CN112834488A - Method for determining contents of lanthanum, cerium, praseodymium, neodymium, samarium, calcium and magnesium in iron ore - Google Patents
Method for determining contents of lanthanum, cerium, praseodymium, neodymium, samarium, calcium and magnesium in iron ore Download PDFInfo
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
Abstract
The invention discloses a method for measuring the contents of lanthanum, cerium, praseodymium, neodymium, samarium, calcium and magnesium in iron ore, which comprises the steps of melting and decomposing a sample by using sodium hydroxide-sodium peroxide, leaching with water, acidifying with hydrochloric acid, separating calcium and magnesium elements by using ammonia water, fixing the volume of filtered filtrate, and measuring the contents of the calcium and magnesium elements by using an ICP-AES method; the filtered precipitate is dissolved by hydrochloric acid to be constant volume, and then the content of the lanthanum, cerium, praseodymium, neodymium and samarium elements is determined by adopting an ICP-AES method, so that the content of the lanthanum, cerium, praseodymium, neodymium, samarium, calcium and magnesium elements in iron ore can be determined by decomposing a sample once.
Description
Technical Field
The invention belongs to the technical field of metallurgical analysis, and particularly relates to a method for measuring the contents of lanthanum, cerium, praseodymium, neodymium, samarium, calcium and magnesium in iron ore.
Background
At present, the content of calcium and magnesium in iron ore is measured according to a national standard method GB/T6730.13-2007, and the principle is as follows: decomposing the sample with hydrochloric acid and nitric acid, and filtering; after removing silicon from the residue with hydrofluoric acid (except for the fluorine-containing sample), potassium pyrosulfate was melted. Filtering and removing iron, aluminum, titanium, manganese and the like by using ammonia water and potassium hydroxide, adding a calcium indicator when the pH value is more than 12, and titrating calcium by using EGTA standard titration solution. At pH 10, calcium was complexed with EGTA followed by addition of a chromium black T indicator and magnesium was titrated with CyDTA standard titration solution. The national standard method has long analysis process, more reagents are used, and the lower limit of the determination is Ca: 1.5%, Mg: 1.0 percent. The determination of the contents of lanthanum, cerium, praseodymium, neodymium and samarium in the iron ore has no national standard or standard method. Document CN108760722A discloses a method for measuring the intensity of lanthanum, cerium, praseodymium, neodymium and samarium elements in a test solution and a calibration curve solution simultaneously by using hydrofluoric acid, hydrochloric acid and perchloric acid to decompose a sample under heating, and a computer automatically calculates the content of rare earth pentabasic elements. However, the method of the document cannot simultaneously determine the contents of calcium and magnesium in the iron ore.
Disclosure of Invention
Aiming at one or more problems in the prior art, the invention provides a method for measuring the content of lanthanum, cerium, praseodymium, neodymium, samarium, calcium and magnesium in iron ore, which comprises the following steps:
1) weighing a sample, placing the sample in a nickel crucible containing sodium hydroxide, covering the sample with sodium peroxide, placing the nickel crucible in a muffle furnace to be melted until tassel red, keeping for 7-10 minutes, taking out and cooling slightly;
2) placing the nickel crucible which is slightly cooled in the step 1) in hot water, heating and leaching, washing with water, and taking out the crucible and a crucible cover to obtain a leaching test solution;
3) adding concentrated hydrochloric acid into a leaching test solution, heating for dissolving, neutralizing with first ammonia water to generate a large amount of precipitates, adding second ammonia water until the pH value is 9.5-10.5, dropwise adding hydrogen peroxide, heating for boiling, standing for precipitating, filtering to obtain a first filtrate and a first precipitate, washing the first precipitate with hot ammonium chloride solution, filtering to obtain a second filtrate and a second precipitate, and mixing the first filtrate and the second filtrate to obtain a solution to be detected for the contents of calcium and magnesium elements;
4) dissolving the second precipitate with hot hydrochloric acid, and heating to dissolve the second precipitate to obtain a solution to be detected, wherein the solution is used as a solution to be detected for the contents of lanthanum, cerium, praseodymium, neodymium and samarium;
5) and determining the contents of calcium and magnesium elements in the liquid to be determined of the contents of calcium and magnesium elements by adopting an ICP-AES method, and determining the contents of lanthanum, cerium, praseodymium, neodymium and samarium elements in the liquid to be determined of the contents of lanthanum, cerium, praseodymium, neodymium and samarium elements.
