CN117368131A - Chromium azure S photometry for detecting aluminum content in steel - Google Patents
Chromium azure S photometry for detecting aluminum content in steel Download PDFInfo
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- CN117368131A CN117368131A CN202311500170.1A CN202311500170A CN117368131A CN 117368131 A CN117368131 A CN 117368131A CN 202311500170 A CN202311500170 A CN 202311500170A CN 117368131 A CN117368131 A CN 117368131A
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- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 161
- 239000010959 steel Substances 0.000 title claims abstract description 161
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 122
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 121
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 229910052804 chromium Inorganic materials 0.000 title claims abstract description 29
- 239000011651 chromium Substances 0.000 title claims abstract description 29
- 238000005375 photometry Methods 0.000 title claims abstract description 20
- 108010007337 Azurin Proteins 0.000 claims abstract description 20
- 238000002835 absorbance Methods 0.000 claims abstract description 16
- 239000002253 acid Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000000243 solution Substances 0.000 claims description 206
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 146
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 72
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 36
- 239000007788 liquid Substances 0.000 claims description 24
- 238000002156 mixing Methods 0.000 claims description 23
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 20
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 18
- 238000011161 development Methods 0.000 claims description 18
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 18
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 18
- 229910017604 nitric acid Inorganic materials 0.000 claims description 18
- 239000012088 reference solution Substances 0.000 claims description 16
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 15
- 238000007865 diluting Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 14
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 14
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims description 13
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims description 13
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 12
- 229910052750 molybdenum Inorganic materials 0.000 claims description 12
- 239000011733 molybdenum Substances 0.000 claims description 12
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 12
- 229910052721 tungsten Inorganic materials 0.000 claims description 12
- 239000010937 tungsten Substances 0.000 claims description 12
- 239000000779 smoke Substances 0.000 claims description 11
- 229910052742 iron Inorganic materials 0.000 claims description 10
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 claims description 9
- 229930195725 Mannitol Natural products 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 9
- 235000010355 mannitol Nutrition 0.000 claims description 9
- 239000000594 mannitol Substances 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical group [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 8
- YTSDVWYUJXKXCC-UHFFFAOYSA-L zinc;2-[2-[carboxylatomethyl(carboxymethyl)amino]ethyl-(carboxymethyl)amino]acetate Chemical compound [Zn+2].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O YTSDVWYUJXKXCC-UHFFFAOYSA-L 0.000 claims description 8
- 238000010790 dilution Methods 0.000 claims description 6
- 239000012895 dilution Substances 0.000 claims description 6
- HVEWQPBJZAWCCX-UHFFFAOYSA-N tetraazanium cyclohexane-1,1-diamine tetraacetate Chemical compound C(C)(=O)[O-].C(C)(=O)[O-].C(C)(=O)[O-].C(C)(=O)[O-].C1(CCCCC1)(N)N.[NH4+].[NH4+].[NH4+].[NH4+] HVEWQPBJZAWCCX-UHFFFAOYSA-N 0.000 claims description 5
- BDOYKFSQFYNPKF-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(carboxymethyl)amino]acetic acid;sodium Chemical compound [Na].[Na].OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O BDOYKFSQFYNPKF-UHFFFAOYSA-N 0.000 claims description 4
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 claims description 4
- 238000012417 linear regression Methods 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- RNMCCPMYXUKHAZ-UHFFFAOYSA-N 2-[3,3-diamino-1,2,2-tris(carboxymethyl)cyclohexyl]acetic acid Chemical compound NC1(N)CCCC(CC(O)=O)(CC(O)=O)C1(CC(O)=O)CC(O)=O RNMCCPMYXUKHAZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 3
- 235000019504 cigarettes Nutrition 0.000 claims description 3
- 230000000391 smoking effect Effects 0.000 claims description 3
- 230000008569 process Effects 0.000 abstract description 5
- 238000001514 detection method Methods 0.000 abstract description 4
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 abstract description 3
- 101001018064 Homo sapiens Lysosomal-trafficking regulator Proteins 0.000 abstract description 3
- 102100033472 Lysosomal-trafficking regulator Human genes 0.000 abstract description 3
- 235000010703 Modiola caroliniana Nutrition 0.000 abstract description 3
- 244000038561 Modiola caroliniana Species 0.000 abstract description 3
- 229910045601 alloy Inorganic materials 0.000 abstract description 3
- 239000000956 alloy Substances 0.000 abstract description 3
- 238000012545 processing Methods 0.000 abstract description 2
- 230000002378 acidificating effect Effects 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 13
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 12
- 239000011787 zinc oxide Substances 0.000 description 6
- 239000004411 aluminium Substances 0.000 description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- IXGIXILVXOCZSV-UHFFFAOYSA-N acetic acid;cyclohexane-1,1-diamine Chemical compound CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O.NC1(N)CCCCC1 IXGIXILVXOCZSV-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 1
- 229910000570 Cupronickel Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000011481 absorbance measurement Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- XTEGARKTQYYJKE-UHFFFAOYSA-N chloric acid Chemical compound OCl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-N 0.000 description 1
- 229940005991 chloric acid Drugs 0.000 description 1
- 229960001701 chloroform Drugs 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000011775 sodium fluoride Substances 0.000 description 1
- 235000013024 sodium fluoride Nutrition 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 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
- 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
-
- 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
- G01N1/38—Diluting, dispersing or mixing samples
-
- 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
-
- 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
Abstract
The invention belongs to the technical field of steel processing, and discloses a chromium azurin S photometry for detecting aluminum content in steel, which comprises the steps of dissolving a steel sample by using mixed acid, generating a mauve complex by aluminum and chromium azurin-S in a weak acidic medium with pH of 5.3-5.9, and measuring absorbance of the mauve complex, so that the aluminum content of the steel sample is calculated according to the absorbance. According to the invention, the chromium azurin S photometry for determining the aluminum content in the steel is optimized, so that ammonium fluoride is not needed in the detection process, the detection process is simple, rapid, accurate and environment-friendly, and the method is suitable for determining the aluminum content of 0.001-12.0% in the steel and the alloy.
