Method for determining neodymium element in high-temperature alloy

Abstract

The invention discloses a method for determining a neodymium element in a high-temperature alloy. The method comprises the following steps: S1, taking a 406.109 nm neodymium element spectral line spectrograph as equipment for detecting the neodymium element and other elements except phosphorus, silicon, boron, magnesium and calcium in the high-temperature alloy; s2, preparing a neodymium element standard solution, a high-temperature alloy standard substance and a reagent; s3, weighing a matrix and coexisting elements, wherein the content of the matrix and the coexisting elements is close to that of the to-be-detected high-temperature alloy sample and the to-be-detected high-temperature alloy sample, and processing into a to-be-detected solution; s4, establishing a working curve of the neodymium element and other elements except phosphorus, silicon, boron, magnesium and calcium by using a spectrograph; s5, the content of the neodymium element in the high-temperature alloy sample in the S3 is measured through a spectrograph; and if the high-temperature alloy standard substance containing other coexisting elements except the neodymium element is supplemented in S4, measuring the contents of other elements except phosphorus, silicon, boron, magnesium and calcium by using a spectrograph. According to the method for determining the neodymium element in the high-temperature alloy, the problem that the neodymium element in the high-temperature alloy cannot be determined in the prior art is solved.

Description

Technical Field

[0001] The invention belongs to the technical field of analysis and testing, and in particular relates to a method for determining neodymium elements in high-temperature alloys. Background Art

[0002] High-temperature alloys are widely used in aerospace, naval aviation, medicine and other fields. They are one of the materials used to manufacture important parts of aircraft engines. Compared with other high-temperature alloy materials, high-temperature alloys have relatively higher high-temperature strength, thermal corrosion resistance, fatigue resistance and creep resistance. The rare earth neodymium element added to high-temperature alloys is mainly used to improve oxidation resistance and has a greater impact on plasticity. It will affect the segregation behavior of other elements, so the control of neodymium content is very strict. The most commonly used high-temperature alloys require the neodymium content to be less than or equal to 0.05%, which requires accurate detection of the neodymium content. At present, there is no standard test method for determining neodymium in high-temperature alloys. Using inductively coupled plasma atomic emission spectrometry, multiple elements can be determined in one dissolution, so the operation is simple, the analysis and determination process is short, time-saving and labor-saving, the amount of reagents is small, environmental pollution is reduced, and the health of test personnel is protected. However, there is no reliable method for accurately determining neodymium in high-temperature alloys with a content of less than or equal to 0.05%. There are no related reports in the journal. At the same time, after searching patents, there is no method for determining neodymium in high-temperature alloys using inductively coupled plasma atomic emission spectrometry. Therefore, it is of great significance to use inductively coupled plasma atomic emission spectrometry to determine neodymium in high-temperature alloys. Summary of the invention

[0003] The purpose of the present invention is to provide a method for determining the neodymium element in a high-temperature alloy, thereby solving the problem that the prior art cannot determine the neodymium element in a high-temperature alloy.

[0004] The technical solution adopted by the present invention is a method for determining the neodymium element in a high-temperature alloy, comprising the following steps:

[0005] S1. A full spectrum direct-reading inductively coupled plasma emission spectrometer that tests the 406.109 nm neodymium element spectrum is used as a device to detect neodymium and other elements except phosphorus, silicon, boron, magnesium and calcium in high-temperature alloys;

[0006] S2. Prepare neodymium standard solution, high temperature alloy standard substances and reagents;

[0007] S3, weighing a high-temperature alloy standard sample and a high-temperature alloy sample to be tested whose contents of the matrix and coexisting elements are close to those of the high-temperature alloy sample to be tested, and treating them into a solution to be tested;

[0008] S4, using the spectrometer in S1 to establish working curves for neodymium and other elements except phosphorus, silicon, boron, magnesium and calcium;

[0009] S5. The content of neodymium in the high-temperature alloy sample in S3 is measured by a spectrometer. If a high-temperature alloy standard material containing other coexisting elements except neodymium is added to S4, the contents of other elements except phosphorus, silicon, boron, magnesium and calcium are measured by a spectrometer.

[0010] The present invention is also characterized in that:

[0011] The performance of the equipment in S1 should ensure that the detection limit of the neodymium element must be better than 0.0001%, the relative standard deviation of 0.10% neodymium element measured for 10 consecutive times is no more than 1.00%, and the linear correlation coefficient of the working curve of the measured neodymium element is greater than 0.999.

[0012] The content of the matrix and coexisting elements of the high-temperature alloy standard material in S2 is close to that of the high-temperature alloy sample to be tested; the content of the neodymium element standard solution is 0.02 mg·mL -1 ; Reagents are sulfuric acid: high grade, ρ is 1.84g·ml -1 ; Phosphoric acid: high purity, ρ is 1.69 g·ml -1 ; Water: secondary water; Nitric acid: high purity, ρ is 1.42g·ml -1 ; Hydrochloric acid: high purity, ρ is 1.19 g·ml -1 .