In the method, the temperature in the muffle furnace in the step 1) is 740-760 ℃.
In the method, the concentration of the first ammonia water in the step 3) is 25% -28%, and the second ammonia water is obtained by mixing strong ammonia water and water according to the volume ratio of 1: 1.
In the method, the hot hydrochloric acid in the step 4) is hydrochloric acid obtained by mixing concentrated hydrochloric acid and water according to the volume ratio of 1: 1.
The method comprises the following steps:
a) weighing 0.2000g of iron ore sample, placing the iron ore sample in a nickel crucible which is pre-filled with 2g of sodium hydroxide with water removed, covering 2g of sodium peroxide, heating the iron crucible on an electric furnace to remove water, shaking the nickel crucible to disperse the sample, placing the nickel crucible in a muffle furnace at 750 ℃ to melt until the sample is red, keeping the molten sample for 7-10 minutes, taking out the sample and cooling the sample slightly;
b) placing the nickel crucible into a 400mL beaker containing about 100mL of hot water, heating and leaching, washing with water, and taking out the crucible and a crucible cover to obtain a leaching test solution;
c) adding 20mL of concentrated hydrochloric acid into a leaching test solution, heating for dissolving, neutralizing with first ammonia water to generate a large amount of precipitate, adding 10mL of second ammonia water until the pH value is 10, dropwise adding 1mL of 30% hydrogen peroxide, heating for boiling for 5 minutes, taking down, standing for a moment, allowing the precipitate to sink, filtering while hot to obtain a first filtrate and a first precipitate, washing a beaker with hot 20g/L ammonium chloride for 3-4 times, washing the first precipitate for 7-8 times, filtering to obtain a second filtrate and a second precipitate, and mixing the first filtrate and the second filtrate to obtain a solution to be tested, wherein the content of calcium and magnesium elements is determined;
d) dissolving the second precipitate with hot hydrochloric acid, and heating to dissolve the second precipitate to obtain a solution to be detected, wherein the solution is used as a solution to be detected for the contents of lanthanum, cerium, praseodymium, neodymium and samarium;
e) and determining the contents of calcium and magnesium elements in the liquid to be determined of the contents of calcium and magnesium elements by adopting an ICP-AES method, and determining the contents of lanthanum, cerium, praseodymium, neodymium and samarium elements in the liquid to be determined of the contents of lanthanum, cerium, praseodymium, neodymium and samarium elements.
According to the method for measuring the contents of lanthanum, cerium, praseodymium, neodymium, samarium, calcium and magnesium in the iron ore, which is provided based on the technical scheme, the sample is decomposed by melting sodium hydroxide-sodium peroxide, water is leached out, hydrochloric acid is used for acidification, calcium and magnesium elements are separated by ammonia water, the volume of filtrate is determined, and the content of the calcium and magnesium elements is measured by an ICP-AES method; the content of the lanthanum, cerium, praseodymium, neodymium and samarium elements in the iron ore can be measured by using an ICP-AES method after the precipitation is dissolved by hydrochloric acid to a constant volume, so that the content of the lanthanum, cerium, praseodymium, neodymium, samarium, calcium and magnesium elements in the iron ore can be measured by decomposing a sample once. The following table 1 shows the measurement ranges of the contents of seven elements, i.e., lanthanum, cerium, praseodymium, neodymium, samarium, calcium and magnesium.
Table 1: elements and measurement ranges
Detailed Description
The invention aims to provide a method for determining the content of seven elements of lanthanum, cerium, praseodymium, neodymium, samarium, calcium and magnesium in iron ore by decomposing a sample once, which mainly comprises the following technical scheme: weighing an iron ore sample, placing the iron ore sample in a nickel crucible, melting with sodium hydroxide and sodium peroxide, extracting with water, acidifying with hydrochloric acid, and separating rare earth, calcium, magnesium and other elements with ammonia water. And (3) determining the content of calcium and magnesium elements by adopting an ICP-AES (inductively coupled plasma-atomic emission spectrometry) method for filtrate constant volume, and determining the content of lanthanum, cerium, praseodymium, neodymium and samarium elements by adopting the ICP-AES method after the precipitate is dissolved by hydrochloric acid for constant volume.