Description
Technical Field
The invention belongs to the technical field of steel processing, and particularly relates to a chromium azure S photometry for detecting aluminum content in steel.
Background
Aluminum is a commonly used deoxidizer in steel, and a small amount of aluminum is added into the steel, so that grains can be refined, and the impact toughness can be improved. Aluminum also has oxidation resistance and corrosion resistance, and the combination of aluminum, chromium and silicon can obviously improve the high-temperature non-skinning performance and the high-temperature corrosion resistance of steel.
The aluminum element content in the steel is generally analyzed by adopting a chromium azure S photometry, the range of the aluminum content in the steel detected by the existing chromium azure S photometry is less than or equal to 2 percent, and in the operation process, ammonium fluoride is required to be added into a reference liquid, so that glassware is easy to corrode and the body health of operators is easily damaged in the operation process. When detecting steel with aluminum content more than 2%, toxic and harmful sodium fluoride precipitation separation or cupronickel reagent is adopted, or trichloromethane precipitation and extraction separation are adopted to separate the interfering elements in the sample, and EDTA titration method is adopted for titration, so that the method has the advantages of multiple steps, environmental protection, long time consumption and high cost.
Therefore, it is necessary to provide a simple, rapid, accurate and environment-friendly chromium azure S photometry for detecting the aluminum content in steel.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide the chromium azure S photometry for detecting the aluminum content in steel, which can simply, rapidly, accurately and environmentally-friendly detect the aluminum content in steel and is suitable for measuring 0.001-12.0% of aluminum content in steel and alloy.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a chrome azure S photometry for detecting aluminum content in steel, comprising:
dissolving a steel sample by using mixed acid to obtain a first solution;
adding perchloric acid into the first solution, heating until smoking, and dropwise adding hydrochloric acid to volatilize chromium to obtain a second solution;
dropwise adding hydrochloric acid into the second solution until white smoke is generated, heating and concentrating the second solution after white smoke generation, and cooling to room temperature;
adding water and first hydrochloric acid into the concentrated second solution, boiling for 20-30 seconds, and cooling to room temperature to obtain a third solution;
diluting the third solution by using water and first hydrochloric acid based on the aluminum content of the steel sample, and filtering and pipetting to obtain a fourth solution;
preparing a color development liquid and a reference liquid by using a fourth solution based on the aluminum content of the steel sample;
measuring the absorbance of the color development liquid at 550nm wavelength by referring to the reference liquid;
weighing a plurality of groups of standard samples to measure absorbance, controlling the aluminum content of the steel sample to be within the range of the aluminum content of the plurality of groups of standard samples, and carrying out linear regression on the corresponding absorbance according to the aluminum content of the plurality of groups of standard samples to obtain a working curve function;
and calculating the aluminum content of the steel sample according to the function of the working curve.
Further, the quality of the steel sample is determined according to the aluminum content of the steel sample;
when the iron content of the steel sample is less than or equal to 0.1 weight percent and less than or equal to 0.2 weight percent, the mass of the steel sample is 0.2g;
when the iron content of the steel sample is more than 0.2wt percent and less than or equal to 12wt percent, the mass of the steel sample is 0.1g.
Further, dissolving the steel sample with the mixed acid, comprising:
placing the steel sample in a mixed acid of second hydrochloric acid and nitric acid, and heating to dissolve the steel sample;
the density of the second hydrochloric acid is 1.19g/mL, and the density of the nitric acid is 1.42g/mL;
the volume ratio of the second hydrochloric acid to the nitric acid in the mixed acid is determined according to the total mass percentage of tungsten and molybdenum in the steel sample;
when the total mass percentage of tungsten and molybdenum is less than or equal to 10 percent, the volume ratio of the second hydrochloric acid to the nitric acid is 3:1-5:1;
when the total mass percentage of the tungsten and the molybdenum is more than 10 percent and less than or equal to 20 percent, the volume ratio of the second hydrochloric acid to the nitric acid is 10:1-13:1.
Further, the density of perchloric acid was 1.67g/mL, and the volume was 20mL.
Further, dropwise adding hydrochloric acid to volatilize chromium, comprising:
repeatedly volatilizing chromium with hydrochloric acid with density of 1.19g/mL, and continuing for 10-30S from the mouth of the bottle to the bottom of the cigarette.
