CN117907250A - Method for determining phosphorus in aluminum iron - Google Patents
Method for determining phosphorus in aluminum iron Download PDFInfo
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- CN117907250A CN117907250A CN202311752085.4A CN202311752085A CN117907250A CN 117907250 A CN117907250 A CN 117907250A CN 202311752085 A CN202311752085 A CN 202311752085A CN 117907250 A CN117907250 A CN 117907250A
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- phosphorus
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- acid
- nitric acid
- sodium fluoride
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 239000011574 phosphorus Substances 0.000 title claims abstract description 54
- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 26
- CYUOWZRAOZFACA-UHFFFAOYSA-N aluminum iron Chemical compound [Al].[Fe] CYUOWZRAOZFACA-UHFFFAOYSA-N 0.000 title claims abstract description 22
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 12
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 8
- 239000011734 sodium Substances 0.000 claims abstract description 8
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 8
- CUIPHAYLXWLSTL-UHFFFAOYSA-K P(=O)(=O)[Mo+3].[Cl-].[Cl-].[Cl-] Chemical compound P(=O)(=O)[Mo+3].[Cl-].[Cl-].[Cl-] CUIPHAYLXWLSTL-UHFFFAOYSA-K 0.000 claims abstract description 4
- 239000002253 acid Substances 0.000 claims abstract description 4
- 238000004737 colorimetric analysis Methods 0.000 claims abstract description 4
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 18
- 238000002835 absorbance Methods 0.000 claims description 11
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 10
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 7
- 239000001119 stannous chloride Substances 0.000 claims description 7
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 claims description 6
- 229940074439 potassium sodium tartrate Drugs 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 235000013024 sodium fluoride Nutrition 0.000 claims description 5
- 239000011775 sodium fluoride Substances 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 4
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 4
- 239000011609 ammonium molybdate Substances 0.000 claims description 4
- 229940010552 ammonium molybdate Drugs 0.000 claims description 4
- 239000011964 heteropoly acid Substances 0.000 claims description 4
- 235000011007 phosphoric acid Nutrition 0.000 claims description 4
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 239000000779 smoke Substances 0.000 claims description 3
- 235000011150 stannous chloride Nutrition 0.000 claims description 3
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 238000009835 boiling Methods 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 235000002906 tartaric acid Nutrition 0.000 claims description 2
- 239000011975 tartaric acid Substances 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 229910000640 Fe alloy Inorganic materials 0.000 abstract description 8
- 239000012086 standard solution Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 238000009628 steelmaking Methods 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical compound [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 description 2
- 235000011006 sodium potassium tartrate Nutrition 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910001021 Ferroalloy Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- KCZFLPPCFOHPNI-UHFFFAOYSA-N alumane;iron Chemical compound [AlH3].[Fe] KCZFLPPCFOHPNI-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000002372 labelling Methods 0.000 description 1
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 1
- 235000019796 monopotassium phosphate Nutrition 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
-
- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Pathology (AREA)
- General Health & Medical Sciences (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Immunology (AREA)
- General Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Plasma & Fusion (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The invention discloses a method for measuring phosphorus in aluminum iron, which comprises the steps of dissolving an aluminum iron alloy sample with mixed acid of hydrochloric acid and nitric acid, and measuring the phosphorus content in the aluminum iron alloy sample by adopting a sodium fluoride-stannous chloride-phosphomolybdenum blue colorimetric method.
Description
Technical Field
The invention belongs to the technical field of ferroalloy analysis, and particularly relates to a method for determining phosphorus in aluminum iron.
Background
The aluminium-iron alloy is a novel deoxidizer used in steelmaking production, can improve the form of inclusions in steelmaking production and reduce the content of gas elements in molten steel, and is an effective novel technology for improving the quality of steel, reducing the cost and saving aluminum. Meanwhile, practice proves that the catalyst also has the advantages of high specific gravity, strong penetrating power and the like. The main hazard of phosphorus in aluminum-iron alloy in steelmaking is that the phosphorus causes cold brittleness of steel during hot working, so that accurate determination of the phosphorus content is of great importance. However, no method for determining the phosphorus content of an aluminum-iron alloy has been reported in the prior art.
Disclosure of Invention
In order to solve the problem that the content of phosphorus in aluminum-iron alloy is not detected, the invention provides a method for determining the content of phosphorus in aluminum-iron, which adopts a sodium fluoride-stannous chloride-phosphomolybdenum blue colorimetric method to determine the content of phosphorus in aluminum-iron, and comprises the following steps:
1) Dissolving a sample by using mixed acid of hydrochloric acid and nitric acid, and oxidizing phosphorus into orthophosphoric acid by using perchloric acid fuming to obtain a first sample;
2) Adding ammonium molybdate into the first sample in a nitric acid medium to generate phosphomolybdic heteropolyacid with phosphoric acid to obtain a second sample;
3) And adding tartaric acid into the second sample to eliminate interference of silicon, adding sodium fluoride coordinated iron, reducing the phosphomolybdic heteropolyacid into phosphomolybdic blue by stannous chloride, and measuring absorbance to obtain the phosphorus amount.