The present invention will be described in detail with reference to specific examples.
In the following, only certain exemplary embodiments are briefly described. As those skilled in the art will recognize, the described embodiments may be modified in various different ways, all without departing from the spirit or scope of the present invention. Accordingly, the following description is to be regarded as illustrative in nature and not as restrictive.
The various biological materials described in the examples are obtained by way of experimental acquisition for the purposes of this disclosure only and should not be limiting as to the source of the biological material of the present invention. In fact, the sources of the biological materials used are wide and any biological material that can be obtained without violating the law and ethics can be used instead as suggested in the examples.
The reagents, instruments (parameters) and analytical procedures used in the examples are as follows:
unless otherwise indicated, only reagent of superior purity and secondary pure water were used in the analysis.
2.1 hydrochloric acid,. rho.1.19 g/ml.
2.2 hydrochloric acid, 1+1, namely concentrated hydrochloric acid and water according to the volume ratio of 1: 1.
2.3 nitric acid,. rho.1.42 g/ml.
2.4 sodium hydroxide, solid.
2.5 sodium peroxide, solid.
2.6 percent of ammonia water, 25 to 28 percent.
2.7 ammonia water, 1+1, namely the mixture of concentrated ammonia water and water according to the volume ratio of 1: 1.
2.8% of hydrogen peroxide, 30%.
2.9 lanthanum oxide, spectrally pure.
2.10 cerium oxide, spectrally pure.
2.11 praseodymium oxide, spectrally pure.
2.12 samarium oxide, spectrally pure.
2.13 Neodymium oxide, spectrally pure.
2.14 g/L ammonium chloride (adjusted to pH 10 with aqueous ammonia).
2.15 Standard solution
2.15.1 La2O3Standard solution, 1000. mu.g/mL.
1.0000g lanthanum oxide (2.9) is weighed out accurately, 50ml hydrochloric acid (2.2) is added, after heating and dissolution, the solution is diluted to 1000ml with water and shaken up.
2.15.2 CeO2Standard solution, 1000. mu.g/mL.
The cerium dioxide (2.10) is burned at 750 ℃ for 30min and then placed in a dryer to be cooled to room temperature. Weighing 1.0000g of the total weight of the mixture, placing the mixture in a beaker, adding 15ml of nitric acid (2.3) and 2ml of hydrogen peroxide (2.8), heating to dissolve the mixture, boiling to decompose excessive hydrogen peroxide, cooling to room temperature, transferring the mixture into a 1000ml volumetric flask, diluting the mixture to a scale with water, and shaking up.
2.15.3 Pr6O11Standard solution, 1000. mu.g/mL.
1.0000g of praseodymium oxide (2.11) is accurately weighed, 50ml of hydrochloric acid (2.2) is added, after heating and dissolving, the solution is diluted to 1000ml by water and shaken up.
2.15.4 Nd2O3Standard solution, 1000. mu.g/mL.
1.0000g of neodymium oxide (2.12) is weighed out accurately, 50ml of hydrochloric acid (2.2) is added, after heating and dissolution, the mixture is diluted to 1000ml with water and shaken up.
2.15.5 Sm2O3Standard solution, 1000. mu.g/mL.
1.0000g of samarium sesquioxide (2.13) is weighed out accurately, 50ml of hydrochloric acid (2.2) is added, after heating and dissolution, the solution is diluted to 1000ml with water and shaken up.
2.15.6 La2O3、CeO2、Pr6O11、Nd2O3、Sm2O3Mixing of standard solutions
2.15.6.1 La2O3、CeO2、Pr6O11、Nd2O3、Sm2O3Standard solution was mixed, 100. mu.g/mL (medium 10% HCl).
Respectively taking La2O3(2.15.1)、CeO2(2.15.2)、Pr6O11(2.15.3)、Nd2O3(2.15.4)、Sm2O3(2.15.5) 10.00mL of the standard solution was put in a 100mL volumetric flask, and 10mL of hydrochloric acid (2.2) was added thereto and diluted to the mark with water, followed by mixing.
2.15.6.2 La2O3、CeO2、Pr6O11、Nd2O3、Sm2O3Standard solution was mixed, 10. mu.g/mL (medium 10% HCl).
Moving La2O3、CeO2、Pr6O11、Nd2O3、Sm2O3Mix standard solution (2.15.6.1)10.00mL into 100mL volumetric flask, add 10mL hydrochloric acid (2.2) and dilute to the mark with water, mix well.