[0013] The specific process of S3 is as follows: weigh 0.1000g of the matrix and 6 high-temperature alloy standard samples whose coexisting element contents are close to those of the high-temperature alloy sample to be tested, a high-temperature alloy standard material containing other elements except phosphorus, silicon, boron, magnesium and calcium, and 0.100g of the sample to be tested in a 150ml conical flask, weigh the high-temperature alloy sample accurately to 0.0001g, add 10ml~30ml of hydrochloric acid and 1ml~4ml of nitric acid in sequence, heat in the temperature range of 100℃~150℃ until the high-temperature alloy sample is completely dissolved, add 3ml~5ml of sulfuric acid and phosphoric acid mixed acid with a volume ratio of (1+2) to the dissolved solution, heat in the temperature range of 300℃~350℃ to generate smoke, decarbonize with 2ml of nitric acid once, and cool; add 15ml~30ml of water along the wall of the flask, heat and boil until the dissolved solution is clear, and after cooling, make up to the volume in a 100ml volumetric flask, shake well, and obtain the solution to be tested.

[0014] The specific process of S4 is as follows: the mass concentration of six neodymium elements is 0 mg·L -1 , 0.2mg·L -1 , 0.4mg·L -1 , 0.6mg·L -1 , 0.8mg·L -1 , 1.0mg·L -1The neodymium standard working solution is tested. If the neodymium element is at a mass fraction of 1.0 mg·L -1 If the linearity is within the range and the linear correlation coefficient is above 0.999, and the correlation coefficients of other elements except phosphorus, silicon, boron, magnesium and calcium are above 0.999, then a working curve is established and the next step is carried out; otherwise, S3 and S4 are repeated until the neodymium element is within the mass fraction of 1.0 mg·L -1 The range is linear, and the linear correlation coefficient is above 0.999. Except for phosphorus, silicon, boron, magnesium and calcium, the correlation coefficients of other elements are above 0.999.

[0015] The beneficial effects of the present invention are:

[0016] 1. Less reagent usage: The present invention firstly uses hydrochloric acid and nitric acid to dissolve the sample, and then adds sulfuric acid and phosphoric acid mixed acid to generate smoke after dissolution. Finally, only 3ml to 5ml of sulfuric acid and phosphoric acid mixed acid with a volume ratio of (1+2) in a 100ml volumetric flask is contained, thereby reducing pollution to the environment and protecting the health of test personnel.

[0017] 2. The 406.109nm neodymium spectrum line can effectively avoid the weak interference of the matrix and the coexisting element cerium on the neodymium element, and improve the accuracy and reliability of the data;

[0018] 3. Use standard substances with similar content of matrix and coexisting elements to the sample plus neodymium standard solution to establish a working curve. This method not only avoids the use of at least 10 kinds of coexisting element standard solutions and high-purity nickel or high-purity iron, but also saves detection costs, simplifies the operation process, and ultimately improves the analysis efficiency and the accuracy and reliability of the test data;

[0019] 4. The sample processing process is simple and easy, including the method of dissolving the sample with acid, using a 150ml conical flask for sample pretreatment, and appropriate heating temperature, which together ensure that the high-temperature alloy standard solution and the high-temperature alloy sample are processed into the solution to be tested in about 20 to 30 minutes;

[0020] 5. The matrix and the coexisting elements and the high-temperature alloy sample are used to prepare a high-temperature alloy matrix blank solution according to S3, and the content of the neodymium element is measured 11 times in the high-temperature alloy matrix blank solution at the same time, and the detection limit of the neodymium element is calculated. The present invention achieves a very low detection limit (Nd: 0.0001%), ensuring that the lower limit of neodymium detection reaches 0.001%;

[0021] 6. The solution prepared by the method used in S3 is used to supplement the high-temperature alloy standard substances containing other elements in addition to phosphorus, silicon, boron, magnesium and calcium in the high-temperature alloy sample, so that the synchronous detection of the remaining elements except phosphorus, silicon, boron, magnesium and calcium can be realized, which significantly improves the detection efficiency and reduces the detection cost;

[0022] 7. Combined with the beneficial effects of the previous 6 points, it is ultimately ensured that the linearity of the 5 neodymium standard solutions can reach above 0.999, and the synchronous detection of the content of neodymium and other elements except phosphorus, silicon, boron, magnesium and calcium in the high-temperature alloy sample can be accurately detected within 1 hour. The process includes preparing reagents, weighing samples, processing samples into test solutions, and finally detecting the content of neodymium and other elements except phosphorus, silicon, boron, magnesium and calcium in the high-temperature alloy sample, which greatly reduces the detection cost, improves the detection efficiency and the accuracy and reliability of the test results;

