, and the unit is milliliter (mL);
c' -concentration of trace element in microgram per milliliter (mug/mL) of analytical element in the solution to be detected;
C′0-the blank solution is analyzed for the concentration of the element in micrograms per milliliter (μ g/mL);
m is the mass of the sample to be measured in grams (g);
20-trace element dilution times;
the contents of rare earth and trace elements in the sample to be tested of the neodymium iron boron matrix are shown in the following table:
table 8 contents of rare earth and trace elements in the neodymium iron boron matrix:
Figure BDA0002757424400000161
the same unknown sample is used for detection, and compared with the result of the embodiment 1, the difference value is small, the detection result is accurate, and the reproducibility is good.
Example 6
(1) Preparing a deplating solution for surface coating treatment in advance, quantitatively weighing a corrosive agent and a complexing agent, adding the corrosive agent and the complexing agent into deionized water, stirring, and after complete dissolution, fixing the volume for later use; wherein the corrosive agent is potassium hydroxide with the concentration of 80 g/L; the complexing agent is ethylene diamine tetra methylene sodium phosphate with the concentration of 20 g/L;
(2) crushing the neodymium iron boron magnet with the same matrix component content as that in the embodiment 1 and the unknown nickel-containing coating, so as to obtain neodymium iron boron fragments with the equivalent diameter of less than 0.5 cm;
(3) weighing about 5g of fragments containing the plating layer, soaking the fragments in 100mL of deplating solution, preheating to 60 ℃, uniformly and quickly deplating the plating layer on the surface of the magnet, and treating the plating layer on the surfaces of the fragments until the fragments are invisible to naked eyes after deplating is finished for about 15 min;
(4) taking out the fragments subjected to deplating, ultrasonically cleaning the fragments in distilled water for about 1min to remove residual deplating agent, and quickly wiping the fragments by using filter paper to serve as a sample to be detected; 2.5057g of sample to be detected is accurately weighed, 20mL of analytically pure nitric acid is used for completely dissolving the sample to be detected, the volume is determined to be 100mL, the solution diluted by 20 times is continuously divided and diluted to be used as the solution to be detected of the trace elements; taking the solution diluted by 400 times as a to-be-detected solution of the rare earth element; simultaneously, performing a blank test;
(5) respectively preparing a mixed standard series solution of rare earth elements and a mixed standard series solution of trace elements: the rare earth elements comprise Nd, Pr, Dy, Ho, Gd, Tb and Ce, and the trace elements comprise Co, Al, Cu, Ga, Zr, Nb and B. Respectively taking rare earth element mixed standard solutions with different volumes, respectively adding the rare earth element mixed standard solutions into four 100mL volumetric flasks to prepare rare earth element mixed standard series solutions with different concentrations, wherein the concentrations of the rare earth element mixed standard series solutions are respectively as follows: 1. mu.g/mL, 5. mu.g/mL, 10. mu.g/mL, 20. mu.g/mL. And then, taking the mixed trace element standard solutions with different volumes, and respectively adding the mixed trace element standard solutions into four 100mL volumetric flasks to prepare the mixed trace element standard solutions with different concentrations. The concentrations are respectively 1 mug/mL, 5 mug/mL, 10 mug/mL and 20 mug/mL, and an iron matrix solution, a neodymium matrix solution and a praseodymium matrix solution with equivalent concentrations are added, and the concentrations are respectively 800 mug/mL, 350 mug/mL and 80 mug/mL;
