CN113252660A - Method for analyzing chemical component content of high-temperature alloy corrosive liquid - Google Patents
Method for analyzing chemical component content of high-temperature alloy corrosive liquid Download PDFInfo
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- 239000007788 liquid Substances 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000000956 alloy Substances 0.000 title claims abstract description 15
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 15
- 239000000126 substance Substances 0.000 title claims abstract description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 150
- 238000004448 titration Methods 0.000 claims abstract description 61
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract description 57
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 47
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims abstract description 32
- 235000019345 sodium thiosulphate Nutrition 0.000 claims abstract description 29
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 19
- 239000003518 caustics Substances 0.000 claims abstract description 18
- 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 abstract description 10
- ZNNZYHKDIALBAK-UHFFFAOYSA-M potassium thiocyanate Chemical compound [K+].[S-]C#N ZNNZYHKDIALBAK-UHFFFAOYSA-M 0.000 claims abstract description 4
- 229940116357 potassium thiocyanate Drugs 0.000 claims abstract description 4
- 239000002244 precipitate Substances 0.000 claims abstract description 4
- 238000002798 spectrophotometry method Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 106
- 238000005530 etching Methods 0.000 claims description 19
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 18
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000012086 standard solution Substances 0.000 claims description 13
- 239000011550 stock solution Substances 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 10
- 235000010323 ascorbic acid Nutrition 0.000 claims description 9
- 229960005070 ascorbic acid Drugs 0.000 claims description 9
- 239000011668 ascorbic acid Substances 0.000 claims description 9
- UDSAIICHUKSCKT-UHFFFAOYSA-N bromophenol blue Chemical compound C1=C(Br)C(O)=C(Br)C=C1C1(C=2C=C(Br)C(O)=C(Br)C=2)C2=CC=CC=C2S(=O)(=O)O1 UDSAIICHUKSCKT-UHFFFAOYSA-N 0.000 claims description 9
- 238000005260 corrosion Methods 0.000 claims description 8
- 230000007797 corrosion Effects 0.000 claims description 8
- 238000002835 absorbance Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 229920002472 Starch Polymers 0.000 claims description 3
- 239000011541 reaction mixture Substances 0.000 claims description 3
- 239000000523 sample Substances 0.000 claims description 3
- 239000012488 sample solution Substances 0.000 claims description 3
- 235000019698 starch Nutrition 0.000 claims description 3
- 239000008107 starch Substances 0.000 claims description 3
- 230000002452 interceptive effect Effects 0.000 abstract description 3
- 150000002500 ions Chemical class 0.000 abstract description 2
- 238000001514 detection method Methods 0.000 description 5
- 239000012490 blank solution Substances 0.000 description 2
- 238000007655 standard test method Methods 0.000 description 2
- 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 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
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- 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
- G01N21/79—Photometric titration
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- 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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
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Abstract
The invention discloses a method for analyzing the chemical component content of high-temperature alloy corrosive liquid, which is based on FeCl in a corrosive agent3Concentration range selection of FeCl3If FeCl is in the etchant3If the concentration range of (1) is more than 50g/L, then carrying out step 2; if FeCl3If the concentration range of (1) is below 5.8g/L, performing step 3; step 2, measuring FeCl by sodium thiosulfate titration method3Content (c); step 3, measuring FeCl by potassium thiocyanate spectrophotometry3Content (c); step 4, dropwise adding a sodium hydroxide solution into the corrosive agent sample without obvious phenomenon, and performing step 5; if a precipitate is generated, performing step 6; step 5, determining the content of HCL by a sodium hydroxide determination method; step 6, adding EDTA solution, and determining the content of HCL by a sodium hydroxide determination method; the invention can avoid the influence of interfering ions and can also avoid the influence of interfering ionsThe concentration of hydrochloric acid and ferric trichloride can be accurately determined.