Further, adding water and first hydrochloric acid to the concentrated second solution, comprising:
50.00mL of water and 20.0mL of first hydrochloric acid are added into the concentrated second solution, and the first hydrochloric acid is prepared by mixing hydrochloric acid with the density of 1.19g/mL and water according to the volume ratio of 1:1.
Further, based on the aluminum content of the steel coupon, the third solution was diluted with water and first hydrochloric acid and filtered, pipetted, comprising:
diluting the third solution to 100.0mL with water when the aluminum content of the steel sample is < 1.25 wt%;
when the aluminum content of the steel sample is less than or equal to 2.5wt percent and less than 1.25wt percent, adding 20.0mL of first hydrochloric acid into the third solution and diluting the solution to 200.0mL by using water;
when the aluminum content of the steel sample is less than or equal to 6wt percent and less than 2.5wt percent, 80mL of first hydrochloric acid is added into the third solution and diluted to 500.0mL by water;
when 6wt% < aluminum content of the steel sample was 12wt%, 160mL of first hydrochloric acid was added to the third solution and diluted with water to 1000.0mL.
Further, preparing a color developing solution and a reference solution based on the aluminum content of the steel sample using a fourth solution, comprising:
when the aluminum content of the steel sample is less than 0.2wt%, adding 10.0mL of mannitol solution with the mass volume concentration of 100g/L, 2.50mL of cyclohexanediamine tetraacetic acid tetra ammonium solution with the concentration of 0.036mol/L or 2.50mL of ethylenediamine tetraacetic acid disodium solution with the concentration of 0.036mol/L, 2.50mL of Zn-EDTA solution with the concentration of 0.20mol/L, 4.00mL of chrome azurin S solution with the mass volume concentration of 0.5g/L and 14.00mL of hexamethylenetetramine solution with the mass volume concentration of 420g/L into 5.00mL of fourth solution, and adding water to dilute to 50.00mL to obtain a color development liquid;
when the aluminum content of the steel sample is less than 0.2wt%, 8.00mL of disodium ethylenediamine tetraacetate solution with the concentration of 0.036mol/L, 4.00mL of chrome azurin S solution with the mass volume concentration of 0.5g/L and 14.00mL of hexamethylenetetramine solution with the mass volume concentration of 420g/L are added into 5.00mL of fourth solution, and water is added for dilution to 50.00mL, so that a reference solution is obtained.
Further, when the steel sample is iron-based and iron-nickel-based, the solution of the tetra-ammonium cyclohexanediamine tetraacetate is selected to prepare the color development liquid, and when the steel sample is nickel-based and nickel-cobalt-based, the solution of the disodium ethylenediamine tetraacetate is selected to prepare the color development liquid.
Further, preparing a color developing solution and a reference solution based on the aluminum content of the steel sample using a fourth solution, comprising:
when 0.2wt% < the aluminum content of the steel sample is not more than 12wt%, 10mL of water, 10.00mL of mannitol solution with a mass volume concentration of 100g/L, 2.50mL of mannitol solution with a concentration of 0.20mol/L are added into 2.00mL of fourth solutionZn-EDTA solution, znCl 2 The solution, 4.00mL of chrome azurin S solution with mass volume concentration of 0.5g/L and 6.00mL of hexamethylenetetramine solution with mass volume concentration of 420g/L are diluted to 50.00mL by adding water to obtain a color development liquid;
wherein ZnCl 2 The concentration of the solution was 0.018mol/L,
ZnCl when 0.2wt% < aluminium content of steel sample is less than or equal to 1.25wt% 2 The addition amount of the solution was 0,
ZnCl when the aluminium content of the steel sample is less than or equal to 2.5wt% and less than 1.25wt% > 2 The addition amount of the solution was 1.00mL,
ZnCl when the aluminum content of the steel sample is less than or equal to 12wt percent of 2.5wt percent 2 The amount of the solution added was 2.00mL.
When the aluminum content of the steel sample is less than 0.2wt%, 5.00mL of disodium ethylenediamine tetraacetate solution with the concentration of 0.036mol/L, 4.00mL of chrome azurin S solution with the mass volume concentration of 0.5g/L and 6.00mL of hexamethylenetetramine solution with the mass volume concentration of 420g/L are added into 5.00mL of fourth solution, and water is added for dilution to 50.00mL, so that a reference solution is obtained.
The invention has the technical effects and advantages that:
according to the invention, the chromium azurin S photometry for measuring the aluminum content in steel is optimized, the steel sample is dissolved by mixed acid, and in weak acid medium with pH of 5.3-5.9, the aluminum and the chromium azurin-S generate a mauve complex, and the absorbance is measured, so that the aluminum content of the steel sample is calculated according to the absorbance, and ammonium fluoride is not needed in the detection process, so that the method is simple, convenient, quick, accurate and environment-friendly, and is suitable for measuring 0.001-12.0% of aluminum content in steel and alloy.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention may be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
Drawings
FIG. 1 is a flow chart of a chromium azure S photometry for detecting aluminum content in steel according to the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
As shown in fig. 1, the present invention provides a chrome azure S photometry for detecting aluminum content in steel, comprising:
dissolving a steel sample by using mixed acid to obtain a first solution;
adding perchloric acid into the first solution, heating until smoking, and dropwise adding hydrochloric acid to volatilize chromium to obtain a second solution;
dropwise adding hydrochloric acid into the second solution until white smoke is generated, heating and concentrating the white smoke-generated second solution, and cooling to room temperature;
adding water and first hydrochloric acid into the concentrated second solution, boiling for 20-30 seconds, and cooling to room temperature to obtain a third solution;
diluting the third solution by using water and first hydrochloric acid based on the aluminum content of the steel sample, and filtering and pipetting to obtain a fourth solution;
preparing a color developing solution and a reference solution by using the fourth solution based on the aluminum content of the steel sample;
measuring the absorbance of the color development liquid at 550nm wavelength by referring to the reference liquid;
weighing a plurality of groups of standard samples to measure absorbance, controlling the aluminum content of the steel sample to be within the range of the aluminum content of the plurality of groups of standard samples, and carrying out linear regression on the corresponding absorbance according to the aluminum content of the plurality of groups of standard samples to obtain a working curve function;
and calculating the aluminum content of the steel sample according to the function of the working curve.
