Sample treatment and phosphorus content detection method for phosphorus-containing rare earth polishing powder

Abstract

The invention discloses a sample treatment and phosphorus content detection method for phosphorus-containing rare earth polishing powder, and belongs to the technical field of detection. The method comprises the following steps: S1, testing by utilizing ICP-OES (Inductively Coupled Plasma-Optical Emission Spectrometer), firstly, carrying out semi-quantitative scanning on a sample of the phosphorus-containing rare earth polishing powder by adopting a qualitative scanning method, determining a concentration range, configuring each standard point of a standard solution according to the concentration range, and establishing a standard curve of to-be-tested elements; s2, respectively measuring the spectral intensity of the P element in the ultrapure water blank solution and the standard solution series in the S1 by adopting an inductively coupled plasma spectrum generator, and establishing a standard working curve of the P element; s3, respectively measuring the spectral intensity of the P element in the solution to be measured and the reagent blank solution by adopting an inductively coupled plasma spectrum generator; and S4, testing, and calculating the mass percentage content of the P element in the sample to be tested: WP = (CP-CP0) * V / (m * 106 * 100%).

Description

Technical Field

[0001] The invention belongs to the field of detection technology, and in particular relates to a sample processing method of phosphorus-containing rare earth polishing powder and a phosphorus content detection method. Background Art

[0002] New glass has played an increasingly important role in the development of the glass industry. In recent years, with the vigorous development of the domestic and foreign LCD panel industry, domestic LCD panel display technology has also developed rapidly, especially high-generation LCD panel display technology. From the perspective of the existing LCD panel industry, whether it is TFT-LCD or OLED, glass substrate is one of the important and key materials required for its production, and it is also the basic component of the LCD panel. At present, the production process of glass substrates includes float and overflow methods. The float process uses the density difference between tin liquid and glass to form glass plates. In order to meet the surface quality requirements, the side of the glass plate in contact with the tin liquid needs to be precisely polished. Glass substrates have the characteristics of large size, thin thickness, low density, high elastic modulus, and high stability, so they are extremely difficult to polish and have extremely high requirements for rare earth polishing materials.

[0003] In the field of precision grinding of high-generation substrate glass surfaces, rare earth polishing powder, as a core consumable, directly affects the processing accuracy and yield rate. Studies have found that in addition to the grinding performance of the main rare earth oxides, phosphorus, as a key additive, plays an important regulatory role in material properties: its content directly affects the dispersion stability of the polishing powder. Too high a phosphorus content will lead to increased particle agglomeration, while too low a phosphorus content will reduce the stability of the suspension system. Therefore, establishing an accurate phosphorus content detection method and optimizing the pre-treatment process are of great engineering value to improve the stability of polishing powder batches and reduce the scratch defect rate on the surface of high-generation glass substrates. Summary of the invention

[0004] In order to facilitate the detection of the phosphorus content in rare earth polishing powder, the present invention designs a sample processing and phosphorus content detection method for phosphorus-containing rare earth polishing powder. The sample processing method and the detection method are simple and highly operable, and can perform complete sample processing and quantitative analysis of the phosphorus content of the rare earth polishing powder. The phosphorus content in the rare earth polishing powder can be more accurately evaluated, and the effect of different contents of phosphorus-containing rare earth polishing powder on the grinding of glass substrates is analyzed, thereby improving the grinding efficiency and grinding quality.

[0005] The purpose of the present invention can be achieved through the following technical solutions:

[0006] A sample processing of phosphorus rare earth polishing powder comprises the following steps:

[0007] S1, drying the rare earth polishing powder to constant weight, taking it out and cooling it for standby use to obtain dry rare earth polishing powder;

[0008] S2, weighing dry rare earth polishing powder, placing it in a polytetrafluoroethylene microwave digestion tank, adding water to moisten it, adding perchloric acid to perform microwave digestion, and then heating to dissolve;

[0009] S3. When the liquid in the digestion tank is completely evaporated, slowly add hydrochloric acid solution to dissolve, cool to room temperature, transfer to a volumetric flask, and obtain a sample of phosphorus-containing rare earth polishing powder.