[0023] The invention solves the problem that there is no relevant detection method for determining the neodymium element in the high-temperature alloy at present. The detection method involved in the invention has the characteristics of small reagent consumption, simple and easy operation process, fast and stable detection, synchronous determination of the contents of other elements except phosphorus, silicon, boron, magnesium and calcium, high accuracy and good precision of the analysis result, etc., and supplements the high-temperature alloy standard substances containing other elements except phosphorus, silicon, boron, magnesium and calcium in the high-temperature alloy sample, and finally ensures that the beneficial effect of accurately and efficiently detecting the contents of the neodymium element and other elements except phosphorus, silicon, boron, magnesium and calcium in the high-temperature alloy of 0.001% to 0.10% can be achieved. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 This is a linear correlation coefficient diagram of the neodymium element in the method for determining the neodymium element in a high-temperature alloy according to the present invention. DETAILED DESCRIPTION

[0025] The present invention is described in detail below in conjunction with specific implementation modes and accompanying drawings.

[0026] The method for determining the neodymium element in a high-temperature alloy provided by the present invention comprises the following steps:

[0027] S1. A full spectrum direct-reading inductively coupled plasma emission spectrometer that tests the 406.109 nm neodymium element spectrum is used as a device to detect neodymium and other elements except phosphorus, silicon, boron, magnesium and calcium in high-temperature alloys;

[0028] Equipment parameters should ensure that the detection limit of neodymium must be better than 0.0001%, the relative standard deviation of 0.10% neodymium measured for 10 consecutive times is no more than 1.00%, and the linear correlation coefficient of the working curve of the measured neodymium is greater than 0.999;

[0029] S2. Prepare neodymium standard solution, high temperature alloy standard substances and reagents;

[0030] The high-temperature alloy standard material has a matrix and coexisting element content close to that of the high-temperature alloy sample to be tested;

[0031] The content of neodymium standard solution is 0.02 mg·mL -1 ;

[0032] The reagents used were sulfuric acid: high-grade pure, ρ1.84g·ml -1 ;

[0033] Phosphoric acid: high purity, ρ is 1.69 g·ml -1 ;

[0034] Water: Secondary water;

[0035] Nitric acid: high purity, ρ is 1.42 g·ml -1 ;

[0036] Hydrochloric acid: high purity, ρ is 1.19 g·ml -1 ;

[0037] S3, weighing a high-temperature alloy standard sample and a high-temperature alloy sample to be tested whose contents of the matrix and coexisting elements are close to those of the high-temperature alloy sample to be tested, and treating them into a solution to be tested;

[0038] The specific process of S3 is as follows: weigh 0.1000g of the matrix and 6 high-temperature alloy standard samples whose coexisting element content is close to that of the high-temperature alloy sample to be tested, high-temperature alloy standard materials containing other elements except phosphorus, silicon, boron, magnesium and calcium, and 0.100g of the sample to be tested in a 150ml conical flask, weigh the high-temperature alloy sample accurately to 0.0001g, add 10ml-30ml of hydrochloric acid and 1ml-4ml of nitric acid in sequence, heat in the temperature range of 100℃-150℃ until the high-temperature alloy sample is completely dissolved, add 3ml-5ml of sulfuric acid and phosphoric acid mixed acid with a volume ratio of (1+2) to the solution, heat in the temperature range of 300℃-350℃ to generate smoke, decarbonize with 2ml of nitric acid once, and cool; add 15ml-30ml of water along the wall of the flask, heat and boil until the solution is clear, and after cooling, adjust the volume in a 100ml volumetric flask, shake well, and obtain the solution to be tested;

[0039] S4. Use the spectrometer in S1 to establish working curves for neodymium and other elements except phosphorus, silicon, boron, magnesium, and calcium, such as Figure 1 As shown;

[0040] The specific process of S4 is as follows: the mass concentration of six neodymium elements is 0 mg·L -1 , 0.2mg·L -1 , 0.4mg·L -1 , 0.6mg·L -1 , 0.8mg·L -1 , 1.0mg·L -1 The neodymium standard working solution is tested. If the neodymium element is at a mass fraction of 1.0 mg·L -1If the linearity is within the range and the linear correlation coefficient is above 0.999, and the correlation coefficients of other elements except phosphorus, silicon, boron, magnesium and calcium are above 0.999, then a working curve is established and the next step is carried out; otherwise, S3 and S4 are repeated until the neodymium element is within the mass fraction of 1.0 mg·L -1 The linear range is linear, and the linear correlation coefficient is above 0.999. Except for phosphorus, silicon, boron, magnesium and calcium, the correlation coefficients of other elements are above 0.999.

[0041] S5. The content of neodymium in the high-temperature alloy sample in S3 is measured by a spectrometer. If a high-temperature alloy standard material containing other coexisting elements except neodymium is added to S4, the contents of other elements except phosphorus, silicon, boron, magnesium and calcium are measured by a spectrometer.