Description
Technical Field
The invention belongs to the technical field of quality detection, and relates to a chemical component content analysis method for high-temperature alloy corrosion liquid.
Background
The corrosive agent is ferric trichloride solution, the solution consists of hydrochloric acid solution and ferric trichloride solution, and the method is suitable for macroscopic corrosion inspection of rough-processed cast and forged high-temperature alloy and finish-processed forged high-temperature alloy. When the concentration of the etchant deviates from the predetermined range, the etching effect is not achieved within a predetermined time, and therefore, the control of the concentration of the etchant component is critical.
Through inquiry, various standards do not have a standard test method for detecting the components of the corrosive agent consisting of a hydrochloric acid solution and a ferric trichloride solution at present, and a set of scientific detection method needs to be made for detecting the chemical components of a project, so that the concentrations of the hydrochloric acid solution and the ferric trichloride solution can be accurately measured, data support is provided for a corrosion line, and the concentration of the components of the corrosive agent is effectively controlled.
Disclosure of Invention
The invention aims to provide a method for analyzing the chemical component content of high-temperature alloy corrosive liquid, which solves the problem that a standard test method for detecting the components of a corrosive agent consisting of a hydrochloric acid solution and a ferric trichloride solution is lacked in the prior art.
The technical scheme adopted by the invention is that the method for analyzing the chemical component content of the high-temperature alloy corrosive liquid is implemented according to the following steps:
step 1, according to FeCl in the corrosive agent3Concentration range selection of FeCl3If FeCl is in the etchant3If the concentration range of (1) is more than 50g/L, then carrying out step 2; if FeCl3If the concentration range of (1) is below 5.8g/L, performing step 3;
step 2, measuring FeCl by sodium thiosulfate titration method3Content (c);
step 3, measuring FeCl by potassium thiocyanate spectrophotometry3Content (c);
step 4, dropwise adding a sodium hydroxide solution into the corrosive agent sample without obvious phenomenon, and performing step 5; if a precipitate is generated, performing step 6;
step 5, determining the content of HCL by a sodium hydroxide determination method;
step 6, adding EDTA solution, and determining the content of HCL by a sodium hydroxide determination method;
and 7, repairing the measured data according to GB/T8170 expression and judgment of numerical value repairing rules and limit numerical values.
The invention is also characterized in that:
step 2 is specifically carried out as follows:
step 2.1, preparing a sodium thiosulfate standard solution, wherein the concentration of the sodium thiosulfate standard solution is 0.10 mol/L;
step 2.2, dividing V ml of corrosive agent stock solution into conical flasks, adding water to dilute the corrosive agent stock solution to 100ml, adding excessive potassium iodide, shaking up to fully dissolve the potassium iodide, adding 2-3 ml of 10g/L starch indicator solution, shaking up, titrating the mixture to green by using a sodium thiosulfate standard titration solution, and recording the volume of the sodium thiosulfate consumption standard titration solution as V1Simultaneously, a blank test is carried out, and the volume of the standard titration solution consuming the sodium thiosulfate is recorded as V0;
Step 2.3, calculating FeCl3Is calculated according to formula (1):
in formula (1):
M(FeCl3) -the molar mass of ferric chloride, g/mol;
csodium thiosulfate-the molar concentration of sodium thiosulfate, mol/L;
V0-blank test consumes sodium thiosulfate standard titration solution volume, ml;
V1consumption of sodium thiosulfate standard titration solution volume, ml;
v, dividing the volume of the stock solution into ml;
d(FeCl3)——FeCl3concentration of (3), g/L.
Step 3 is specifically carried out as follows:
step 3.1, making a standard curve;
step 3.2, drawing a standard curve;
step 3.3, developing and measuring absorbance value, substituting the absorbance value into a standard curve to calculate FeCl3Calculated as follows:
in formula (3):
m(Fe3+) -finding Fe on the working curve3+Mass of (2), mg;
m(FeCl3)——FeCl3mass of (c), g;
M(FeCl3)——FeCl3with respect to the mass of the molecules,
M(Fe3+)——Fe3+relative atomic mass.