In some embodiments, step 1) is dissolving the sample with aqua regia.
In some embodiments, the concentration of nitric acid medium in step 2) is 0.8 to 1.2mol/L.
In some embodiments, the method comprises the steps of:
S1) weighing 0.0500g of sample in a 150mL high beaker, adding 10mL aqua regia, heating until the sample is dissolved, adding 10mL perchloric acid (ρ1.69), and continuously heating until the perchloric acid smoke is completely emitted; adding 10mL of nitric acid (2+5) to dissolve salts, boiling, and taking down;
S2) immediately adding 5mL of ammonium molybdate-potassium sodium tartrate mixed solution, shaking for 10S, adding 35mL of sodium fluoride-stannous chloride mixed solution, shaking uniformly, measuring the absorbance by using an intelligent high-speed analyzer, and calculating the percentage content according to a phosphorus working curve.
In some embodiments, the linear relationship of the phosphorus working curve, with absorbance values on the ordinate and percent phosphorus concentration on the abscissa, is: y=1.6136x+0.0026, r 2 =0.9999.
The method for determining the phosphorus in the aluminum iron based on the technical scheme comprises the steps of dissolving an aluminum iron alloy sample with mixed acid of hydrochloric acid and nitric acid, and determining the phosphorus content in the aluminum iron alloy sample by adopting a sodium fluoride-stannous chloride-phosphomolybdenum blue colorimetric method. The embodiment uses a method of marking and recycling to prove that the method has higher accuracy and can provide accurate data for the content of phosphorus in the aluminum iron.
Drawings
FIG. 1 is a graph showing the operation of determination of phosphorus content in aluminum iron.
Detailed Description
The invention aims to provide a method for measuring the phosphorus content in aluminum iron.
The present invention will be described in more detail with reference to examples. These examples are merely illustrative of the best modes of carrying out the invention and are not intended to limit the scope of the invention in any way.
The main instruments and reagents used in the following examples:
1. nitric acid (ρ1.42) (2+5);
2. Perchloric acid (ρ1.69);
3. hydrochloric acid (ρ1.19);
4. Aqua regia: mixing three parts of hydrochloric acid and one part of nitric acid;
5. Potassium permanganate solution (40 g/L);
6. Potassium sodium tartrate solution (150 g/L);
7. Ammonium molybdate solution (150 g/L);
8. ammonium molybdate-potassium sodium tartrate mixed solution: mixing ammonium molybdate (150 g/L) and potassium sodium tartrate (150 g/L) in equal volume (filtering when precipitation exists);
9. Sodium fluoride solution (24 g/L): 24g of sodium fluoride are dissolved in 1000mL of water;
10. adding 2g of stannous chloride into a sodium fluoride-stannous chloride mixed solution (24 g/L of sodium fluoride solution per liter), dissolving and shaking uniformly;
11. Phosphorus standard solution
11.1 Phosphorus stock solution (50.0. Mu.g/mL)
0.2197G of potassium dihydrogen phosphate (G.R) is weighed and dissolved in distilled water, then the distilled water is transferred into a 1000mL volumetric flask, and diluted with water until the scale is shaken up;
11.2 phosphorus standard solution (10.0. Mu.g/mL)
50.00ML of the phosphorus stock solution (50.0. Mu.g/mL) was taken in a 250mL volumetric flask and diluted with water to a scale and shaken well.
12. Instrument for measuring and controlling the intensity of light
Intelligent high-speed analyzer
Example 1: method for measuring phosphorus content in aluminum iron
1.1 Determination of the phosphorus content in AlFe
0.0500G of the sample was weighed into a 150mL beaker, 10mL aqua regia was added, the sample was heated until it dissolved, 10mL perchloric acid (ρ1.69) was added, and the heating was continued until the smoke of perchloric acid was clear. 10mL of nitric acid (2+5) is added to dissolve salts, boiled and removed.
Immediately adding 5mL of ammonium molybdate-potassium sodium tartrate mixed solution, shaking for 10s, adding 35mL of sodium fluoride-stannous chloride mixed solution, and shaking uniformly. And (3) measuring the absorbance by using an intelligent high-speed analyzer, and calculating the percentage content of phosphorus in the aluminum iron according to a phosphorus standard curve. Blank tests were performed along with the test specimens.
1.2 Phosphorus standard solution and phosphorus content
As shown in Table 1 below, 0.00, 1.00, 2.00, 4.00, 6.00mL of the phosphorus standard solution (10.0. Mu.g/mL) was taken, followed by the same analysis procedure as in 1.1 above.
