CN112147271A - Erbium oxide purity detection method - Google Patents
Erbium oxide purity detection method Download PDFInfo
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- CN112147271A CN112147271A CN202011059344.1A CN202011059344A CN112147271A CN 112147271 A CN112147271 A CN 112147271A CN 202011059344 A CN202011059344 A CN 202011059344A CN 112147271 A CN112147271 A CN 112147271A
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Abstract
The invention discloses an erbium oxide purity detection method, which comprises the following steps: s1, taking erbium oxide to be measured, and recording the mass of the erbium oxide to be measured as m0Adding hydrochloric acid solution into erbium oxide to be detected, heating and dissolving to obtain test solution, and recording volume of the test solution as V1(ii) a S2, dividing and taking a proper amount of test solution to obtain divided test solution, and recording the volume of the divided test solution as V2Adding ascorbic acid and sulfosalicylic acid solution; s3, using methyl orange as an indicator, adjusting the solution to be just yellow by ammonia water and hydrochloric acid, and then adding hexamethylenetetramine buffer solution; s4, taking xylenol orange as an indicator, taking EDTA standard titration solution, recording the concentration of the EDTA standard titration solution as c, carrying out complexometric titration until the solution is changed from red to yellow, and recording the volume of the consumed EDTA standard titration solution as V; and S5, calculating the mass percent content of the erbium oxide. The advantages are that: the detection accuracy of the high-purity (more than 99.5 percent) erbium oxide is high, and the detection method is simple and convenient.
Description
Technical Field
The invention relates to a compound purity detection method, in particular to an erbium oxide purity detection method.
Background
The nanometer erbium oxide is used as raw material for preparing various high-performance materials, such as fluorescent materials, biological activating enzyme, optical fiber, sensitive elements and the like. The performance of the materials is closely related to the purity of erbium oxide, and the higher the purity is, the better the performance of the materials is.
At present, analyzers such as ICP-AES and ICP-MS are adopted for detecting the purity of erbium oxide, but experiments find that the method is not suitable for detecting the purity of high-purity (more than 99.5%) erbium oxide, and the reason is that the purity is high, and multi-step dilution is needed, so that the detection error is large. And the operation steps are too many, and the operation is too complicated and complicated.
Disclosure of Invention
In order to improve the accuracy of the purity detection of the high-purity erbium oxide and simplify the detection operation, the invention provides the erbium oxide purity detection method.
The technical scheme adopted by the invention is as follows: the erbium oxide purity detection method comprises the following steps:
s1, taking erbium oxide to be measured, and recording the mass of the erbium oxide to be measured as m0Adding hydrochloric acid solution into erbium oxide to be detected, heating to completely dissolve erbium oxide to obtain test solution, and recording the volume of the test solution as V1；
S2, dividing and taking a proper amount of test solution to obtain divided test solution, and recording the volume of the divided test solution as V2Adding ascorbic acid into the separated sample solution, and adding sulfosalicylic acid solution;
s3, using methyl orange as an indicator, adjusting the solution to be just yellow by ammonia water and hydrochloric acid, and then adding hexamethylenetetramine buffer solution;
s4, taking xylenol orange as an indicator, taking EDTA standard titration solution, recording the concentration of the EDTA standard titration solution as c, carrying out complexometric titration until the solution is changed from red to yellow, and recording the volume of the consumed EDTA standard titration solution as V;
s5, calculating the mass percent content of the erbium oxide according to the following formula:
in the formula: m- -the molar mass of erbium oxide, g/mol;
c- -concentration of EDTA standard titration solution, mol/L;
v- -consumes the volume of EDTA standard titrant, mL;
V1a- -test solutionVolume, mL;
V2-dividing the volume of the sample solution, mL;
m0-mass of erbium oxide, g.
As a further improvement of the present invention, the steps S1, S2, and S3 are specifically:
s1: taking 0.6g of erbium oxide to be measured, and recording the mass as m0Adding 10mL of hydrochloric acid solution 1+1 into erbium oxide to be detected, heating to 70-80 ℃ to completely dissolve the erbium oxide, cooling to room temperature to obtain a test solution, and recording the volume of the test solution as V1；
S2: dividing 10mL of test solution to obtain divided test solution, and recording the volume of the divided test solution as V2Adding 50mL of water and 0.2g of ascorbic acid into the separated sample solution, and adding 2mL of sulfosalicylic acid solution with the concentration of 100 g/L;
s3, using methyl orange as indicator, adjusting the solution to turn yellow with ammonia and hydrochloric acid, and then adding 5mL hexamethylenetetramine buffer solution.