Step 5 is specifically implemented as follows:
step 5.1, preparing a sodium hydroxide standard titration solution, wherein the concentration of the sodium hydroxide standard titration solution is 1.0 mol/L;
step 5.2, dividing and taking corrosive liquid V'0Putting into conical flask, adding water to 100ml, adding ascorbic acid solution, and shaking thoroughly to obtain Fe3+All conversion to Fe2+Adding 8-10 drops of bromophenol blue indicator, shaking up, titrating to purple with sodium hydroxide standard titration solution, and reading volume V 'of sodium hydroxide consumed standard titration solution'1;
And 5.3, calculating the content of HCl according to the following calculation formula:
in the formula (4), the reaction mixture is,
d (HCl) -content of hydrochloric acid in the etching solution, g/L
V’1-titrating the volume, ml, of the sodium hydroxide standard titration solution consumed by the etching solution;
V’0-dividing the volume of the etching solution, ml;
cNaOH-molarity, mol/L of sodium hydroxide standard solution;
d(FeCl3) FeCl in corrosive liquid3The content of (a) in (b),g/L;
m (HCl) -molar mass of HCl, g/mol;
M(FeCl3)——FeCl3molar mass of (a), g/mol.
Step 6 is implemented according to the following steps:
step 6.1, dividing and taking the corrosive liquid V0Putting the mixture into an erlenmeyer flask, adding water to 100ml, adding an ascorbic acid solution, and fully shaking the mixture until the solution is Fe3+All conversion to Fe2+Adding a proper amount of EDTA solution, shaking up, adding 8-10 drops of bromophenol blue indicator, shaking up, titrating to purple by using sodium hydroxide standard titration solution, reading volume V of sodium hydroxide consumption standard titration solution1”;
Step 6.2, blank titration solution: in order to keep the volume consistent, 10.00ml of water is divided to replace a sample solution, water is added to 100ml, an EDTA solution is added to shake up, 8-10 drops of bromophenol blue indicator are added to shake up, sodium hydroxide standard titration solution is used for titration until the solution becomes purple, and the volume V of the sodium hydroxide standard titration solution consumed is read2”;
And 6.3, calculating the content of HCl according to the following calculation formula:
in formula (5):
d(HCl)-the content of hydrochloric acid in the etching solution, g/L;
V”1-titrating the volume, ml, of the sodium hydroxide standard titration solution consumed by the etching solution;
V”2-titration of the volume of sodium hydroxide standard titration solution consumed for the blank solution, ml;
V”0-dividing the volume of the etching solution, ml;
cNaOH-concentration of sodium hydroxide standard solution, mol/L;
d(FeCl3) FeCl in corrosive liquid3The content of (a), g/L;
M(HCl)——molar mass of HCl, g/mol;
M(FeCl3)——FeCl3molar mass of (a), g/mol.
Ascorbic acid and Fe3+The theoretical quantitative relationship of (1) is as follows:
m(C6H8O6)=1.57×m(Fe3+) (3)
in the formula (3), m (C)6H8O6)——C6H8O6Molar mass of (a), g/mol.
The invention has the beneficial effects that:
1. the invention is suitable for FeCl3FeCl in the corrosive liquid with the concentration of more than 50g/L3And (4) measuring the content. After the sodium thiosulfate standard solution is diluted, the lower limit of detection can be expanded; the stock solution is diluted, and the detection upper limit can be expanded.
2. The invention is suitable for FeCl3FeCl in the etching solution with the concentration of less than 5.8g/L3The content measurement and the volume of the diluted stock solution can expand the upper limit of detection.
3. The invention can avoid the influence of the existence of interfering ions and can also achieve the purpose of accurately measuring the concentrations of hydrochloric acid and ferric trichloride.
The present invention will be described in detail with reference to the following embodiments.