In some embodiments of the invention, the quality of the steel coupon is determined based on the aluminum content of the steel coupon;
when the iron content of the steel sample is less than or equal to 0.1 weight percent and less than or equal to 0.2 weight percent, the mass of the steel sample is 0.2g;
when the iron content of the steel sample is more than 0.2wt percent and less than or equal to 12wt percent, the mass of the steel sample is 0.1g.
The approximate aluminum content range of the steel sample was determined according to the type and specification of the steel.
In some embodiments of the invention, dissolving a steel sample with a mixed acid includes:
placing the steel sample in a mixed acid of second hydrochloric acid and nitric acid, and heating to dissolve the steel sample;
the density of the second hydrochloric acid is 1.19g/mL, and the density of the nitric acid is 1.42g/mL;
the volume ratio of the second hydrochloric acid to the nitric acid in the mixed acid is determined according to the total mass percentage of tungsten and molybdenum in the steel sample;
when the total mass percentage of tungsten and molybdenum is less than or equal to 10 percent, the volume ratio of the second hydrochloric acid to the nitric acid is 3:1-5:1;
when the total mass percentage of the tungsten and the molybdenum is more than 10 percent and less than or equal to 20 percent, the volume ratio of the second hydrochloric acid to the nitric acid is 10:1-13:1.
The total mass percentage of tungsten and molybdenum in the steel sample is determined according to the type and specification of the steel.
In some embodiments of the invention, the perchloric acid has a density of 1.67g/mL and a volume of 20mL.
In some embodiments of the invention, the dropping of hydrochloric acid to volatilize chromium comprises:
repeatedly volatilizing chromium with hydrochloric acid with density of 1.19g/mL, and continuing for 10-30S from the mouth of the bottle to the bottom of the cigarette.
In some embodiments of the invention, adding water and first hydrochloric acid to the concentrated second solution comprises:
50mL of water and 20.0mL of first hydrochloric acid are added into the concentrated second solution, and the first hydrochloric acid is prepared by mixing hydrochloric acid with the density of 1.19g/mL and water according to the volume ratio of 1:1.
In some embodiments of the invention, the third solution is diluted with water and first hydrochloric acid and filtered, pipetted based on the aluminum content of the steel sample, comprising:
diluting the third solution to 100.0mL with water when the aluminum content of the steel sample is < 1.25 wt%;
when the aluminum content of the steel sample is less than or equal to 2.5wt percent and less than 1.25wt percent, adding 20.0mL of first hydrochloric acid into the third solution and diluting the solution to 200.0mL by using water;
when the aluminum content of the steel sample is less than or equal to 6wt percent and less than 2.5wt percent, 80mL of first hydrochloric acid is added into the third solution and diluted to 500.0mL by water;
when 6wt% < aluminum content of the steel sample was 12wt%, 160mL of first hydrochloric acid was added to the third solution and diluted with water to 1000.0mL.
In some embodiments of the invention, a color developing solution and a reference solution are configured based on the aluminum content of a steel sample, comprising:
when the aluminum content of the steel sample is less than 0.2wt%, adding 10.0mL of mannitol solution with the mass volume concentration of 100g/L, 2.50mL of cyclohexanediamine tetraacetic acid tetra ammonium solution with the concentration of 0.036mol/L or 2.50mL of ethylenediamine tetraacetic acid disodium solution with the concentration of 0.036mol/L, 2.50mL of Zn-EDTA solution with the concentration of 0.20mol/L, 4.00mL of chrome azurin S solution with the mass volume concentration of 0.5g/L and 14.00mL of hexamethylenetetramine solution with the mass volume concentration of 420g/L into 5.00mL of fourth solution, and adding water to dilute to 50.00mL to obtain a color development liquid;
when the aluminum content of the steel sample is less than 0.2wt%, 8.00mL of disodium ethylenediamine tetraacetate solution with the concentration of 0.036mol/L, 4.00mL of chrome azurin S solution with the mass volume concentration of 0.5g/L and 14.00mL of hexamethylenetetramine solution with the mass volume concentration of 420g/L are added into 5.00mL of fourth solution, and water is added for dilution to 50.00mL, so that a reference solution is obtained.
In some embodiments of the invention, when the steel sample is iron-based and iron-nickel-based, the developing solution is prepared by using a solution of tetra-ammonium cyclohexanediamine tetraacetate, and when the steel sample is nickel-based and nickel-cobalt-based, the developing solution is prepared by using a solution of disodium ethylenediamine tetraacetate.