[0042] Example 1

[0043] The method for determining the neodymium element in the high-temperature alloy proposed in this embodiment comprises the following steps:

[0044] Analysis of high temperature alloy standard sample G1

[0045] Step 1, using a full spectrum direct-reading inductively coupled plasma emission spectrometer that tests the 406.109 nm neodymium element spectrum as a device for detecting the neodymium content in the high-temperature alloy standard sample G1;

[0046] The parameters set by the equipment ensure that the detection limit of the neodymium element is 0.00009%, which is better than 0.0001%. The relative standard deviation of 0.10% neodymium element measured for 10 consecutive times is 0.77%, which is less than 1.00%. The linear correlation coefficient of the working curve of the measured neodymium element is greater than 0.999, which meets the requirements of the present invention.

[0047] Step 2: Prepare the neodymium standard solution, high temperature alloy standard substances and reagents:

[0048] Neodymium standard solution: content 0.02mg·mL -1 Neodymium element standard solution;

[0049] High temperature alloy standard material: The content of matrix and coexisting elements is close to that of the high temperature alloy standard sample G1 to be tested;

[0050] The reagents used were sulfuric acid: high-grade pure, ρ1.84g·ml -1 ;

[0051] Phosphoric acid: high purity, ρ is 1.69 g·ml -1 ;

[0052] Water: Secondary water;

[0053] Nitric acid: high purity, ρ is 1.42 g·ml-1 ;

[0054] Hydrochloric acid: high purity, ρ is 1.19 g·ml -1 ;

[0055] Step 3, weigh the matrix and the coexisting elements content close to the high temperature alloy standard sample G1 to be tested and the high temperature alloy standard sample G1 to be tested and process them into a solution to be tested,

[0056] Specifically, 0.1000g of the matrix and 6 high-temperature alloy standard samples whose coexisting element contents are close to that of the high-temperature alloy standard sample G1 to be tested and 0.100g of the standard sample G1 to be tested are weighed in a 150ml conical flask, the high-temperature alloy standard sample G1 is weighed accurately to 0.0001g, 10ml of hydrochloric acid and 3ml of nitric acid are added in sequence, and heated at 100°C until the high-temperature alloy sample is completely dissolved, 3ml of sulfuric acid and phosphoric acid mixed acid with a volume ratio of (1+2) is added to the solution, heated at 330°C to generate smoke, carbonized with 2ml of nitric acid once, and cooled; 15ml of water is added along the wall of the flask, heated and boiled until the solution is clear, and after cooling, it is fixed to volume in a 100ml volumetric flask, shaken well, and the solution to be tested is obtained;

[0057] Step 4, using the spectrometer in step 1 to establish a neodymium element working curve;

[0058] The specific process is as follows: the mass concentration of six parts of neodymium elements are 0 mg·L -1 , 0.2mg·L -1 , 0.4mg·L -1 , 0.6mg·L -1 , 0.8mg·L -1 , 1.0mg·L -1 The neodymium standard working solution was tested, that is, the neodymium standard working solution with the same matrix composition as the high-temperature alloy standard sample G1 was used to draw the working curve. The neodymium element was at a mass fraction of 1.0 mg·L -1 The range is linear, and the linear correlation coefficient is 0.9999. If it is above 0.999, proceed to the next step;

[0059] Step 5, input the weight of the high-temperature alloy standard sample G1 in step 3 and the volume of the high-temperature alloy solution to be tested, and measure the content of neodymium in the high-temperature alloy standard sample G1 by a spectrometer; the results are shown in Table 1. It can be seen from Table 1 that the measured value of the standard sample is consistent with the recognized value, and the relative standard deviation is less than 5%. This method has high accuracy and good precision;

[0060] Table 1 Analysis results of high temperature alloy standard sample G1 (n=10)

[0061]

[0062] In addition, the matrix and the coexisting elements and the high-temperature alloy standard sample G1 are used to prepare a high-temperature alloy matrix blank solution according to step 3, and the content of the neodymium element is determined 11 times in the high-temperature alloy matrix blank solution at the same time, and the detection limit of the neodymium element is calculated. The present invention achieves a very low detection limit (Nd: 0.00009%). The method of the present invention ensures that the detection limit of the neodymium element reaches 0.001%. The method of the present invention meets the requirements for neodymium element analysis. When the equipment of step 1 is used to determine the neodymium element again using the method of the present invention, this step operation can be omitted.

[0063] Example 2

[0064] Analysis of high temperature alloy standard sample G2

[0065] Step 1, using a full spectrum direct-reading inductively coupled plasma emission spectrometer that tests the 406.109 nm neodymium element spectrum as a device for detecting the neodymium content in the high-temperature alloy standard sample G2;

[0066] The parameters set by the equipment ensure that the detection limit of the neodymium element is 0.00009%, which is better than 0.0001%. The relative standard deviation of 0.10% neodymium element measured for 10 consecutive times is 0.77%, which is less than 1.00%. The linear correlation coefficient of the working curve of the measured neodymium element is greater than 0.999, which meets the requirements of the present invention.