The invention relates to a method for analyzing the chemical component content of high-temperature alloy corrosive liquid, which is implemented according to the following steps:
step 1, according to FeCl in the corrosive agent3Concentration range selection of FeCl3If FeCl is in the etchant3If the concentration range of (1) is more than 50g/L, then carrying out step 2; if FeCl3If the concentration range of (1) is below 5.8g/L, performing step 3;
step 2, measuring FeCl by sodium thiosulfate titration method3Content (c);
step 3, measuring FeCl by potassium thiocyanate spectrophotometry3Content (c);
step 4, dropwise adding a sodium hydroxide solution into the corrosive agent sample without obvious phenomenon, and performing step 5; if a precipitate is generated, performing step 6;
step 5, determining the content of HCL by a sodium hydroxide determination method;
step 6, adding EDTA solution, and determining the content of HCL by a sodium hydroxide determination method;
and 7, repairing the measured data according to GB/T8170 expression and judgment of numerical value repairing rules and limit numerical values.
Step 2 is specifically carried out as follows:
step 2.1, preparing a sodium thiosulfate standard solution, wherein the concentration of the sodium thiosulfate standard solution is 0.10 mol/L;
step 2.2, dividing V ml of corrosive agent stock solution into conical flasks, adding water to dilute the corrosive agent stock solution to 100ml, adding excessive potassium iodide, shaking up to fully dissolve the potassium iodide, adding 2-3 ml of 10g/L starch indicator solution, shaking up, titrating the mixture to green by using a sodium thiosulfate standard titration solution, and recording the volume of the sodium thiosulfate consumption standard titration solution as V1Simultaneously, a blank test is carried out, and the volume of the standard titration solution consuming the sodium thiosulfate is recorded as V0;
Step 2.3, calculating FeCl3Is calculated according to formula (1):
in formula (1):
M(FeCl3) -the molar mass of ferric chloride, g/mol;
csodium thiosulfate-the molar concentration of sodium thiosulfate, mol/L;
V0-blank test consumes sodium thiosulfate standard titration solution volume, ml;
V1consumption of sodium thiosulfate standard titration solution volume, ml;
v, dividing the volume of the stock solution into ml;
d(FeCl3)——FeCl3concentration of (3), g/L.
Step 3 is specifically carried out as follows:
step 3.1, making a standard curve;
step 3.2, drawing a standard curve;
step 3.3, developing and measuring absorbance value, substituting the absorbance value into a standard curve to calculate FeCl3Calculated as follows:
in formula (3):
m(Fe3+) -finding Fe on the working curve3+Mass of (2), mg;
m(FeCl3)——FeCl3mass of (c), g;
M(FeCl3)——FeCl3with respect to the mass of the molecules,
M(Fe3+)——Fe3+relative atomic mass.
Step 5 is specifically implemented as follows:
step 5.1, preparing a sodium hydroxide standard titration solution, wherein the concentration of the sodium hydroxide standard titration solution is 1.0 mol/L;
step 5.2, dividing and taking corrosive liquid V'0Putting into conical flask, adding water to 100ml, adding ascorbic acid solution, and shaking thoroughly to obtain Fe3+All conversion to Fe2+Adding 8-10 drops of bromophenol blue indicator, shaking up, titrating to purple with sodium hydroxide standard titration solution, and reading volume V 'of sodium hydroxide consumed standard titration solution'1;
And 5.3, calculating the content of HCl according to the following calculation formula:
in the formula (4), the reaction mixture is,
d (HCl) -content of hydrochloric acid in corrosive liquid, g/LV'1-titrating the volume, ml, of the sodium hydroxide standard titration solution consumed by the etching solution;
V’0-dividing the volume of the etching solution, ml;
cNaOH-molarity, mol/L of sodium hydroxide standard solution;
d(FeCl3) FeCl in corrosive liquid3The content of (a), g/L;
m (HCl) -molar mass of HCl, g/mol;
M(FeCl3)——FeCl3molar mass of (a), g/mol.