[0010] Furthermore, the drying temperature is 230-270°C.

[0011] Furthermore, the mass of the dry rare earth polishing powder is weighed accurately to 0.0001 g.

[0012] Furthermore, the amount of perchloric acid added is 8-12 mL.

[0013] Furthermore, the temperature of the heating and dissolving is 180-200° C., and the heating time is 20-30 min.

[0014] Furthermore, the hydrochloric acid solution is 10-15 mL of hydrochloric acid solution; the hydrochloric acid solution is prepared by mixing concentrated hydrochloric acid and ultrapure water in a ratio of 1:1.

[0015] Furthermore, when transferring to the volumetric flask, ultrapure water is used to clean the digestion tank in small amounts multiple times, and the cleaned liquid is transferred to the volumetric flask.

[0016] A method for detecting the phosphorus content of a sample of phosphorus-containing rare earth polishing powder comprises the following steps:

[0017] S1. Using ICP-OES to test, firstly adopt a qualitative scanning method to perform semi-quantitative scanning on the treated sample of phosphorus rare earth polishing powder to determine the concentration range, and then configure each standard point of the standard solution according to the concentration range, and finally use it to establish a standard curve of the element to be tested;

[0018] S2, using an inductively coupled plasma spectrometer to measure the spectral intensity of the P element in the ultrapure water blank solution and the standard solution series in S1, and establish a standard working curve of the P element;

[0019] S3, using an inductively coupled plasma spectrometer to respectively measure the spectral intensity of the P element in the test solution and the reagent blank solution;

[0020] S4. Test, input the dilution volume and dissolved mass, i.e. the mass m of the sample weighed after drying and cooling, through the calculation function of the equipment, and obtain the content of P in the rare earth polishing powder, and calculate the mass percentage of P element in the sample to be tested: W P =(C P -C P0 )×V / (m×106 ×100%).

[0021] Furthermore, the standard solution adopts a single element phosphorus standard solution, specification: 1000 μg / mL, manufacturer: National Nonferrous Metals and Electronic Materials Analysis and Testing Center.

[0022] Furthermore, W is the mass percentage of the element to be tested in the sample, in %; C P is the P element concentration of the solution to be tested, in μg / mL; C P0 is the concentration of P element in the reagent blank solution, in μg / mL; V is the fixed volume, in mL; m is the mass of the sample to be tested, in g.

[0023] Furthermore, the inductively coupled plasma spectrometer uses the Optima 8000 plasma emission spectrometer produced by PerkinElmer, and the test conditions are: RF power is 120-14000W, plasma gas intake rate is 10-15L / min; auxiliary gas intake rate is 0.23-0.4L / min, and atomization gas intake rate is 0.65-0.75L / min.

[0024] Furthermore, the method for determining the concentration range is: based on the qualitative result content ppm of the element scan, that is, the numerical size of mg / kg, this result is the estimated concentration value of the solution to be tested, the concentration range of the standard curve must include this result, and the upper limit of the concentration is the maximum concentration of the qualitative result + the maximum concentration of the qualitative result * (100%~140%) as the upper limit point of the standard curve. Setting the upper limit concentration point in this way can ensure the accuracy of the test result, that is, ensure that the estimated result is within the range of the standard curve.

[0025] The advantage is that the use of a microwave digestion tank to dissolve the sample can ensure that the sample is completely dissolved without the need for filtering or other operations, thereby ensuring the accuracy of the sample analysis.

[0026] The advantage is that perchloric acid is used as a single strong acid to dissolve the sample, and the chemical reagent used is a high-grade pure strong acid without other interfering reagents, which can reduce the introduction of impurities from external chemical reagents.

[0027] The advantage is that the use of ICP for content detection is more accurate than the previous spectrophotometer photometry method.

[0028] The advantage is that ICP qualitative analysis is first used to determine the concentration range of the sample to be tested, and then the standard curve method is used for quantitative analysis.

[0029] The advantage of the present invention is that the sample to be tested is first dried at a temperature of 250° C. to ensure the accuracy of the net weight of the sample.