Table 1: relationship between phosphorus content in phosphorus standard solution
| Reference numerals | Phosphorus standard solution | Phosphorus content% |
| Standard curve 1 | 0.00mL | 0.00 |
| Standard curve 2 | 1.00mL(10μg/mL) | 0.05 |
| Standard curve 3 | 2.00mL(10μg/mL) | 0.10 |
| Standard curve 4 | 4.00mL(10μg/mL) | 0.20 |
| Standard curve 5 | 6.00mL(10μg/mL) | 0.30 |
1.3 Drawing of phosphorus Standard Curve
Drawing a phosphorus standard curve through Excel by taking absorbance value as an ordinate and phosphorus content (%) as an abscissa, wherein the relation between the phosphorus content and absorbance value (A) is shown in the following table 2, and the drawn phosphorus standard curve is shown in fig. 1, and the linear relation is: y=1.6136x+0.0026, r 2 =0.9999.
Table 2: relationship between standard curve absorbance value and phosphorus content
| Reference numerals | Absorbance value (A) | Phosphorus content% |
| Standard curve 1 | 0.002 | 0.00 |
| Standard curve 2 | 0.083 | 0.05 |
| Standard curve 3 | 0.164 | 0.10 |
| Standard curve 4 | 0.328 | 0.20 |
| Standard curve 5 | 0.485 | 0.30 |
Example 2: precision and accuracy detection of the method of the present invention
2.1 The same sample (AlFe H6-24) was continuously measured 10 times according to the method for measuring phosphorus content in sample of example 1 described above to verify the precision of the method, and the results are shown in Table 3. It can be seen that RSD is significantly less than 1% and therefore the method of the present invention has a better precision.
Table 3: method precision experiment
2.2, The accuracy of the assay method was recovered by labelling in the absence of a suitable standard sample. The phosphorus standard solution is added when phosphorus is measured. The corresponding amounts of the additives and the results of the labeled recovery measurements are shown in Table 4. The accuracy of the detection result can be ensured by the method.
Table 4: method accuracy experiment
In conclusion, the invention provides a reliable novel analysis method for determining the phosphorus content in the aluminum iron. The method has the advantages of simple operation, easy grasp, high accuracy and precision of the measurement result, and the like, can completely meet the detection and analysis requirements, and provides accurate data for the research of aluminum iron.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. The method for determining the content of phosphorus in the aluminum iron by adopting a sodium fluoride-stannous chloride-phosphomolybdenum blue colorimetric method comprises the following steps of:
1) Dissolving a sample by using mixed acid of hydrochloric acid and nitric acid, and oxidizing phosphorus into orthophosphoric acid by using perchloric acid fuming to obtain a first sample;
2) Adding ammonium molybdate into the first sample in a nitric acid medium to generate phosphomolybdic heteropolyacid with phosphoric acid to obtain a second sample;
3) And adding tartaric acid into the second sample to eliminate interference of silicon, adding sodium fluoride coordinated iron, reducing the phosphomolybdic heteropolyacid into phosphomolybdic blue by stannous chloride, and measuring absorbance to obtain the phosphorus amount.
2. The method according to claim 1, wherein the sample is dissolved in aqua regia in step 1).
3. The process according to claim 1 or 2, wherein the concentration of nitric acid medium in step 2) is 0.8-1.2mol/L.
4. A method according to any one of claims 1-3, comprising the steps of:
S1) weighing 0.0500g of sample in a 150mL high beaker, adding 10mL aqua regia, heating until the sample is dissolved, adding 10mL perchloric acid (ρ1.69), and continuously heating until the perchloric acid smoke is completely emitted; adding 10mL of nitric acid (2+5) to dissolve salts, boiling, and taking down;
S2) immediately adding 5mL of ammonium molybdate-potassium sodium tartrate mixed solution, shaking for 10S, adding 35mL of sodium fluoride-stannous chloride mixed solution, shaking uniformly, measuring the absorbance by using an intelligent high-speed analyzer, and calculating the percentage content according to a phosphorus working curve.
5. The method of claim 4, wherein the linear relationship of the phosphorus work curve with absorbance values on the ordinate and percent phosphorus concentration on the abscissa is: y=1.6136x+0.0026, r 2 =0.9999.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311752085.4A CN117907250A (en) | 2023-12-19 | 2023-12-19 | Method for determining phosphorus in aluminum iron |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311752085.4A CN117907250A (en) | 2023-12-19 | 2023-12-19 | Method for determining phosphorus in aluminum iron |
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| Publication Number | Publication Date |
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| CN117907250A true CN117907250A (en) | 2024-04-19 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202311752085.4A Pending CN117907250A (en) | 2023-12-19 | 2023-12-19 | Method for determining phosphorus in aluminum iron |
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| Country | Link |
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| CN (1) | CN117907250A (en) |
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2023
- 2023-12-19 CN CN202311752085.4A patent/CN117907250A/en active Pending
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