(6) testing the emission light intensity of the mixed standard series solution of the rare earth elements and the mixed standard series solution of the trace elements by using an inductively coupled plasma emission spectrometer, and constructing a standard curve by taking the concentration of each element as an X axis and the analysis linear intensity as a Y axis;
(7) testing the emission light intensity of the liquid to be tested obtained in the step (4) by using an inductively coupled plasma emission spectrometer, and calculating the percentage content of each element in the deplated neodymium iron boron substrate by using the standard curve in the step (4);
(8) (6) and (7) the inductively coupled plasma emission spectrometer test conditions:
parameter(s) Set value Parameter(s) Set value
High frequency transmitter power (W) 1300 Plasma gas flow (L/min) 12
Auxiliary gas flow (L/min) 0.4 Atomizer gas flow (L/min) 0.7
Observation mode Vertical observation Analysis Pump speed (mL/min) 1.5
Characteristic analysis line (nm) of Nd 406.109 Characteristic analysis line (nm) of Pr 390.844
Characteristic analysis line (nm) of Dy 353.175 Characteristic analysis spectral line (nm) of Ho 345.600
Characteristic analysis line (nm) of Gd 376.844 Characteristic analysis line (nm) of Tb 350.917
Characteristic analysis line (nm) of Co 413.764 Characteristic analysis line (nm) of Al 273.313
Characteristic analysis line (nm) of Cu 324.755 Characteristic analysis line (nm) of Ga 294.364
Characteristic analysis line (nm) of Zr 343.823 Characteristic analytical line (nm) of Nb 316.340
Characteristic analysis line (nm) of B 208.889
(9) The rare earth elements in the sample to be detected comprise Nd, Pr, Dy, Ho, Gd, Tb and Ce according to the mass fraction wreIn% by weight, the value is calculated according to formula (1):
Figure BDA0002757424400000171
in formula (1):
v is the volume of the solution of the rare earth element to be detected, and the unit is milliliter (mL);
c is the concentration of the analysis element of the rare earth element solution to be detected, and the unit is microgram per milliliter (mu g/mL);
C0-the blank solution is analyzed for the concentration of the element in micrograms per milliliter (μ g/mL);
m is the mass of the sample to be measured in grams (g);
400-rare earth element dilution factor;
(10) the trace elements in the sample to be detected comprise Co, Al, Cu, Ga, Zr, Nb and B according to the mass fraction wteIn% by weight, the value is calculated according to equation (2):
Figure BDA0002757424400000181
in formula (2):
v is the volume of the solution of the trace element to be detected, and the unit is milliliter (mL);
c' -concentration of trace element in microgram per milliliter (mug/mL) of analytical element in the solution to be detected;
C′0-the blank solution is analyzed for the concentration of the element in micrograms per milliliter (μ g/mL);
m is the mass of the sample to be measured in grams (g);
20-trace element dilution times;
the contents of rare earth and trace elements in the sample to be tested of the neodymium iron boron matrix are shown in the following table:
table 9 contents of rare earth and trace elements in the neodymium iron boron matrix:
Figure BDA0002757424400000182
the same unknown sample is used for detection, and compared with the result of the embodiment 1, the difference value is small, the detection result is accurate, and the reproducibility is good.
The invention and its embodiments have been described above schematically, without limitation, and the actual method is not limited thereto. Therefore, if the person skilled in the art receives the teaching, without departing from the spirit of the invention, the person skilled in the art shall not inventively design the similar structural modes and embodiments to the technical solution, but shall fall within the scope of the invention.