[0030] Beneficial effects of the present invention:

[0031] (1) The present invention provides an efficient and accurate method for processing samples of phosphorus-containing rare earth polishing powder and detecting phosphorus content, aiming to provide reliable data support for the study of the correlation between phosphorus content and grinding performance in the glass substrate grinding process through simplified operation procedures and precise analysis techniques. The sample processing stage is divided into three steps: first, the sample to be tested is placed in a constant temperature drying oven for drying to completely remove moisture and volatile impurities to ensure weighing accuracy; second, a microwave digestion tank is used in combination with a single high-grade pure perchloric acid for gradient temperature digestion to achieve complete dissolution of the sample and avoid phosphorus loss caused by filtration; finally, the molten sample is precipitated with dilute hydrochloric acid to effectively avoid interference from impurities.

[0032] (2) The present invention uses an inductively coupled plasma optical emission spectrometer (ICP-OES) coupling technique: first, the concentration range is qualitatively determined by full spectrum scanning, and then a standard curve is established for quantitative analysis. Compared with traditional spectrophotometry, this method utilizes the high sensitivity and anti-interference ability of ICP-OES to reduce the relative standard deviation of detection and cover a wider concentration range. This method can systematically evaluate the effects of different phosphorus ratios on the dispersibility of polishing powder, grinding efficiency and surface roughness of glass substrates by accurately determining the phosphorus content, providing key technical support for the development of high-performance polishing materials and process optimization. DETAILED DESCRIPTION

[0033] The specific embodiments of the present invention are described in detail below, but it should be understood that the protection scope of the present invention is not limited by the specific embodiments.

[0034] According to the invention, this embodiment and the comparative example both use the Optima 8000 plasma emission spectrometer produced by PerkinElmer, and the test conditions are: RF power 1300W, plasma gas: 12L / min; auxiliary gas 0.3L / min, atomizing gas 0.7L / min. The specific steps are as follows:

[0035] (1) Turn on the host power and preheat for 0.5h;

[0036] (2) Turn on the circulating water device, confirm that the set temperature is 20°C, and confirm that the output pressure is 0.4MPa; connect the argon gas and control the pressure at 0.8MPa; turn on the air compressor, confirm that the output pressure is 0.75MPa, and open the ventilation hood;

[0037] (3) Turn on the computer and enter the ICP operating system. First, check whether the instrument is normal. Then create a new folder and set the conditions according to the measurement needs: plasma gas 12 L / min, auxiliary gas 0.3 L / min, and nebulizer gas 0.7 L / min;

[0038] (4) Ignite the plasma flame and perform optical initialization until the value is within the allowable range, generally required to be between ±50. If it exceeds the range, it is necessary to use 1ppm Mn standard solution to perform axial and directional alignment observation positions respectively to ensure the accuracy of the equipment detection results.

[0039] (5) After the measurement is completed, first extinguish the torch flame, close the argon valve, and then turn off the power.

[0040] Examples 1-6

[0041] This embodiment provides a method for sample processing and phosphorus content detection of phosphorus-containing rare earth polishing powder, comprising the following steps:

[0042] S1. Sample processing of phosphorus rare earth polishing powder:

[0043] (1) placing rare earth polishing powders of manufacturers A and B in a weighing bottle with constant weight, drying at 250° C. to constant weight, taking out and placing in a dryer, cooling, and obtaining dry rare earth polishing powders; weighing the rare earth polishing powder samples of manufacturers A and B that have been dried and cooled to a constant temperature, respectively, are Example 1 (A1#0.1001g), Example 2 (A2#0.1000g), Example 3 (A3#0.1002g), Example 4 (B1#0.1002g), Example 5 (B2#0.1001g), and Example 6 (B3#0.1000g);

[0044] (2) Weighing and drying the rare earth polishing powder was placed in a polytetrafluoroethylene microwave digestion tank, and then 10 mL of perchloric acid was accurately added for microwave digestion. The polytetrafluoroethylene digestion tank containing the sample was placed on an electric heating furnace and heated at 200° C. for dissolution;

[0045] (3) After 30 minutes, observe the dissolution in the digestion tank. When the liquid is completely evaporated, slowly add 10 mL of hydrochloric acid solution (prepared with 1:1 concentrated hydrochloric acid and ultrapure water) to dissolve. After complete dissolution, remove the polytetrafluoroethylene beaker in the digestion tank, cool it, and transfer it to a 100 mL volumetric flask. Use ultrapure water to clean the digestion tank in small amounts and multiple times. Transfer the cleaned liquid to the volumetric flask to ensure that it is transferred to the volumetric flask as completely as possible.