As a further improvement of the invention, the buffer solution of hexamethylene tetramine is prepared according to the following method: weighing a certain amount of hexamethylenetetramine in a container, adding 100mL of water into every 100g of hexamethylenetetramine for dissolution, then adding 1+1 hydrochloric acid solution into every 100g of hexamethylenetetramine and 35mL of hydrochloric acid, and adding water into every 100g of hexamethylenetetramine for dilution to 500mL for dilution to a target volume.
The invention has the beneficial effects that: the detection accuracy of the high-purity (more than 99.5 percent) erbium oxide is high, and the detection method is simple and convenient.
Detailed Description
The present invention will be further described with reference to the following examples.
The first embodiment is as follows:
the purity of the erbium oxide sample is detected according to the following method:
firstly, a detection device:
burette, erlenmeyer flask, beaker, electric furnace, analytical balance, volumetric flask, pipette, muffle furnace, oven, platinum crucible.
II, detection reagent:
ascorbic acid, ammonia water 1+1, hydrochloric acid solution 1+1, sulfosalicylic acid solution (100g/L), xylenol orange (2g/L), methyl orange (2g/L), hexamethylenetetramine buffer solution (pH 5.5) and EDTA standard solution (0.03 mol/L).
The hexamethylene tetramine buffer solution is prepared according to the following method: 200 plus or minus 0.1g of hexamethylenetetramine is weighed into a 500mL beaker, dissolved in 200mL of water, added with 70mL of hydrochloric acid solution 1+1 and diluted to 1L by water.
The EDTA solution to be marked is prepared according to the following method: weighing 11.2 +/-0.001 g of EDTA in a 1000mL beaker, heating to dissolve, cooling, and roughly preparing 0.03mol/L EDTA solution to be labeled.
Thirdly, calculating the concentration of the EDTA standard titration solution:
weighing 2 +/-0.001 g of standard reagent zinc oxide which is burnt to constant weight in a muffle furnace at 850 ℃, wetting the zinc oxide by using a small amount of water, adding 20.00mL of hydrochloric acid solution 1+1 for dissolution, transferring the zinc oxide into a 500mL volumetric flask, and fixing the volume. Transfer 25.00mL of this sample into an Erlenmeyer flask, adjust the pH to 7.7 with 1+1 ammonia, add 10.00mL ammonia-ammonium chloride buffer (pH 10) and 5 drops of chrome Black T indicator, titrate with prepared EDTA until the solution changes from purple to pure blue. Meanwhile, a blank test is carried out, and the concentration of the EDTA is calculated. The EDTA concentration was calculated as follows:
in the formula: m-zinc oxide mass in units of (g),
v1- -the volume of the zinc oxide solution removed in mL (mL),
v2- -the volume of EDTA standard liquid consumed in mL (mL),
v3- -blank consumption of EDTA standard volume in mL (mL),
m- -Zinc oxide molar mass in grams per mole (g/moL)
[M(ZnO)＝81.39]。
Fourthly, detecting the purity of the erbium oxide sample:
weighing 0.6 ±)A0.001 g sample of erbium oxide (known to have a purity of 99.6%) was recorded as m by mass0Adding 10.00mL of hydrochloric acid solution 1+1 into a 100mL beaker, covering a watch glass, heating to 80 ℃ to completely dissolve, cooling to room temperature to obtain a test solution, and recording the volume of the test solution as V1. The sample solution was transferred to a 100mL volumetric flask and mixed well.
10.00mL of the sample solution was removed and the volume was recorded as V2In a 250mL Erlenmeyer flask, 50.00mL of water, 0.20g of ascorbic acid, and 2.00mL of sulfosalicylic acid (100g/L) were added.
Adding 1 drop of methyl orange, adjusting the solution to turn yellow by ammonia water and hydrochloric acid, adding 5.00mL of hexamethylenetetramine buffer solution,
2 drops of xylenol orange are added and titrated with the above calibrated EDTA until the solution turns from red to yellow as the end point.
The erbium oxide main content was calculated by the following formula, and expressed in mass fraction (%):
in the formula: m- -the molar mass of erbium oxide, g/mol;
c- -concentration of EDTA standard titration solution, mol/L;
v- -consumes the volume of EDTA standard titrant, mL;
V1-total volume of sample, mL;
V2-dividing the volume of the sample solution, mL;
m0-mass of erbium oxide, g.
The results are shown in Table 1.
Example two:
the assay was repeated exactly as in example one and the results are shown in Table 1.
Example three:
the assay was repeated exactly as in example one and the results are shown in Table 1.
Example four:
the assay was repeated exactly as in example one and the results are shown in Table 1.
Example five:
the assay was repeated exactly as in example one and the results are shown in Table 1.