2.16 Mg Standard solution, 1000. mu.g/mL (Medium 5% HCl), national Standard solution.
2.16.1 Mg Standard solution, 100. mu.g/mL (medium 5% HCl).
10.00mL of Ca standard solution (2.16) is transferred into a 100mL volumetric flask, 10mL of hydrochloric acid (2.2) is added and diluted to the mark with water, and the mixture is mixed evenly.
2.17 Ca Standard solution, 1000. mu.g/mL (Medium 5% HCl), national Standard solution.
2.17.1 Ca standard solution, 100. mu.g/mL (medium 5% HCl).
10.00mL of Ca standard solution (2.17) is transferred into a 100mL volumetric flask, 10mL of hydrochloric acid (2.2) is added and diluted to the mark with water, and the mixture is mixed evenly.
2.18 iron oxide, Fe2O3>99.99％。
2.19 hydrochloric acid, 1+95, i.e. concentrated hydrochloric acid and water, in a volume ratio of 1: 95.
3 Main instruments and test conditions
3.1 Optima7300V inductively coupled plasma spectrometer, manufactured by PE corporation, USA.
3.2 working parameters of the instrument: see table 2.
Table 2: operating parameters of the instrument
4 analytical step
4.1 sample decomposition
Weighing 0.2000g of iron ore sample, placing the iron ore sample in a nickel crucible (2 g of sodium hydroxide (2.4) with water removed in advance), covering 2g of sodium peroxide (2.5), heating the iron crucible on an electric furnace to remove water, shaking the crucible to disperse the sample, placing the iron ore sample in a muffle furnace at 750 ℃ to melt until the sample is red, keeping the sample for 7-10 minutes (taking out the iron ore sample, shaking the iron ore sample once), and taking out the iron ore sample for cooling. The crucible was placed in a 400mL beaker containing about 100mL of hot water, heat leached, rinsed with water and the crucible and crucible lid were removed. Then, 20mL of hydrochloric acid (2.1) was added thereto and the mixture was heated to dissolve it. Neutralizing with ammonia water (2.6) to generate a large amount of precipitate, adding 10mL of ammonia water (2.7) (the pH value is about 10 at the moment), dropwise adding 1mL of hydrogen peroxide (2.8), heating and boiling for 5 minutes, taking down and placing for a moment to enable the precipitate to sink, filtering in a 250mL volumetric flask with quick qualitative filter paper while hot, washing a beaker with hot ammonium chloride (2.14) for 3-4 times, washing the precipitate for 7-8 times, and diluting the filtrate to a scale with water after cooling. And (5) measuring the content of calcium and magnesium elements.
Dissolving the precipitate on a funnel by using hot hydrochloric acid (2.2) in a primary beaker, washing filter paper by using hot hydrochloric acid (2.19) until the filter paper is yellow, and washing the filter paper by using hot water for 3-4 times. The solution is heated to be clear, cooled to room temperature, transferred to a 250mL volumetric flask, diluted to the mark with water and mixed evenly. And (5) measuring the content of the rare earth five-element.
4.2 blank test and validation test
Each time operating according to 4.1, a standard sample of the same type of ore and a blank should be analyzed in parallel with the sample under the same conditions. The blank should use the same amount of iron oxide (2.18) instead of the sample.
Preparation of 4.3 series calibration solutions
To meet the similar requirements between the test sample and the calibration solutions, each calibration solution followed the procedure recommended in 4.1, replacing the test sample with an amount of iron equivalent to that in the test sample. The standard solution, flux and acid required for the calibration solution concentration must be added before final dilution to 250 mL. The iron content of the iron ore is generally 50% -70%, and 0.172g of iron oxide (2.18) can be used instead of the sample (corresponding to 60% of iron in the sample). A set of rare earth five-element calibration solution and a set of calcium and magnesium calibration solution are prepared according to the addition amount of the standard solution given in Table 3.