[0046] (4) Prepare a blank solution according to steps (2)-(3) and set aside.

[0047] S2. Phosphorus content detection

[0048] (1) Select the range of 180nm-800nm ​​to first perform a qualitative scan on the prepared test solution. The scanning results of the element P to be tested are shown in Table 1.

[0049] Table 1

[0050] factory Content / ppm Example 1 1570 Example 2 1560 Example 3 1556 Example 4 8350 Example 5 8200 Example 6 8315

[0051] (2) According to the elemental composition and semi-quantitative results of the qualitative scan, the maximum content of element P is 8350ppm. In the actual ICP test process, it is necessary to dilute it for testing, that is, take 0.5mL from the configured 100mL volumetric flask, dilute it to a 100mL volumetric flask, and test it to ensure the accuracy of the test data. That is, the maximum content of element P after conversion is about 42ppm. The maximum concentration of the qualitative result + the maximum concentration of the qualitative result * (100%~140%) is used as the upper limit concentration point of the standard curve. The specific preparation method is as follows: prepare 6 100mL volumetric flasks and number them 0#, 1#, 2#, 3#, 4#, and 5# respectively, and draw 0, 0.5, 1, 2, 5, and 10mL of standard solution (the standard solution uses phosphorus single element standard solution, specification: 1000μg / mL, manufacturer: National Nonferrous Metals and Electronic Materials Analysis and Testing Center), respectively, and add 10mL (1:1) concentrated hydrochloric acid at the same time, and finally add ultrapure water to the scale line. The configuration is complete and set aside.

[0052] (3) Set the element detection spectrum conditions, the detection spectrum wavelength of the element P to be tested is 213.618nm. Test result processing: The P element concentration C of the solution to be tested P and the P element concentration C in the reagent blank solution P0 ; Using formula W P =(C P -C P0 )×V / (m×10 6 ×100%), where W is the mass percentage of the element to be tested in the sample, in %; C P is the P element concentration of the solution to be tested, in μg / mL; C P0 is the concentration of P element in the blank solution of the reagent, in μg / mL; V is the fixed volume, in mL; m is the mass of the sample to be tested, in g; the phosphorus content in the final rare earth polishing powder obtained by calculation is shown in Table 2 below,

[0053] Table 2

[0054]

[0055] Example 1 is configured according to theoretical data, and the phosphorus content is 10.2%. The method of the present invention is used for detection and analysis. By analyzing and statistically analyzing the data obtained by the method of the present invention, it is found that the average value of the measured results is 10.3%, which deviates from the theoretical value by 0.1%, thereby proving the feasibility and effectiveness of the method of the present invention.

[0056] Embodiment 7-9

[0057] Phosphorus-free polishing powder was selected to add industrial sodium hexametaphosphate (content 68%) to verify the invention method, as follows:

[0058] S1. Sample processing: drying the phosphorus-free rare earth polishing powder and adding sodium hexametaphosphate.

[0059] (1) Take an appropriate amount of rare earth polishing powder into a weighing bottle with constant weight, dry it at 250° C. to constant weight, take it out and put it into a dryer, cool it for standby use; weigh 4.0000 g of the rare earth polishing powder that has been dried and cooled to a constant temperature, and add 4.0000 g of sodium hexametaphosphate, mix them completely, and obtain a mixed rare earth polishing powder sample; the weighed mixed rare earth polishing powder samples are respectively Example 7 (1# 0.1001 g), Example 8 (2# 0.1000 g), and Example 9 (3# 0.1002 g);

[0060] (2) Place the weighed sample in a polytetrafluoroethylene microwave digestion vessel, moisten it with water, then accurately add 10 mL of perchloric acid for microwave digestion, and place the polytetrafluoroethylene digestion vessel containing the sample in an electric heating furnace and heat it at 200°C for dissolution;

[0061] (3) After 30 minutes, observe the dissolution in the digestion tank. When the liquid is completely evaporated, slowly add 10 mL of 1:1 hydrochloric acid to dissolve it. After complete dissolution, remove the polytetrafluoroethylene beaker in the digestion tank, cool it, transfer it to a 100 mL volumetric flask, and wash it with ultrapure water in small amounts and multiple times to ensure that it is transferred to the volumetric flask as completely as possible.