Step 6 is implemented according to the following steps:
step 6.1, dividing and taking the corrosive liquid V0Putting the mixture into an erlenmeyer flask, adding water to 100ml, adding an ascorbic acid solution, and fully shaking the mixture until the solution is Fe3+All conversion to Fe2+Adding a proper amount of EDTA solution, shaking up, adding 8-10 drops of bromophenol blue indicator, shaking up, titrating to purple by using sodium hydroxide standard titration solution, reading volume V of sodium hydroxide consumption standard titration solution1”;
Step 6.2, blank titration solution: in order to keep the volume consistent, 10.00ml of water is divided to replace a sample solution, water is added to 100ml, an EDTA solution is added to shake up, 8-10 drops of bromophenol blue indicator are added to shake up, sodium hydroxide standard titration solution is used for titration until the solution becomes purple, and the volume V of the sodium hydroxide standard titration solution consumed is read2”;
And 6.3, calculating the content of HCl according to the following calculation formula:
in formula (5):
d(HCl)-the content of hydrochloric acid in the etching solution, g/L;
V”1-titrating the volume, ml, of the sodium hydroxide standard titration solution consumed by the etching solution;
V2"-the volume of sodium hydroxide standard titration solution consumed for titration of the blank solution, ml;
V0"— dividing the volume of the etching solution, ml;
cNaOH-Hydrogen oxygenThe concentration of the sodium chemical standard solution, mol/L;
d(FeCl3) FeCl in corrosive liquid3The content of (a), g/L;
M(HCl)-molar mass of HCl, g/mol;
M(FeCl3)——FeCl3molar mass of (a), g/mol.
Ascorbic acid and Fe3+The theoretical quantitative relationship of (1) is as follows:
m(C6H8O6)=1.57×m(Fe3+) (3)
in the formula (3), m (C)6H8O6)——C6H8O6Molar mass of (a), g/mol.
Claims (6)
1. The method for analyzing the chemical component content of the high-temperature alloy corrosive liquid is characterized by comprising the following steps:
step 1, according to FeCl in the corrosive agent3Concentration range selection of FeCl3If FeCl is in the etchant3If the concentration range of (1) is more than 50g/L, then carrying out step 2; if FeCl3If the concentration range of (1) is below 5.8g/L, performing step 3;
step 2, measuring FeCl by sodium thiosulfate titration method3Content (c);
step 3, measuring FeCl by potassium thiocyanate spectrophotometry3Content (c);
step 4, dropwise adding a sodium hydroxide solution into the corrosive agent sample without obvious phenomenon, and performing step 5; if a precipitate is generated, performing step 6;
step 5, determining the content of HCL by a sodium hydroxide determination method;
step 6, adding EDTA solution, and determining the content of HCL by a sodium hydroxide determination method;
and 7, repairing the measured data according to GB/T8170 expression and judgment of numerical value repairing rules and limit numerical values.
2. The method for analyzing the chemical component content of the corrosion liquid of the high-temperature alloy as claimed in claim 1, wherein the step 2 is specifically performed according to the following steps:
step 2.1, preparing a sodium thiosulfate standard solution, wherein the concentration of the sodium thiosulfate standard solution is 0.10 mol/L;
step 2.2, dividing V ml of corrosive agent stock solution into conical flasks, adding water to dilute the corrosive agent stock solution to 100ml, adding excessive potassium iodide, shaking up to fully dissolve the potassium iodide, adding 2-3 ml of 10g/L starch indicator solution, shaking up, titrating the mixture to green by using a sodium thiosulfate standard titration solution, and recording the volume of the sodium thiosulfate consumption standard titration solution as V1Simultaneously, a blank test is carried out, and the volume of the standard titration solution consuming the sodium thiosulfate is recorded as V0;
Step 2.3, calculating FeCl3Is calculated according to formula (1):
in formula (1):
M(FeCl3) -the molar mass of ferric chloride, g/mol;
csodium thiosulfate-the molar concentration of sodium thiosulfate, mol/L;
V0-blank test consumes sodium thiosulfate standard titration solution volume, ml;
V1consumption of sodium thiosulfate standard titration solution volume, ml;
v, dividing the volume of the stock solution into ml;
d(FeCl3)——FeCl3concentration of (3), g/L.