Table 3: calibration solution-standard solution addition volume
Table 3 illustrates: the content of the elements of the standard solution
4.4 determination
Adjusting the instrument conditions according to a working parameter table 2, selecting La 408.672nm, Ce 418.660nm, Pr 422.293nm, Nd 406.109nm, Sm 359.260nm, or 442.434nm, Ca 317.933nm and Mg 285.213nm as analysis lines, introducing the calibration solution, blank, sample and standard verification sample solution of 4.3, 4.2 and 4.1 into an inductively coupled plasma emission spectrometer to measure the signal intensity of the element to be measured, drawing a calibration solution working curve by taking the signal intensity of the element to be measured as a vertical coordinate and the ion mass percent as a horizontal coordinate, and calculating the mass percent of the element to be measured according to the known mass percent calibration curve.
4.5 calculation of results
4.5.1 the content of each element is calculated according to the formula: w (measured component) (%) ═ Wi-W0
In the formula: w is the mass percentage of the element in the sample; wi is the mass percentage of the element in the sample to be measured; w0 is the mass percentage of element in the blank solution to be measured.
4.5.2 conversion factor of oxide
The conversion factors of the element concentration and the oxide concentration are shown in table 4.
Table 4: conversion of element content to oxide content factor
5 precision
After the sample decomposition treatment is carried out according to the 4 analysis steps, precision experiments (n is 10) are respectively carried out on the baotite R-717, the baotite R-715 and the baotite concentrate B-K-2 which are three standard substances, and the measurement results are shown in tables 5, 6 and 7.
Table 5: precision test of Baotou Ore (R-717)
Table 6: precision test of Baotou Ore (R-715)
Table 7: precision experiment of Baotou concentrate (B-K-2)
As can be seen from the experimental data in tables 5, 6 and 7, the relative standard deviation of the precision experimental data of seven elements of the three standard substances is less than 5%, which shows that the method has higher precision.
6 accuracy test
And (4) carrying out sample treatment according to the analysis steps of 4, and respectively carrying out accuracy experiments on four standard substances, namely baotite R-717, baotite R-715, baotite concentrate B-K-1 and baotite concentrate B-K-2. Because the reference value given by the standard sample is the sum of the contents of all the rare earth elements and more than 98% of the rare earth elements in the baotite are all light rare earth elements, the experiment also compares the contents of the rare earth elements measured by all the samples. And the standard substance baotite R-717 is sent to a rare earth institute for analysis and comparison. And performing a labeling recovery experiment on the Baotou concentrate B-K-2. The measurement results are shown in tables 8 and 9.
As can be seen from the data in Table 8, the difference between the measurement results of the method and the reference values given for the standard substances is small; as can be seen from the data in Table 9, the measured values of the elements of the rare earth in the baotite R-717 are consistent with the measured value results of the rare earth institute, and the total amount of the rare earth is consistent with the standard value; the standard recovery rate of the baotou concentrate B-K-2 is 98-102%, and the three aspects prove that the method has higher accuracy and can accurately determine the content of each rare earth element in the sample.
Table 8: accuracy experiment
Table 9: accuracy experiment
7 conclusion
The relative standard deviation of the precision experimental data of seven elements of three standard substances is less than 5 percent through the precision experiment, which shows that the method has higher precision. The result of the accuracy experiment is that: the calcium and magnesium measurement result of the method is consistent with the difference value of the reference value given by the standard substance by comparison; the measured values of all elements of the rare earth in the standard substance are consistent with the measured value results of the rare earth hospital, and the total amount of the rare earth is consistent with a given reference value; the recovery rate of the added standard is 98-102%. The three aspects prove that the method has higher accuracy and can accurately determine the content of each rare earth element in the sample.
8 tolerance difference
The repeatability and reproducibility limits of the elements in the iron ore are shown in Table 10.