[0062] (4) Prepare a blank solution according to steps (2)-(3) and set aside;

[0063] S2. Phosphorus content detection

[0064] According to the steps of Example 1, a suitable wavelength was selected for scanning, and the concentration range was first qualitatively analyzed, and then the quantitative analysis was completed by establishing a standard curve. The results are shown in Table 3.

[0065] Table 3

[0066]

[0067] Actual addition amount: the phosphorus content in sodium hexametaphosphate is 30%, and the content of sodium hexametaphosphate is 68%, so the actual phosphorus content is 20.4% in total. By adding 50% of the mixed rare earth polishing powder, the average value of the measured result is 10.36%, which deviates from the theoretical value by 0.16%. The actual content is consistent with the test result, which is sufficient to prove the feasibility and accuracy of the method of the present invention.

[0068] Further observation of the data of Examples 1-9 shows that the parallelism between each parallel sample data is good, thereby proving the stability of the present method.

[0069] Comparative Examples 1-3

[0070] The conventional spectrophotometric method, i.e., GB / T 12690.10-20 Chemical analysis method for non-rare earth impurities in rare earth metals and their oxides - Determination of phosphorus content - Molybdenum blue spectrophotometric method, was used to conduct comparative tests of Example 7. The same sample as Example 7, i.e., phosphorus-free polishing powder, was added with industrial sodium hexametaphosphate (content 68%) to conduct comparative verification of the inventive method, as follows:

[0071] S1. Sample processing: drying the phosphorus-free rare earth polishing powder and adding sodium hexametaphosphate.

[0072] (1) taking an appropriate amount of rare earth polishing powder into a weighing bottle with a constant weight, drying it at 250° C. to a constant weight, taking it out into a dryer, cooling it for standby use; weighing 4.0000 g of the rare earth polishing powder that has been dried and cooled to a constant temperature, adding 4.0000 g of sodium hexametaphosphate, and mixing them completely to obtain a mixed rare earth polishing powder;

[0073] S2. Sample analysis

[0074] (1) Accurately weigh 5.0000 g of analytical grade sodium hydroxide into a nickel crucible and heat at low temperature in a closed electric furnace to remove moisture;

[0075] (2) Accurately weigh the mixed rare earth polishing powders, namely, Comparative Example 1 (0.5000 g), Comparative Example 2 (0.5001 g), and Comparative Example 3 (0.5002 g), respectively, and place them in nickel crucibles filled with pre-dried sodium hydroxide, and melt them in a muffle furnace at 700-750° C. for 6-7 minutes. After taking them out and cooling them slightly, place them in a 300 mL beaker and soak them with about 150 mL of hot water. Rinse the crucible with hot water, cool to room temperature, transfer them to a 200 mL volumetric flask, dilute to the mark with water, and shake well.

[0076] (3) Filter with rapid quantitative filter paper, take 0.5 mL of the filtered solution and place it in a 25 mL volumetric flask, add a drop of p-nitrophenol (10 g / L), adjust the solution to yellow with 10% ammonia water, and adjust the solution to yellow with 25% hydrochloric acid. Add 1.6 mL of 50% hydrochloric acid, 0.6 mL of ammonium molybdate, shake while adding, 2 mL of starch solution, 1.5 mL of ascorbic acid (20 g / L), 0.5 mL of potassium antimony tartrate solution, dilute to the mark with high-purity water, shake well and set aside;

[0077] (4) 10 minutes after color development, immediately use an L3S spectrophotometer. Use a 1 cm cuvette, a wavelength of 690 nm, and adjust the reagent blank to zero. Draw a standard curve with the absorbance measured by the instrument as the ordinate and the corresponding phosphate content as the abscissa;