3. The method for analyzing the chemical component content of the corrosion liquid of the high-temperature alloy as claimed in claim 1, wherein the step 3 is specifically performed as follows:
step 3.1, making a standard curve;
step 3.2, drawing a standard curve;
step 3.3, developing and determining the absorbance value, substituting the absorbance value intoCalculating FeCl by the standard curve3Calculated as follows:
in formula (3):
m(Fe3+) -finding Fe on the working curve3+Mass of (2), mg;
m(FeCl3)——FeCl3mass of (c), g;
M(FeCl3)——FeCl3with respect to the mass of the molecules,
M(Fe3+)——Fe3+relative atomic mass.
4. The method for analyzing the chemical component content of the corrosion liquid of the high-temperature alloy as claimed in claim 1, wherein the step 5 is specifically performed as follows:
step 5.1, preparing a sodium hydroxide standard titration solution, wherein the concentration of the sodium hydroxide standard titration solution is 1.0 mol/L;
step 5.2, dividing and taking corrosive liquid V'0Putting into conical flask, adding water to 100ml, adding ascorbic acid solution, and shaking thoroughly to obtain Fe3+All conversion to Fe2+Adding 8-10 drops of bromophenol blue indicator, shaking up, titrating to purple with sodium hydroxide standard titration solution, and reading volume V 'of sodium hydroxide consumed standard titration solution'1;
And 5.3, calculating the content of HCl according to the following calculation formula:
in the formula (4), the reaction mixture is,
d (HCl) -content of hydrochloric acid in the etching solution, g/L
V’1-titrating the volume, ml, of the sodium hydroxide standard titration solution consumed by the etching solution;
V’0-dividing the volume of the etching solution, ml;
cNaOH-molarity, mol/L of sodium hydroxide standard solution;
d(FeCl3) FeCl in corrosive liquid3The content of (a), g/L;
m (HCl) -molar mass of HCl, g/mol;
M(FeCl3)——FeCl3molar mass of (a), g/mol.
5. The method for analyzing the chemical component content of the corrosion liquid of the high-temperature alloy, as set forth in claim 1, wherein the step 6 is specifically carried out according to the following steps:
step 6.1, dividing and taking the corrosive liquid V0Putting the mixture into an erlenmeyer flask, adding water to 100ml, adding an ascorbic acid solution, and fully shaking the mixture until the solution is Fe3+All conversion to Fe2+Adding a proper amount of EDTA solution, shaking up, adding 8-10 drops of bromophenol blue indicator, shaking up, titrating to purple by using sodium hydroxide standard titration solution, reading volume V of sodium hydroxide consumption standard titration solution1”;
Step 6.2, blank titration solution: in order to keep the volume consistent, 10.00ml of water is divided to replace a sample solution, water is added to 100ml, an EDTA solution is added to shake up, 8-10 drops of bromophenol blue indicator are added to shake up, sodium hydroxide standard titration solution is used for titration until the solution becomes purple, and the volume V of the sodium hydroxide standard titration solution consumed is read2”;
And 6.3, calculating the content of HCl according to the following calculation formula:
in formula (5):
d(HCl)-the content of hydrochloric acid in the etching solution, g/L;
V”1-titrating the volume, ml, of the sodium hydroxide standard titration solution consumed by the etching solution;
V2"-titration blank solutionVolume of sodium hydroxide standard titration solution consumed, ml;
V”0-dividing the volume of the etching solution, ml;
cNaOH-concentration of sodium hydroxide standard solution, mol/L;
d(FeCl3) FeCl in corrosive liquid3The content of (a), g/L;
M(HCl)-molar mass of HCl, g/mol;
M(FeCl3)——FeCl3molar mass of (a), g/mol.