In some embodiments of the invention, the developing solution and the reference solution are configured with a fourth solution based on the aluminum content of the steel sample, comprising:
when the aluminum content of the steel sample is less than or equal to 12wt percent and less than 0.2wt percent, 10mL of water, 10.00mL of mannitol solution with the mass volume concentration of 100g/L, 2.50mL of Zn-EDTA solution with the concentration of 0.20mol/L and ZnCl are added into 2.00mL of fourth solution 2 The solution, 4.00mL of chrome azurin S solution with mass volume concentration of 0.5g/L and 6.00mL of hexamethylenetetramine solution with mass volume concentration of 420g/L are diluted to 50.00mL by adding water to obtain a color development liquid;
wherein ZnCl 2 The concentration of the solution was 0.018mol/L,
ZnCl when 0.2wt% < aluminium content of steel sample is less than or equal to 1.25wt% 2 The addition amount of the solution was 0,
ZnCl when the aluminium content of the steel sample is less than or equal to 2.5wt% and less than 1.25wt% > 2 The addition amount of the solution was 1.00mL,
ZnCl when the aluminum content of the steel sample is less than or equal to 12wt percent of 2.5wt percent 2 The amount of the solution added was 2.00mL.
When the aluminum content of the steel sample is less than 0.2wt%, 5.00mL of disodium ethylenediamine tetraacetate solution with the concentration of 0.036mol/L, 4.00mL of chrome azurin S solution with the mass volume concentration of 0.5g/L and 6.00mL of hexamethylenetetramine solution with the mass volume concentration of 420g/L are added into 5.00mL of fourth solution, and water is added for dilution to 50.00mL, so that a reference solution is obtained.
For a better illustration of the present solution, the following examples are also provided.
Examples
The aluminum content of the standard samples A42 GH105, B50F 162, 157GH37, 229Cr7Al7, YSBC11515-93 K3 and YSBC11507-93 GH140 were detected by the method of the invention. Unless otherwise indicated, only reagents identified as analytically pure and distilled or deionized water or water of comparable purity were used in the analysis.
S1: the solution was prepared as follows.
Zn-EDTA solution (0.20 mol/L): weighing 32.72g of zinc oxide in a 1000mL clean wide-mouth beaker, adding 200mL of hydrochloric acid (the hydrochloric acid with the concentration of ρ1.19g/mL and water are configured according to the volume ratio of 1:1), heating and dissolving, weighing 148.9g of disodium ethylenediamine tetraacetate (containing two crystal waters) in the clean 2000mL wide-mouth beaker, adding 500mL of water, adding 80mL of ammonia water (with the concentration of ρ0.90 g/mL), stirring until the solution is clear and transparent, combining the solutions in the two wide-mouth beakers, stirring uniformly, cooling to room temperature, accurately diluting to 2000mL with water, mixing uniformly, and storing in a plastic barrel.
ZnCl 2 Solution (0)018mol/L, about 0.05mol/L hydrochloric acid medium): 2.930g of zinc oxide is weighed into a clean 600mL wide-mouth beaker, 50mL of water is added, 30.0mL of hydrochloric acid (ρ1.19 g/mL) is added, and the mixture is uniformly mixed; after the violent reaction is stopped, the zinc oxide is heated again until the zinc oxide is completely dissolved, cooled to the room temperature, diluted to 1000mL accurately with water and evenly mixed.
Hexamethylenetetramine solution (420 g/L): 420g of hexamethylenetetramine is weighed into a 1000mL clean wide-mouth beaker, water is added until the volume is close to 1000mL but slightly less than 1000mL, the mixture is heated, stirred and dissolved completely, cooled to room temperature, accurately diluted to 1000mL by a 1000mL volumetric flask, and uniformly mixed.
Tetraammonium cyclohexanediamine tetraacetate solution (0.0360 mol/L): 26.208g of cyclohexanediamine tetraacetic acid is weighed into a clean 1000mL wide-mouth plastic beaker, 300mL of water is added, 20.0mL of ammonia water (rho 0.90 g/mL) is added, the mixture is uniformly mixed until the solid is completely dissolved, the mixture is transferred into a clean 2000mL volumetric flask, accurately diluted to a scale with water, uniformly mixed and stored in a plastic barrel.
Zn-CYDTA solution (0.2 mol/L): weighing 32.556g of zinc oxide in a 1000mL clean wide-mouth plastic beaker, adding 200mL of water, adding 120mL of hydrochloric acid (rho 1.19g/mL of hydrochloric acid and water are configured according to the volume ratio of 1:1), and uniformly mixing until the zinc oxide is completely dissolved; weighing 145.6g of cyclohexanediamine tetraacetic acid in a clean 1000mL wide-mouth plastic beaker, adding 300-400 mL of water, adding 160mL of ammonia water (ρ0.90 g/mL), and uniformly mixing until the solid is completely dissolved; the solutions in the two wide-mouth plastic beakers are combined in a 2000mL clean volumetric flask, accurately diluted to the scale with water, evenly mixed and stored in a plastic bucket.