[0078] (5)P 2 O 5 (%) = (10000*C / 10 6 *G) / 1.338*100=C / G*1.338

[0079] In the above formula, C: phosphate concentration value (μg / mL) obtained from the standard curve; G: weight of the sample taken (g); 10 6 : Conversion factor between g and μg; 10000: dilution factor of the sample; 1.338: PO 4- With P 2 O 5 The results are shown in Table 4:

[0080] Table 4

[0081]

[0082] Analysis of results: The deviation from the theoretical value is 0.23%. Through comparison of the test data of Examples 7-9 and Comparative Examples 1-3, it is verified that the test results of Examples 7-9 according to the method of the present invention deviate from the theoretical value by 0.16%, and the deviation of Comparative Examples 1-3 is 0.23%, which can verify the detection accuracy and effectiveness of the method of the present invention.

[0083] Comparative Examples 4-6

[0084] Phosphorus-free polishing powder was added with industrial sodium hexametaphosphate (content 68%) for comparative examples 4-6, and the method of the present invention was further verified with examples 7-9. The specific difference was that the prepared phosphorus-free polishing powder was directly added with industrial sodium hexametaphosphate (content 68%) for weighing, and the dissolution method of the present invention was used for testing and analysis. The details are as follows:

[0085] S1. Sample processing

[0086] (1) Weigh the mixed rare earth polishing powder samples as Comparative Example 4 (1# 0.1002 g), Comparative Example 5 (2# 0.1001 g), and Comparative Example 6 (3# 0.1000 g);

[0087] (2) Place the weighed sample in a polytetrafluoroethylene microwave digestion vessel, moisten it with water, then accurately add 10 mL of perchloric acid for microwave digestion, and place the polytetrafluoroethylene digestion vessel containing the sample in an electric heating furnace and heat it at 200°C for dissolution;

[0088] (3) After 30 minutes, observe the dissolution in the digestion tank. When the liquid is completely evaporated, slowly add 10 mL of 1:1 hydrochloric acid to dissolve it. After complete dissolution, remove the polytetrafluoroethylene beaker in the digestion tank, cool it, transfer it to a 100 mL volumetric flask, and wash it with ultrapure water in small amounts and multiple times to ensure that it is transferred to the volumetric flask as completely as possible.

[0089] (4) Prepare a blank solution according to steps (2)-(3) and set aside;

[0090] S2. Phosphorus content detection

[0091] (1) According to the steps of Example 7, a suitable wavelength was selected for scanning, and the concentration range was first qualitatively analyzed, and then a standard curve was established to complete the quantitative analysis. The results are shown in Table 5;

[0092] Table 5

[0093]

[0094] According to the theoretical calculation value of Example 7, the theoretical phosphorus content of the sample is 10.2%. The average value of the measured results of this comparative example is 9.93%, which deviates from the theoretical value by 0.27%, and the deviation is relatively large.

[0095] To further verify the method of the present invention, the samples in comparative examples 4-6 were dried at 250°C to constant weight, and the loss on ignition was calculated to be 2.37%. The actual content of the sample calculated based on the loss on ignition was about 10.17%, which was close to the theoretical value, thereby further demonstrating the feasibility and accuracy of the method of the present invention.

[0096] The above disclosures are only several specific embodiments of the present invention. However, the embodiments of the present invention are not limited thereto. Any changes that can be conceived by those skilled in the art should fall within the protection scope of the present invention.

Claims

1. A method for detecting the phosphorus content of a sample of phosphorus-containing rare earth polishing powder, characterized in that: The following steps are involved: S1. Using ICP-OES to test, firstly adopt a qualitative scanning method to perform semi-quantitative scanning on the treated sample of phosphorus rare earth polishing powder to determine the concentration range, and then configure each standard point of the standard solution according to the concentration range to establish a standard curve of the element to be tested; S2. Establishing a standard working curve of element P using an inductively coupled plasma spectrometer; S3, using an inductively coupled plasma spectrometer to respectively measure the spectral intensity of the P element in the test solution and the reagent blank solution; S4. Perform the test and calculate the mass percentage of P element in the sample to be tested: W P =(C P -C P0 )×V / (m×10 6 ×100%).