[0067] Step 2: Prepare the neodymium standard solution, high temperature alloy standard substances and reagents:

[0068] Neodymium standard solution: content 0.02mg·mL -1 Neodymium element standard solution;

[0069] High temperature alloy standard material: The content of matrix and coexisting elements is close to that of the high temperature alloy standard sample G2 to be tested;

[0070] The reagents used were sulfuric acid: high-grade pure, ρ1.84g·ml -1 ;

[0071] Phosphoric acid: high purity, ρ is 1.69 g·ml -1 ;

[0072] Water: Secondary water;

[0073] Nitric acid: high purity, ρ is 1.42 g·ml -1 ;

[0074] Hydrochloric acid: high purity, ρ is 1.19 g·ml -1 ;

[0075] Step 3, weighing the matrix and the coexisting element content close to the high-temperature alloy standard sample G2 to be tested and the high-temperature alloy standard sample G2 to be tested and processing them into a solution to be tested;

[0076] Specifically, 0.1000g of the matrix and 6 high-temperature alloy standard samples whose coexisting element contents are close to that of the high-temperature alloy standard sample G2 to be tested and 0.100g of the standard sample G2 to be tested are weighed in a 150ml conical flask, the high-temperature alloy standard sample G2 is weighed accurately to 0.0001g, 15ml of hydrochloric acid and 1ml of nitric acid are added in sequence, and heated at 120°C until the high-temperature alloy sample is completely dissolved, 5ml of sulfuric acid and phosphoric acid mixed acid with a volume ratio of (1+2) is added to the solution, heated at 340°C to generate smoke, carbonized with 2ml of nitric acid once, and cooled; 20ml of water is added along the wall of the flask, heated and boiled until the solution is clear, and after cooling, it is fixed to volume in a 100ml volumetric flask, shaken well, and the solution to be tested is obtained;

[0077] Step 4, using the spectrometer in step 1 to establish a neodymium element working curve;

[0078] The specific process is as follows: the mass concentration of six parts of neodymium elements are 0 mg·L -1 , 0.2mg·L -1 , 0.4mg·L -1 , 0.6mg·L -1 , 0.8mg·L -1 , 1.0mg·L -1 The neodymium standard working solution was tested, that is, the neodymium standard working solution with the same matrix composition as the high-temperature alloy standard sample G2 was used to draw the working curve. The neodymium element was at a mass fraction of 1.0 mg·L -1 The range is linear, and the linear correlation coefficient is 0.9997. If it is above 0.999, proceed to the next step;

[0079] Step 5, input the weight of the high-temperature alloy standard sample G2 in step 3 and the volume of the high-temperature alloy solution to be tested, and measure the content of neodymium in the high-temperature alloy standard sample G2 by full-spectrum direct-reading inductively coupled plasma emission spectrometer; the results are shown in Table 2. It can be seen from Table 2 that the measured value of the standard sample is consistent with the recognized value, and the relative standard deviation is less than 5%. This method has high accuracy and good precision;

[0080] Table 2 Analysis results of high temperature alloy standard sample G2 (n=10)

[0081]

[0082] Example 3

[0083] Analysis of Spiked Recovery Rate of High-temperature Alloy Standard Sample G2

[0084] Step 1, using a full spectrum direct-reading inductively coupled plasma emission spectrometer that tests the 406.109 nm neodymium element spectrum as a spike recovery analysis device for detecting the neodymium content in the high-temperature alloy standard sample G2;

[0085] The parameters set by the equipment ensure that the detection limit of the neodymium element is 0.00009%, which is better than 0.0001%. The relative standard deviation of 0.10% neodymium element measured for 10 consecutive times is 0.77%, which is less than 1.00%. The linear correlation coefficient of the working curve of the measured neodymium element is greater than 0.999, which meets the requirements of the present invention.

[0086] Step 2: Prepare the neodymium standard solution, high temperature alloy standard substances and reagents:

[0087] Neodymium standard solution: content 0.02mg·mL -1 Neodymium element standard solution;

[0088] High temperature alloy standard material: The content of matrix and coexisting elements is close to that of the high temperature alloy standard sample G2 to be tested;

[0089] The reagents used were sulfuric acid: high-grade pure, ρ1.84g·ml -1 ;

[0090] Phosphoric acid: high purity, ρ is 1.69 g·ml -1 ;

[0091] Water: Secondary water;

[0092] Nitric acid: high purity, ρ is 1.42 g·ml -1 ;

[0093] Hydrochloric acid: high purity, ρ is 1.19 g·ml -1 ;

[0094] Step 3, weighing the matrix and the coexisting element content close to the high-temperature alloy standard sample G2 to be tested and the high-temperature alloy standard sample G2 to be tested and processing them into a solution to be tested;