Disodium ethylenediamine tetraacetate solution (0.036 mol/L): 26.8012g of disodium ethylenediamine tetraacetate (containing two crystal waters) was weighed into a clean 1000mL wide-mouth plastic beaker, approximately 800mL of water was added, heated to dissolve completely, cooled to room temperature, diluted to scale with a 2000mL volumetric flask and the solution was stored in a 3000mL plastic bucket.
S2: steel samples of A42 GH105, B50F 162, 157GH37, 229Cr7Al7, YSBC11515-93 K3 and YSBC11507-93 GH140 were prepared according to GB/T20066 or the appropriate national standards, and the sample weights of the steel samples are shown in Table 1 (accurate to 0.0001 g) along with a blank reagent with an asymmetric steel sample.
Table 1 weighing steel sample amounts
S3: placing the steel sample in a 300mL clean conical flask, adding a proper amount of second hydrochloric acid (ρ1.19 g/mL) and nitric acid (ρ1.42 g/mL) mixed acid in a proper proportion, wherein when the total mass percentage of tungsten and molybdenum in the steel sample is less than or equal to 10%, the volume ratio of the second hydrochloric acid to the nitric acid is 3:1-5:1; when the total mass percentage of tungsten and molybdenum in the steel sample is less than or equal to 20 percent, the volume ratio of hydrochloric acid to nitric acid is 10:1-13:1.
Heating at a low temperature until the steel sample is completely decomposed to obtain a first solution; adding 20mL of perchloric acid (ρ1.67 g/mL) into the first solution, uniformly mixing, heating until the smoke (the high chloric acid smoke) is generated and the smoke bottom reaches the bottle mouth, dropwise adding hydrochloric acid (ρ1.19 g/mL) to volatilize chromium, repeatedly volatilizing chromium until the smoke is generated and the smoke bottom reaches the bottle mouth for 10-30S, and obtaining a second solution; dropwise adding hydrochloric acid (ρ1.19 g/mL) into the second solution, heating and concentrating until the second solution is nearly dry when the smoke is nearly white, and cooling to room temperature; adding about 50mL of water into the concentrated second solution, adding 20.0mL of first hydrochloric acid (prepared by mixing ρ1.19g/mL of hydrochloric acid and water according to a volume ratio of 1:1), uniformly mixing, heating to boil for 20-30 seconds, and cooling to room temperature to obtain a third solution;
when the aluminum content of the steel sample is less than 1.25wt%, diluting the third solution to 100.0mL with water, mixing uniformly,
when the aluminum content of the steel sample is less than or equal to 2.5wt percent and less than 1.25wt percent, adding 20.0mL of first hydrochloric acid into the third solution, uniformly mixing, diluting to 200.0mL by using water, uniformly mixing,
when the aluminum content of the steel sample is less than or equal to 6wt percent and less than 2.5wt percent, adding 80.0mL of first hydrochloric acid into the third solution, uniformly mixing, diluting to 500.0mL by using water, uniformly mixing,
when the aluminum content of the steel sample is less than or equal to 12wt percent and less than 6wt percent, 160mL of first hydrochloric acid is added into the third solution, the mixture is uniformly mixed, diluted to 1000.0mL by water, and the mixture is uniformly mixed;
if the diluted third solution is turbid, filtering the diluted third solution by using slow filter paper;
when the aluminum content of the steel sample is less than 0.2wt%, transferring 5.00mL of the diluted and filtered third solution into a 50mL volumetric flask as a fourth solution,
when the aluminum content of the steel sample is less than or equal to 12wt percent and less than 0.2wt percent, transferring 2.00mL of the diluted and filtered third solution into a 50mL volumetric flask as a fourth solution.
S4: when the aluminum content of the steel sample is less than 0.2wt%, 10.0mL of mannitol solution (100 g/L) is added into a 50mL volumetric flask containing 5.00mL of fourth solution, the mixture is uniformly mixed, 2.50mL of cyclohexanediamine tetraacetic acid tetraammonium solution (0.036 mol/L) is added into the iron-based and iron-nickel-based steel sample, 2.50mL of ethylenediamine tetraacetic acid disodium solution (0.036 mol/L) is added into the nickel-based and nickel-cobalt-based sample, the mixture is uniformly mixed, 2.50mL of Zn-EDTA solution (0.20 mol/L) is added, the mixture is uniformly mixed, 4.00mL of chrome azure S solution (0.5 g/L) is added, 14.00mL of hexamethylenetetramine solution (420 g/L) is added, the mixture is uniformly mixed, the mixture is diluted to a scale with water, and the color development solution is obtained,
when the aluminum content of the steel sample is less than 0.2wt%, adding 8.0mL of disodium ethylenediamine tetraacetate solution (0.036 mol/L), adding 4.00mL of chrome azurin S solution (0.5 g/L), adding 14.00mL of hexamethylenetetramine solution (420 g/L), uniformly mixing, diluting to a scale with water, and uniformly mixing to obtain a reference solution;
when the aluminum content of the steel sample is less than or equal to 12wt percent, adding 10.0mL of water into a 50mL volumetric flask containing 2.00mL of fourth solution, uniformly mixing, adding 10.0mL of mannitol solution (100 g/L), uniformly mixing, adding 2.50mL of Zn-EDTA solution (0.20 mol/L), uniformly mixing, and adding ZnCl according to the aluminum content in the steel sample 2 Mixing the solutions, adding 4.00mL of chrome azure S solution (0.5 g/L), mixing, adding 6.00mL of hexamethylenetetramine solution (420 g/L), mixing, diluting with water to scale, mixing to obtain color development liquid,
wherein ZnCl is not added when the aluminum content of the steel sample is less than or equal to 1.25wt% and less than 0.2wt% 2 When the aluminum content of the solution is less than or equal to 2.5 weight percent of 1.25 weight percent of the steel sample, 1.00mL of ZnCl is added 2 Solution (0.018 mol/L), when 2.5 wt.% < aluminum content of steel sample. Ltoreq.12 wt.%, add 2.00mL ZnCl 2 The solution (0.018 mol/L),
when the aluminum content of the steel sample is less than or equal to 12wt percent, 5.0mL of disodium ethylenediamine tetraacetate solution (0.036 mol/L) is added into a 50mL volumetric flask containing 2.00mL of fourth solution, 4.00mL of chrome azure-S solution (0.5 g/L) is added, 6.00mL of hexamethylenetetramine solution (420 g/L) is added, the mixture is uniformly mixed, diluted to a scale by water, and the mixture is uniformly mixed, thus obtaining the reference solution.