Comparative example one:
the ICP method is adopted to detect the same sample, and the specific detection method is as follows:
(1) weighing 0.1000g of erbium oxide burnt at 9000 ℃ for 1h, placing the erbium oxide in a 100mL beaker, adding 10.00mL of hydrochloric acid solution 1+1, covering a watch glass, heating to 80 ℃ to completely dissolve the erbium oxide, cooling to room temperature, transferring the solution into a 100mL volumetric flask, diluting to a scale, mixing uniformly, and diluting into 1.00mL of standard solutions containing 100 micrograms, 50 micrograms and 10 micrograms respectively.
(2) Weighing 0.6 +/-0.001 g of erbium oxide sample into a 100mL beaker, adding 10.00mL of hydrochloric acid solution 1+1, covering a watch glass, heating to 80 ℃ to completely dissolve the erbium oxide sample, cooling to room temperature, transferring the solution into a 100mL volumetric flask, diluting to a scale, and uniformly mixing. Transferring 1.00mL of the solution into a 100mL volumetric flask, diluting to the mark, and mixing uniformly.
(3) The purity of erbium oxide was tested using ICP.
The results are shown in Table 1.
Table 1: purity detection result of sample erbium oxide
As can be seen from table 1, the RSD of the erbium oxide content detection result is less than 5% after the method of this embodiment is tested for 5 times, which indicates that the method can accurately measure the erbium oxide content.
In addition, as can be seen from table 1, the measurement result of ICP is significantly large, and the result error is large due to high purity and multi-step dilution, so that in the detection of high-purity erbium oxide (purity > 99.5%), the method of the present invention has higher accuracy than the ICP method, and has higher detection accuracy.
Claims (3)
1. The erbium oxide purity detection method comprises the following steps:
s1, taking erbium oxide to be measured, and recording the mass of the erbium oxide to be measured as m0Adding hydrochloric acid solution into erbium oxide to be detected, heating to completely dissolve erbium oxide to obtain test solution, and recording the volume of the test solution as V1；
S2, dividing and taking a proper amount of test solution to obtain divided test solution, and recording the volume of the divided test solution as V2Adding ascorbic acid into the separated sample solution, and adding sulfosalicylic acid solution;
s3, using methyl orange as an indicator, adjusting the solution to be just yellow by ammonia water and hydrochloric acid, and then adding hexamethylenetetramine buffer solution;
s4, taking xylenol orange as an indicator, taking EDTA standard titration solution, recording the concentration of the EDTA standard titration solution as c, carrying out complexometric titration until the solution is changed from red to yellow, and recording the volume of the consumed EDTA standard titration solution as V;
s5, calculating the mass percent content of the erbium oxide according to the following formula:
in the formula: m- -the molar mass of erbium oxide, g/mol;
c- -concentration of EDTA standard titration solution, mol/L;
v- -consumes the volume of EDTA standard titrant, mL;
V1-total volume of sample, mL;
V2-dividing the volume of the sample solution, mL;
m0-mass of erbium oxide, g.
2. An erbium oxide purity detection method according to claim 1, characterized in that: the steps S1, S2, and S3 are specifically:
s1: taking 0.6g of erbium oxide to be measured, and recording the mass as m0Then adding 10 into the erbium oxide to be testedmL hydrochloric acid solution 1+1, heating to 70-80 ℃ to completely dissolve erbium oxide, cooling to room temperature to obtain a test solution, and recording the volume of the test solution as V1；
S2: dividing 10mL of test solution to obtain divided test solution, and recording the volume of the divided test solution as V2Adding 50mL of water and 0.2g of ascorbic acid into the separated sample solution, and adding 2mL of sulfosalicylic acid solution with the concentration of 100 g/L;
s3, using methyl orange as indicator, adjusting the solution to turn yellow with ammonia and hydrochloric acid, and then adding 5mL hexamethylenetetramine buffer solution.
3. An erbium oxide purity detection method according to any one of claims 1 or 2, wherein: the buffer solution of hexamethylene tetramine is prepared according to the following method: weighing a certain amount of hexamethylenetetramine in a container, adding 100mL of water into every 100g of hexamethylenetetramine for dissolution, then adding 1+1 hydrochloric acid solution into every 100g of hexamethylenetetramine and 35mL of hydrochloric acid, and adding water into every 100g of hexamethylenetetramine for dilution to 500mL for dilution to a target volume.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104749318A (en) * | 2013-12-30 | 2015-07-01 | 北京有色金属与稀土应用研究所 | Method for volumetric method determination of zinc content in silver copper zinc cadmium nickel solder |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104749318A (en) * | 2013-12-30 | 2015-07-01 | 北京有色金属与稀土应用研究所 | Method for volumetric method determination of zinc content in silver copper zinc cadmium nickel solder |
Non-Patent Citations (2)
| Title |
|---|
| 郝茜 等: "《实用稀土冶金分析》", 31 May 2018, 冶金工业出版社 * |
| 龙旭东等: "EDTA滴定法测定稀土铝中间合金中稀土总量", 《冶金分析》 * |
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