[0095] Specifically, 0.1000g of the matrix and 6 high-temperature alloy standard samples whose coexisting element contents are close to that of the high-temperature alloy standard sample G2 to be tested and 0.100g of the standard sample G2 to be tested are weighed in a 150ml conical flask, the high-temperature alloy standard sample G2 is weighed accurately to 0.0001g, 15ml of hydrochloric acid and 2ml of nitric acid are added in sequence, and heated at 130°C until the high-temperature alloy sample is completely dissolved, 5ml of sulfuric acid and phosphoric acid mixed acid with a volume ratio of (1+2) is added to the solution, heated at 340°C to generate smoke, carbonized with 2ml of nitric acid once, and cooled; 20ml of water is added along the wall of the flask, heated and boiled until the solution is clear, and after cooling, it is fixed to volume in a 100ml volumetric flask, shaken well, and the solution to be tested is obtained;

[0096] Step 4, using the full spectrum direct reading inductively coupled plasma emission spectrometer in step 1 to establish a neodymium element working curve;

[0097] The specific process is as follows: the mass concentration of six parts of neodymium elements are 0 mg·L -1 , 0.2mg·L -1 , 0.4mg·L -1 , 0.6mg·L -1 , 0.8mg·L -1 , 1.0mg·L -1 The neodymium standard working solution was tested, that is, the neodymium standard working solution with the same matrix composition as the high-temperature alloy standard sample G2 was used to draw the working curve. The neodymium element was at a mass fraction of 1.0 mg·L -1 The range is linear, and the linear correlation coefficient is 0.9996. If it is above 0.999, proceed to the next step;

[0098] Step 5, input the sample weight of the spiked recovery rate of the high-temperature alloy standard sample G2 in step 3 and the volume of the high-temperature alloy solution to be tested, and measure the spiked recovery rate content of the neodymium element in the high-temperature alloy standard sample G2 by full-spectrum direct-reading inductively coupled plasma emission spectrometer. The results are shown in Table 3. It can be seen from Table 3 that the measured value of the standard sample is consistent with the recognized value, the spiked recovery rate is 100.6%, and the method has high accuracy;

[0099] Table 3 Analysis results of spike recovery of high temperature alloy standard sample G2 (n=4)

[0100]

[0101] Example 4

[0102] Analysis of high temperature alloy standard sample G3

[0103] Step 1, using a full spectrum direct-reading inductively coupled plasma emission spectrometer that tests the 406.109 nm neodymium element spectrum as a device for detecting the neodymium content in the high-temperature alloy standard sample G3;

[0104] The parameters set by the equipment ensure that the detection limit of the neodymium element is 0.00009%, which is better than 0.0001%. The relative standard deviation of 0.10% neodymium element measured for 10 consecutive times is 0.77%, which is less than 1.00%. The linear correlation coefficient of the working curve of the measured neodymium element is greater than 0.999, which meets the requirements of the present invention.

[0105] Step 2: Prepare the neodymium standard solution, high temperature alloy standard substances and reagents:

[0106] Neodymium standard solution: content 0.02mg·mL -1 Neodymium element standard solution;

[0107] High temperature alloy standard material: The content of matrix and coexisting elements is close to that of the high temperature alloy standard sample G3 to be tested;

[0108] The reagents used were sulfuric acid: high-grade pure, ρ1.84g·ml -1 ;

[0109] Phosphoric acid: high purity, ρ is 1.69 g·ml -1 ;

[0110] Water: Secondary water;

[0111] Nitric acid: high purity, ρ is 1.42 g·ml -1 ;

[0112] Hydrochloric acid: high purity, ρ is 1.19 g·ml -1 ;

[0113] Step 3, weighing the matrix and the coexisting element content close to the high-temperature alloy standard sample G3 to be tested and the high-temperature alloy standard sample G3 to be tested and processing them into a solution to be tested;

[0114] Specifically, 0.1000g of the matrix and 6 high-temperature alloy standard samples whose coexisting element contents are close to that of the high-temperature alloy standard sample G3 to be tested and 0.100g of the standard sample G3 to be tested are weighed in a 150ml conical flask, the high-temperature alloy standard sample G3 is weighed accurately to 0.0001g, 20ml of hydrochloric acid and 4ml of nitric acid are added in sequence, and heated at 140°C until the high-temperature alloy sample is completely dissolved, 3ml of sulfuric acid and phosphoric acid mixed acid with a volume ratio of (1+2) is added to the solution, heated at 300°C to generate smoke, carbonized with 2ml of nitric acid once, and cooled; 25ml of water is added along the wall of the flask, heated and boiled until the solution is clear, and after cooling, it is fixed to volume in a 100ml volumetric flask, shaken well, and the solution to be tested is obtained;

[0115] Step 4, using the full spectrum direct reading inductively coupled plasma emission spectrometer in step 1 to establish a neodymium element working curve;