S5: placing the color development liquid and the reference liquid for 20-30 minutes at room temperature, and then, selecting a 1cm absorption vessel on a visible spectrophotometer, taking the corresponding reference liquid as a reference, and measuring the absorbance of the corresponding color development liquid at the wavelength of 550 nm.
S6: weighing 5-6 standard samples, controlling the aluminum content of the steel sample within the aluminum content range of the standard samples, operating according to the analysis steps, measuring the absorbance of each standard sample, and carrying out linear regression on the aluminum content of the standard samples to obtain a working curve function on the corresponding absorbance.
S7: and calculating the aluminum content of the steel sample according to the function of the working curve, wherein the calculation formula is as follows:
wherein: w (W) A1 For the aluminium content, m of the steel sample 1 In order to find the aluminum content corresponding to the absorbance measurement value of the developing solution from the function of the working curve, m is the mass of the steel sample.
The test results are shown in Table 2.
Table 2 sample test data table
As can be seen from Table 2, the difference between the result of detecting the aluminum content in the standard sample and the standard value is smaller than the allowable difference of the navigation mark, the difference between the detected double sample results is smaller than the allowable difference of the navigation mark, and the detection result is accurate.
Finally, it should be noted that: the foregoing description is only illustrative of the preferred embodiments of the present invention, and 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 modifications may be made to the embodiments described, or equivalents may be substituted for elements thereof, and any modifications, equivalents, improvements or changes may be made without departing from the spirit and principles of the present invention.
Claims (10)
1. A chrome azure S photometry for detecting aluminum content in steel, comprising:
dissolving the steel sample by using mixed acid to obtain a first solution;
adding perchloric acid into the first solution, heating until smoking, and dropwise adding hydrochloric acid to volatilize chromium to obtain a second solution;
dropwise adding hydrochloric acid into the second solution until white smoke is generated, heating and concentrating the second solution after white smoke generation, and cooling to room temperature;
adding water and first hydrochloric acid into the concentrated second solution, boiling for 20-30 seconds, and cooling to room temperature to obtain a third solution;
diluting the third solution by using water and first hydrochloric acid based on the aluminum content of the steel sample, and filtering and pipetting to obtain a fourth solution;
preparing a color developing solution and a reference solution by using the fourth solution based on the aluminum content of the steel sample;
measuring absorbance of the color development liquid at 550nm wavelength by referring to the reference liquid;
weighing a plurality of groups of standard samples to measure absorbance, controlling the aluminum content of the steel sample to be within the aluminum content measuring value ranges of the plurality of groups of standard samples, and carrying out linear regression on the corresponding absorbance according to the aluminum content of the plurality of groups of standard samples to obtain a working curve function;
and calculating the aluminum content of the steel sample according to the working curve function.
2. A chromium azurin S photometry for detecting aluminum content in steel according to claim 1, wherein,
the quality of the steel sample is determined according to the aluminum content of the steel sample;
when the iron content of the steel sample is less than or equal to 0.1 weight percent and less than or equal to 0.2 weight percent, the mass of the steel sample is 0.2g;
when the iron content of the steel sample is more than 0.2wt percent and less than or equal to 12wt percent, the mass of the steel sample is 0.1g.
3. A chrome azurin S photometry for detecting aluminum content in steel according to claim 1, wherein said dissolving said steel sample with mixed acid comprises:
placing the steel sample in a second mixed acid of hydrochloric acid and nitric acid, and heating to dissolve the steel sample;
the density of the second hydrochloric acid is 1.19g/mL, and the density of the nitric acid is 1.42g/mL;
the volume ratio of the second hydrochloric acid to the nitric acid in the mixed acid is determined according to the total mass percentage of tungsten and molybdenum in the steel sample;
when the total mass percentage of tungsten and molybdenum is less than or equal to 10 percent, the volume ratio of the second hydrochloric acid to the nitric acid is 3:1-5:1;
when the total mass percentage of the tungsten and the molybdenum is more than 10 percent and less than or equal to 20 percent, the volume ratio of the second hydrochloric acid to the nitric acid is 10:1-13:1.