Table 10: the repeatability and reproducibility limits of the elements in iron ore
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. A method for measuring the contents of lanthanum, cerium, praseodymium, neodymium, samarium, calcium and magnesium in iron ore comprises the following steps:
1) weighing a sample, placing the sample in a nickel crucible containing sodium hydroxide, covering the sample with sodium peroxide, placing the nickel crucible in a muffle furnace to be melted until tassel red, keeping for 7-10 minutes, taking out and cooling slightly;
2) placing the nickel crucible which is slightly cooled in the step 1) in hot water, heating and leaching, washing with water, and taking out the crucible and a crucible cover to obtain a leaching test solution;
3) adding concentrated hydrochloric acid into a leaching test solution, heating for dissolving, neutralizing with first ammonia water to generate a large amount of precipitates, adding second ammonia water until the pH value is 9.5-10.5, dropwise adding hydrogen peroxide, heating for boiling, standing for precipitating, filtering to obtain a first filtrate and a first precipitate, washing the first precipitate with hot ammonium chloride solution, filtering to obtain a second filtrate and a second precipitate, and mixing the first filtrate and the second filtrate to obtain a solution to be detected for the contents of calcium and magnesium elements;
4) dissolving the second precipitate with hot hydrochloric acid, and heating to dissolve the second precipitate to obtain a solution to be detected, wherein the solution is used as a solution to be detected for the contents of lanthanum, cerium, praseodymium, neodymium and samarium;
5) and determining the contents of calcium and magnesium elements in the liquid to be determined of the contents of calcium and magnesium elements by adopting an ICP-AES method, and determining the contents of lanthanum, cerium, praseodymium, neodymium and samarium elements in the liquid to be determined of the contents of lanthanum, cerium, praseodymium, neodymium and samarium elements.
2. The method for determining the contents of lanthanum, cerium, praseodymium, neodymium, samarium, calcium and magnesium in iron ore according to claim 1, wherein the temperature in the muffle furnace in step 1) is 740-760 ℃.
3. The method for determining the content of lanthanum, cerium, praseodymium, neodymium, samarium, calcium and magnesium in iron ore according to claim 1 or 2, wherein the concentration of the first ammonia water in the step 3) is 25-28%, and the second ammonia water is obtained by mixing concentrated ammonia water and water according to the volume ratio of 1: 1.
4. The method for determining the content of lanthanum, cerium, praseodymium, neodymium, samarium, calcium and magnesium in iron ore according to any one of claims 1 to 3, wherein the hot hydrochloric acid in the step 4) is hydrochloric acid obtained by mixing concentrated hydrochloric acid and water according to a volume ratio of 1: 1.
5. The method for determining the contents of lanthanum, cerium, praseodymium, neodymium, samarium, calcium and magnesium in iron ore according to any one of claims 1 to 4, which comprises the steps of:
a) weighing 0.2000g of iron ore sample, placing the iron ore sample in a nickel crucible which is pre-filled with 2g of sodium hydroxide with water removed, covering 2g of sodium peroxide, heating the iron crucible on an electric furnace to remove water, shaking the nickel crucible to disperse the sample, placing the nickel crucible in a muffle furnace at 750 ℃ to melt until the sample is red, keeping the molten sample for 7-10 minutes, taking out the sample and cooling the sample slightly;
b) placing the nickel crucible into a 400mL beaker containing about 100mL of hot water, heating and leaching, washing with water, and taking out the crucible and a crucible cover to obtain a leaching test solution;
c) adding 20mL of concentrated hydrochloric acid into a leaching test solution, heating for dissolving, neutralizing with first ammonia water to generate a large amount of precipitate, adding 10mL of second ammonia water until the pH value is 10, dropwise adding 1mL of 30% hydrogen peroxide, heating for boiling for 5 minutes, taking down, standing for a moment, allowing the precipitate to sink, filtering while hot to obtain a first filtrate and a first precipitate, washing a beaker with hot 20g/L ammonium chloride for 3-4 times, washing the first precipitate for 7-8 times, filtering to obtain a second filtrate and a second precipitate, and mixing the first filtrate and the second filtrate to obtain a solution to be tested for the content of calcium and magnesium elements;
d) dissolving the second precipitate with hot hydrochloric acid, and heating to dissolve the second precipitate to obtain a solution to be detected, wherein the solution is used as a solution to be detected for the contents of lanthanum, cerium, praseodymium, neodymium and samarium;
e) and determining the contents of calcium and magnesium elements in the liquid to be determined of the contents of calcium and magnesium elements by adopting an ICP-AES method, and determining the contents of lanthanum, cerium, praseodymium, neodymium and samarium elements in the liquid to be determined of the contents of lanthanum, cerium, praseodymium, neodymium and samarium elements.
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Cited By (2)
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|---|---|---|---|---|
| CN115684136A (en) * | 2022-10-28 | 2023-02-03 | 湖南稀土金属材料研究院有限责任公司 | Method for measuring content of calcium oxide in samarium oxide |
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