Claims (7)

1. A method for measuring contents of rare earth and trace elements in a nickel-plated neodymium iron boron matrix by ICP-AES is characterized by comprising the following steps:
(1) preparing a deplating solution for surface coating treatment in advance, quantitatively weighing a corrosive agent and a complexing agent, adding the corrosive agent and the complexing agent into deionized water, stirring, and fixing the volume for later use after complete dissolution;
(2) crushing the nickel-containing plated neodymium iron boron magnet with unknown matrix component content to obtain neodymium iron boron fragments with equivalent diameter less than or equal to 0.5 cm;
(3) weighing 5g of fragments containing the plating layer, soaking the fragments in a deplating solution preheated to 60-80 ℃, uniformly and quickly removing the plating layer on the surface of the magnet, and treating the plating layer on the surface of the fragments until the fragments are invisible to naked eyes after deplating is finished;
(4) taking out fragments of the neodymium iron boron matrix subjected to deplating, ultrasonically cleaning the fragments in distilled water to remove residual deplating agent, and quickly wiping the fragments with filter paper to be used as a sample to be detected; accurately weighing 2.5g (accurate to 0.0001g) of sample to be detected, heating the sample to be detected by using 20mL of analytically pure nitric acid at low temperature until the sample is completely dissolved, fixing the volume to a 100mL volumetric flask, continuously taking and diluting the solution by 20 times, and taking the solution as the solution to be detected of the trace elements; taking the solution diluted by 400 times as a to-be-detected solution of the rare earth element; simultaneously, performing a blank test;
(5) respectively preparing a mixed standard series solution of rare earth elements and a mixed standard series solution of trace elements: the rare earth elements comprise Nd, Pr, Dy, Ho, Gd, Tb and Ce, and the trace elements comprise Co, Al, Cu, Ga, Zr, Nb and B; respectively taking rare earth element mixed standard solutions with different volumes, and respectively adding the rare earth element mixed standard solutions into four 100mL volumetric flasks to prepare rare earth element mixed standard series solutions with different concentrations; then, mixing trace element mixed standard solutions with different volumes, and adding the mixed standard solutions into four 100mL volumetric flasks respectively to prepare trace mixed standard series solutions with different concentrations; wherein, iron matrix solution, neodymium matrix solution and praseodymium matrix solution with equivalent concentration are added into the mixed standard series solution of the trace elements;
(6) testing the emission light intensity of the mixed standard series solution of the rare earth elements and the mixed standard series solution of the trace elements by using an inductively coupled plasma emission spectrometer, and constructing a standard curve by taking the concentration of each element as an X axis and the analysis linear intensity as a Y axis;
(7) and (5) testing the emission light intensity of the liquid to be tested obtained in the step (4) by using an inductively coupled plasma emission spectrometer, and calculating the percentage content of each element in the removed neodymium iron boron substrate by using the standard curve in the step (6).
2. The method of claim 1, wherein: the deplating agent in the step (1) comprises the following components in percentage by weight: the corrosive agent is sodium hydroxide or potassium hydroxide, and the content of the corrosive agent is 30-80 g/L; the complexing agent is disodium ethylene diamine tetraacetate, tetrasodium ethylene diamine tetraacetate, sodium ethylene diamine tetracetate or sodium citrate, the content of the disodium ethylene diamine tetraacetate and the tetrasodium ethylene diamine tetracetate is 5-20 g/L, the content of the sodium ethylene diamine tetracetate is 10-30 g/L, and the content of the sodium citrate is 3-15 g/L.
3. The method of claim 1, wherein: the volume-to-weight ratio of the deplating agent to the neodymium-iron-boron magnet containing the plating layer in the step (3) is 100 mL: 5g of the total weight.
4. The method of claim 1, wherein: the concentration of the mixed standard series solution of the rare earth elements in the step (5) is respectively as follows: 1. mu.g/mL, 5. mu.g/mL, 10. mu.g/mL, 20. mu.g/mL; the concentrations of the mixed standard series solutions of the trace elements are respectively 1 mug/mL, 5 mug/mL, 10 mug/mL and 20 mug/mL, wherein the concentration of an iron matrix is 800 mug/mL, the concentration of a neodymium matrix is 350 mug/mL, and the concentration of a praseodymium matrix is 80 mug/mL.