4. A chromium azurin S photometry for detecting aluminum content in steel according to claim 1, wherein,
the density of the perchloric acid is 1.67g/mL, and the volume is 20mL.
5. The chromium azurin S photometry for detecting aluminum content in steel according to claim 1, wherein the dropping hydrochloric acid for volatilizing chromium comprises:
repeatedly volatilizing chromium with hydrochloric acid with density of 1.19g/mL, and continuing for 10-30S from the mouth of the bottle to the bottom of the cigarette.
6. A chromated azure S photometry for detecting aluminum content in steel according to claim 1, wherein said adding water and first hydrochloric acid to said second solution after concentration comprises:
and adding 50mL of water and 20.0mL of first hydrochloric acid into the concentrated second solution, wherein the first hydrochloric acid is prepared by mixing hydrochloric acid with the density of 1.19g/mL and water according to the volume ratio of 1:1.
7. The method for detecting aluminum content in steel according to claim 6, wherein the third solution is diluted with water and first hydrochloric acid based on aluminum content of steel sample, filtered and pipetted, comprising:
diluting the third solution with water to 100.0mL when the aluminum content of the steel sample is < 1.25 wt%;
when the aluminum content of the steel sample is less than or equal to 2.5wt percent and less than 1.25wt percent, adding 20.0mL of first hydrochloric acid into the third solution and diluting the solution to 200.0mL by water;
when the aluminum content of the steel sample is less than or equal to 6wt percent and less than 2.5wt percent, 80mL of first hydrochloric acid is added into the third solution, and the third solution is diluted to 500.0mL by water;
when 6wt% < aluminum content of the steel sample was 12wt%, 160mL of first hydrochloric acid was added to the third solution and diluted with water to 1000.0mL.
8. The method for detecting aluminum content in steel according to claim 1, wherein the preparing the color developing solution and the reference solution based on the aluminum content of the steel sample by using the fourth solution comprises:
when the aluminum content of the steel sample is less than 0.2wt%, adding 10.0mL of mannitol solution with the mass volume concentration of 100g/L, 2.50mL of cyclohexanediamine tetraacetic acid tetra ammonium solution with the concentration of 0.036mol/L or 2.50mL of ethylenediamine tetraacetic acid disodium solution with the mass volume concentration of 0.036mol/L, 2.50mL of Zn-EDTA solution with the mass volume concentration of 0.20mol/L, 4.00mL of chrome azure S solution with the mass volume concentration of 0.5g/L and 14.00mL of hexamethylenetetramine solution with the concentration of 420g/L into 5.00mL of the fourth solution, and adding water to dilute to 50.00mL to obtain a color development liquid;
when the aluminum content of the steel sample is less than 0.2wt%, 8.00mL of disodium ethylenediamine tetraacetate solution with the concentration of 0.036mol/L, 4.00mL of chrome azurin S solution with the mass volume concentration of 0.5g/L and 14.00mL of hexamethylenetetramine solution with the mass volume concentration of 420g/L are added into 5.00mL of the fourth solution, and water is added for dilution to 50.00mL, so that a reference solution is obtained.
9. A chromium azurin S photometry for detecting aluminum content in steel according to claim 8, wherein,
when the steel sample is iron-based and iron-nickel-based, the solution of the cyclohexanediamine tetraacetic acid is selected to prepare the color development liquid, and when the steel sample is nickel-based and nickel-cobalt-based, the solution of the ethylenediamine tetraacetic acid is selected to prepare the color development liquid.
10. The method for detecting aluminum content in steel according to claim 8, wherein the preparing the color developing solution and the reference solution based on the aluminum content of the steel sample by using the fourth solution comprises:
when the aluminum content of the steel sample is less than or equal to 12wt percent and less than 0.2wt percent, 10mL of water, 10.00mL of mannitol solution with the mass volume concentration of 100g/L, 2.50mL of Zn-EDTA solution with the concentration of 0.20mol/L and ZnCl are added into 2.00mL of the fourth solution 2 The solution, 4.00mL of chrome azurin S solution with mass volume concentration of 0.5g/L and 6.00mL of hexamethylenetetramine solution with mass volume concentration of 420g/L are diluted to 50.00mL by adding water to obtain a color development liquid;
wherein the ZnCl 2 The concentration of the solution was 0.018mol/L,
when 0.2wt% < aluminum content of steel sample is 1.25wt% or less, the ZnCl 2 The addition amount of the solution was 0,
when 1.25wt% < aluminum content of steel sample is 2.5wt% or less, the ZnCl 2 The addition amount of the solution was 1.00mL,
when the aluminum content of the steel sample is less than or equal to 12 weight percent of 2.5 weight percent, the ZnCl 2 The addition amount of the solution was 2.00mL,
when the aluminum content of the steel sample is less than 0.2wt%, 5.00mL of disodium ethylenediamine tetraacetate solution with the concentration of 0.036mol/L, 4.00mL of chrome azurin S solution with the mass volume concentration of 0.5g/L and 6.00mL of hexamethylenetetramine solution with the mass volume concentration of 420g/L are added into 5.00mL of the fourth solution, and water is added for dilution to 50.00mL, so that a reference solution is obtained.
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