2. The method for detecting the phosphorus content of a sample of a phosphorus-containing rare earth polishing powder according to claim 1, characterized in that: The step of establishing the standard working curve of the P element comprises: respectively measuring the spectral intensity of the P element in the ultrapure water blank solution and the standard solution series in S1.

3. The method for detecting the phosphorus content of a sample of a phosphorus-containing rare earth polishing powder according to claim 1, characterized in that: The test comprises: inputting the dilution volume and the dissolved mass, that is, the mass m of the sample weighed after drying and cooling, through the calculation function of the equipment, to obtain the content of P in the rare earth polishing powder.

4. The method for detecting the phosphorus content of a sample of a phosphorus-containing rare earth polishing powder according to claim 1, characterized in that: The standard solution adopts phosphorus single element standard solution, with a specification of 1000 μg / mL, and the manufacturer is the National Nonferrous Metals and Electronic Materials Analysis and Testing Center; W is the mass percentage of the element to be tested in the sample, in %; C P is the P element concentration of the solution to be tested, in μg / mL; C P0 is the concentration of P element in the reagent blank solution, in μg / mL; V is the fixed volume, in mL; m is the mass of the sample to be tested, in g.

5. The method for detecting the phosphorus content of a sample of a phosphorus-containing rare earth polishing powder according to claim 1, characterized in that: The inductively coupled plasma spectrometer is an Optima 8000 plasma emission spectrometer produced by PerkinElmer, and the test conditions are: RF power is 120-14000W, and the plasma gas intake rate is 10-15L / min; The auxiliary gas intake rate is 0.23-0.4L / min, and the atomizing gas intake rate is 0.65-0.75L / min.

6. The method for detecting the phosphorus content of a sample of a phosphorus-containing rare earth polishing powder according to claim 1, characterized in that: The method for determining the concentration range is: based on the qualitative result content ppm of the element scan, that is, the numerical value of mg / kg, this result is the estimated concentration value of the solution to be tested, the concentration range of the standard curve must include this result, and the upper limit of the concentration is the maximum concentration of the qualitative result + the maximum concentration of the qualitative result * (100%~140%) as the upper limit point of the standard curve. Setting the upper limit concentration point in this way can ensure the accuracy of the test result, that is, ensure that the estimated result is within the range of the standard curve.

7. The method for detecting the phosphorus content of a sample of a phosphorus-containing rare earth polishing powder according to claim 1, characterized in that: The sample of the treated phosphorus rare earth polishing powder comprises the following steps: S1, drying the rare earth polishing powder to constant weight, taking it out and cooling it for standby use to obtain dry rare earth polishing powder; S2, weighing dry rare earth polishing powder, placing it in a polytetrafluoroethylene microwave digestion tank, adding water to moisten it, adding perchloric acid to perform microwave digestion, and then heating to dissolve; S3. When the liquid in the digestion tank is completely evaporated, slowly add hydrochloric acid solution to dissolve, cool to room temperature, transfer to a volumetric flask, and obtain a sample of phosphorus-containing rare earth polishing powder.

8. The method for detecting the phosphorus content of a sample of phosphorus-containing rare earth polishing powder according to claim 7, characterized in that: The drying temperature is 230-270° C.; the heating and dissolving temperature is 180-200° C., and the heating time is 20-30 min; the mass of the dry rare earth polishing powder is weighed accurately to 0.0001 g.

9. The method for detecting the phosphorus content of a sample of phosphorus-containing rare earth polishing powder according to claim 7, characterized in that: The amount of perchloric acid added is 8-12 mL.

10. The method for detecting the phosphorus content of a sample of phosphorus-containing rare earth polishing powder according to claim 7, characterized in that: The hydrochloric acid solution is 10-15mL of hydrochloric acid solution; the hydrochloric acid solution is prepared by mixing concentrated hydrochloric acid and ultrapure water in a ratio of 1:1; when transferring to a volumetric flask, ultrapure water is used to clean the digestion tank in small amounts multiple times, and the cleaned liquid is transferred to the volumetric flask.

Images