5. The method of claim 1, wherein: and (5) testing conditions of the inductively coupled plasma emission spectrometer in the steps (6) and (7):
parameter(s) Set value Parameter(s) Set value High frequency transmitter power (W) 1300 Plasma gas flow (L/min) 12 Auxiliary gas flow (L/min) 0.4 Atomizer gas flow (L/min) 0.7 Observation mode Vertical observation Analysis Pump speed (mL/min) 1.5 Characteristic analysis line (nm) of Nd 406.109 Characteristic analysis line (nm) of Pr 390.844 Characteristic analysis line (nm) of Dy 353.175 Characteristic analysis spectral line (nm) of Ho 345.600 Characteristic analysis line (nm) of Gd 376.844 Characteristic analysis line (nm) of Tb 350.917 Characteristic analysis line (nm) of Co 413.764 Characteristic analysis line (nm) of Al 273.313 Characteristic analysis line (nm) of Cu 324.755 Characteristic analysis line (nm) of Ga 294.364 Characteristic analysis line (nm) of Zr 343.823 Characteristic analytical line (nm) of Nb 316.340 Characteristic analysis line (nm) of B 208.889
。
6. The method of claim 1, wherein:
the content of the rare earth elements including Nd, Pr, Dy, Ho, Gd, Tb and Ce in the neodymium iron boron matrix in the step (7) is in mass fraction wreIn% by weight, the value is calculated according to formula (1):
Figure FDA0002757424390000021
in formula (1):
v is the volume of the solution of the rare earth element to be detected, and the unit is milliliter (mL);
c is the concentration of the analysis element of the rare earth element solution to be detected, and the unit is microgram per milliliter (mu g/mL);
C0-the blank solution is analyzed for the concentration of the element in micrograms per milliliter (μ g/mL);
m is the mass of the sample to be measured in grams (g);
400-rare earth element dilution factor.
7. The method of claim 1, wherein:
the microelements in the neodymium iron boron matrix in the step (7) comprise the contents of Co, Al, Cu, Ga, Zr, Nb and B in mass fraction wteIn% by weight, the value is calculated according to equation (2):
Figure FDA0002757424390000031
in formula (2):
v is the volume of the solution of the microelement to be detected, and the unit is milliliter (mL);
c' -concentration of trace element to be detected analysis element in microgram per milliliter (mug/mL);
C′0-the blank solution is analyzed for the concentration of the element in micrograms per milliliter (μ g/mL);
m is the mass of the sample to be measured in grams (g);
20-trace element dilution factor.
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CN112946055A (en) * 2021-02-08 2021-06-11 北京首钢股份有限公司 Method for measuring content of trace elements in galvanized steel

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102644080A (en) * 2012-04-28 2012-08-22 杭州广荣科技有限公司 Stripping liquid for sintering neodymium iron boron magnet chemical nickel plating layers
CN102787321A (en) * 2012-07-30 2012-11-21 牛凯 Deplating liquid for NiCuNi plating on surface of sintered NdFeB and deplating process thereof
CN109540804A (en) * 2018-09-30 2019-03-29 大冶特殊钢股份有限公司 The detection method of boron element in a kind of manganeisen
CN111272602A (en) * 2020-02-16 2020-06-12 南通市产品质量监督检验所 Method for measuring Al content of zinc-aluminum coating

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102644080A (en) * 2012-04-28 2012-08-22 杭州广荣科技有限公司 Stripping liquid for sintering neodymium iron boron magnet chemical nickel plating layers
CN102787321A (en) * 2012-07-30 2012-11-21 牛凯 Deplating liquid for NiCuNi plating on surface of sintered NdFeB and deplating process thereof
CN109540804A (en) * 2018-09-30 2019-03-29 大冶特殊钢股份有限公司 The detection method of boron element in a kind of manganeisen
CN111272602A (en) * 2020-02-16 2020-06-12 南通市产品质量监督检验所 Method for measuring Al content of zinc-aluminum coating

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
张友亮: "烧结钕铁硼产品不合格镍／铜／镍镀层退除速率的研究", 《电镀与环保》 *
董礼男等: "ICP-AES 法测定热镀锌−铝−镁合金层中 Al、Mg、Fe 的含量", 《电镀与涂饰》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112946055A (en) * 2021-02-08 2021-06-11 北京首钢股份有限公司 Method for measuring content of trace elements in galvanized steel

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