[0116] The specific process is as follows: the mass concentration of six parts of neodymium elements are 0 mg·L -1 , 0.2mg·L -1 , 0.4mg·L -1 , 0.6mg·L -1 , 0.8mg·L -1 , 1.0mg·L -1 The neodymium standard working solution was tested, that is, the neodymium standard working solution with the same matrix composition as the high-temperature alloy standard sample G3 was used to draw the working curve. The neodymium element was at a mass fraction of 1.0 mg·L -1 The range is linear, and the linear correlation coefficient is 0.9995. If it is above 0.999, proceed to the next step;

[0117] Step 5, input the weight of the high temperature alloy standard sample G3 in step 3 and the volume of the high temperature alloy solution to be tested, and measure the content of neodymium in the high temperature alloy standard sample G3 by full spectrum direct reading inductively coupled plasma emission spectrometer. The results are shown in Table 4. It can be seen from Table 4 that the measured value of the standard sample is consistent with the recognized value, and the relative standard deviation is less than 5%. This method has high accuracy and good precision;

[0118] Table 4 Analysis results of high temperature alloy standard sample G4 (n=10)

[0119]

[0120] Example 5

[0121] Analysis of high temperature alloy sample GH4079

[0122] Step 1, using a full spectrum direct-reading inductively coupled plasma emission spectrometer that tests the 406.109 nm neodymium element spectrum as a device for detecting the content of multiple elements in the high-temperature alloy sample GH4079;

[0123] Step 2: Prepare the neodymium standard solution, high temperature alloy standard substances and reagents:

[0124] Neodymium standard solution: content 0.02mg·mL -1 Neodymium element standard solution;

[0125] High temperature alloy standard material: The content of matrix and coexisting elements is close to that of the high temperature alloy sample GH4079 to be tested;

[0126] The reagents used were sulfuric acid: high-grade pure, ρ1.84g·ml -1 ;

[0127] Phosphoric acid: high purity, ρ is 1.69 g·ml -1 ;

[0128] Water: Secondary water;

[0129] Nitric acid: high purity, ρ is 1.42 g·ml -1 ;

[0130] Hydrochloric acid: high purity, ρ is 1.19 g·ml -1 ;

[0131] Step 3, weighing a high-temperature alloy standard sample and a high-temperature alloy sample GH4079 whose contents of the matrix and coexisting elements are close to those of the high-temperature alloy sample to be tested GH4079 and treating them into a solution to be tested;

[0132] Specifically, 0.1000g of the matrix and 6 high-temperature alloy standard samples with coexisting element contents close to the high-temperature alloy sample GH4079 to be tested, 5 high-temperature alloy standard materials containing the remaining coexisting elements except neodymium, phosphorus, silicon, boron, magnesium and calcium, and 0.100g of the sample GH4079 to be tested are weighed in a 150ml conical flask, the high-temperature alloy sample GH4079 is weighed accurately to 0.0001g, 10ml of hydrochloric acid and 3ml of nitric acid are added in sequence, and heated at 100°C until the high-temperature alloy sample is completely dissolved, 3ml of sulfuric acid and phosphoric acid mixed acid with a volume ratio of (1+2) is added to the dissolved solution, heated at 330°C to emit smoke, carbonized once with 2ml of nitric acid, and cooled; 15ml of water is added along the wall of the flask, heated and boiled until the dissolved solution is clear, and after cooling, it is fixed to volume in a 100ml volumetric flask, shaken well, and the solution to be tested is obtained;

[0133] Step 4, using the full spectrum direct-reading inductively coupled plasma emission spectrometer in step 1 to establish a working curve of the neodymium element and the remaining coexisting elements except neodymium, phosphorus, silicon, boron, magnesium, and calcium;

[0134] Specifically, the mass concentrations of the six neodymium elements were 0 mg·L -1 , 0.2mg·L -1 , 0.4mg·L -1 , 0.6mg·L -1 , 0.8mg·L -1 , 1.0mg·L -1The standard working solution of GH4079 was tested with 5 high-temperature alloy standard materials of coexisting elements except neodymium, phosphorus, silicon, boron, magnesium and calcium. That is, the standard working solution of neodymium with the same matrix composition as the high-temperature alloy sample GH4079 and the 5 standard working solutions of coexisting elements except neodymium, phosphorus, silicon, boron, magnesium and calcium were used to establish the working curve. -1 The linearity is within the range, and the linear correlation coefficient is 0.99998. If it is above 0.999, except for neodymium, phosphorus, silicon, boron, magnesium, and calcium, the linear correlation coefficient of the standard working solution of other coexisting elements is above 0.999, and the next step is carried out;

[0135] Step 5, input the weight of the high-temperature alloy sample GH4079 in step 3 and the volume of the high-temperature alloy solution to be tested, and measure the content of neodymium and other coexisting elements except neodymium, phosphorus, silicon, boron, magnesium and calcium in the high-temperature alloy sample GH4079 by full-spectrum direct-reading inductively coupled plasma emission spectrometer. The accuracy and practicality of the evaluation method are shown in Tables 5 and 6. It can be seen from Table 5 that the relative standard deviation of neodymium in the high-temperature alloy sample GH4079 is less than 5%, and the method has high accuracy and good precision; the content results of other coexisting elements except neodymium, phosphorus, silicon, boron, magnesium and calcium are shown in Table 6. It can be seen from Table 6 that the present invention can also realize the accurate test of other coexisting elements except neodymium, phosphorus, silicon, boron, magnesium and calcium in the high-temperature alloy sample GH4079, and the method has high accuracy and high detection efficiency;

[0136] Table 5 Analysis results of neodymium in high temperature alloy sample GH4079 (n=10)

[0137]

[0138] Table 6 Analysis results of other coexisting elements in GH4079 except neodymium, phosphorus, silicon, boron, magnesium and calcium

[0139]

Claims

1. A method for determining neodymium in a high temperature alloy, characterized in that: The following steps are involved: S1. A full spectrum direct-reading inductively coupled plasma emission spectrometer that tests the 406.109 nm neodymium element spectrum is used as a device to detect neodymium and other elements except phosphorus, silicon, boron, magnesium and calcium in high-temperature alloys; S2. Prepare neodymium standard solution, high temperature alloy standard substances and reagents; S3, weighing a high-temperature alloy standard sample and a high-temperature alloy sample to be tested whose contents of the matrix and coexisting elements are close to those of the high-temperature alloy sample to be tested, and treating them into a solution to be tested; S4, using the spectrometer in S1 to establish working curves for neodymium and other elements except phosphorus, silicon, boron, magnesium and calcium; S5. The content of neodymium in the high-temperature alloy sample in S3 is measured by a spectrometer. If a high-temperature alloy standard material containing other coexisting elements except neodymium is added to S4, the contents of other elements except phosphorus, silicon, boron, magnesium and calcium are measured by a spectrometer.

2. The method for determining neodymium in high temperature alloy according to claim 1, characterized in that: The performance of the equipment described in S1 should ensure that the detection limit of the neodymium element must be better than 0.0001%, the relative standard deviation of 0.10% neodymium element measured for 10 consecutive times is no more than 1.00%, and the linear correlation coefficient of the working curve of the measured neodymium element is greater than 0.

999.

3. The method for determining neodymium in high temperature alloy according to claim 1, characterized in that: The high-temperature alloy standard material in S2 has a matrix and coexisting element content close to that of the high-temperature alloy sample to be tested; the content of the neodymium element standard solution is 0.02 mg·mL -1 The reagents are sulfuric acid: high-grade pure, ρ is 1.84g ml -1 ; Phosphoric acid: high purity, ρ is 1.69 g·ml -1 ; Water: secondary water; nitric acid: high purity, ρ is 1.42g·ml -1 ; Hydrochloric acid: high purity, ρ is 1.19 g·ml -1 .

4. The method for determining neodymium in high temperature alloy according to claim 1, characterized in that: The specific process of S3 is as follows: weigh 0.1000g of the matrix and 6 high-temperature alloy standard samples whose coexisting element contents are close to that of the high-temperature alloy sample to be tested, high-temperature alloy standard materials containing other elements except phosphorus, silicon, boron, magnesium and calcium, and 0.100g of the sample to be tested in a 150ml conical flask, weigh the high-temperature alloy sample accurately to 0.0001g, add 10ml-30ml of hydrochloric acid and 1ml-4ml of nitric acid in sequence, heat in the temperature range of 100℃-150℃ until the high-temperature alloy sample is completely dissolved, add 3ml-5ml of sulfuric acid and phosphoric acid mixed acid with a volume ratio of (1+2) to the dissolved solution, heat in the temperature range of 300℃-350℃ to generate smoke, decarbonize with 2ml of nitric acid once, and cool; add 15ml-30ml of water along the wall of the flask, heat and boil until the dissolved solution is clear, and after cooling, make up to the volume in a 100ml volumetric flask, shake well, and obtain the solution to be tested.

5. The method for determining neodymium in high temperature alloy according to claim 4, characterized in that: The specific process of S4 is: using the full spectrum direct reading inductively coupled plasma emission spectrometer in S1 to measure the mass concentrations of the six neodymium elements, 0 mg·L -1 , 0.2mg·L -1 , 0.4mg·L -1 , 0.6mg·L -1 , 0.8mg·L -1 , 1.0mg·L -1 The neodymium standard working solution is tested. If the neodymium element is at a mass fraction of 1.0 mg·L -1 If the linearity is within the range and the linear correlation coefficient is above 0.999, and the correlation coefficients of other elements except phosphorus, silicon, boron, magnesium and calcium are above 0.999, then a working curve is established and the next step is carried out; otherwise, S3 and S4 are repeated until the neodymium element is within the mass fraction of 1.0 mg·L -1 The range is linear, and the linear correlation coefficient is above 0.

999. Except for phosphorus, silicon, boron, magnesium and calcium, the correlation coefficients of other elements are above 0.999.

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