6. The method for analyzing the chemical composition content of the corrosion liquid of the high-temperature alloy as claimed in claim 4 or 5, wherein the ascorbic acid and the Fe3+The theoretical quantitative relationship of (1) is as follows:
m(C6H8O6)=1.57×m(Fe3+) (3)
in the formula (3), m (C)6H8O6)——C6H8O6Molar mass of (a), g/mol.
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Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113670844A (en) * | 2021-09-08 | 2021-11-19 | 中航金属材料理化检测科技有限公司 | Method for detecting content of ferric chloride in high-temperature alloy corrosive liquid |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH02268271A (en) * | 1989-04-10 | 1990-11-01 | Kawasaki Steel Corp | Method and apparatus for quantitative analysis of isolated acid and metal ion in solution |
WO2011064788A1 (en) * | 2009-11-25 | 2011-06-03 | Rajapurkar Mohan M | A method and a kit for detection of acute coronary syndrome based on concentration of unbound iron present in a biological sample |
CN105223200A (en) * | 2014-07-02 | 2016-01-06 | 西安航空动力股份有限公司 | A kind of method of content of hydrochloric acid in Accurate Determining iron chloride etchant solution |
CN105424684A (en) * | 2015-11-03 | 2016-03-23 | 苏州市晶协高新电子材料有限公司 | Method for determining hydrochloric acid and ferric trichloride contents in ITO etching solution |
CN106645117A (en) * | 2016-09-30 | 2017-05-10 | 中国航空工业标准件制造有限责任公司 | Analysis method of cadmium plating bath solution |
CN112179899A (en) * | 2020-10-09 | 2021-01-05 | 蒙自海关综合技术中心 | Method for detecting total iron content in iron ore |
-
2021
- 2021-05-13 CN CN202110519790.4A patent/CN113252660A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH02268271A (en) * | 1989-04-10 | 1990-11-01 | Kawasaki Steel Corp | Method and apparatus for quantitative analysis of isolated acid and metal ion in solution |
WO2011064788A1 (en) * | 2009-11-25 | 2011-06-03 | Rajapurkar Mohan M | A method and a kit for detection of acute coronary syndrome based on concentration of unbound iron present in a biological sample |
CN105223200A (en) * | 2014-07-02 | 2016-01-06 | 西安航空动力股份有限公司 | A kind of method of content of hydrochloric acid in Accurate Determining iron chloride etchant solution |
CN105424684A (en) * | 2015-11-03 | 2016-03-23 | 苏州市晶协高新电子材料有限公司 | Method for determining hydrochloric acid and ferric trichloride contents in ITO etching solution |
CN106645117A (en) * | 2016-09-30 | 2017-05-10 | 中国航空工业标准件制造有限责任公司 | Analysis method of cadmium plating bath solution |
CN112179899A (en) * | 2020-10-09 | 2021-01-05 | 蒙自海关综合技术中心 | Method for detecting total iron content in iron ore |
Non-Patent Citations (4)
Title |
---|
冶金工业部有色金属研究院: "《有机金属合金分析》", 28 February 1981, 北京:冶金工业出版社 * |
吴蠡荪等: "《药品检验操作规范 第2版》", 31 January 2018, 太原:山西科学技术出版社 * |
张勇: "《矿业开采可行性分析研究与开采新模式及矿产品分析试验方法技术标准实用手册 第4卷》", 28 February 2005, 银声音像出版社 * |
盛恩宏: "《普通化学》", 30 September 2020, 安徽师范大学出版社 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113670844A (en) * | 2021-09-08 | 2021-11-19 | 中航金属材料理化检测科技有限公司 | Method for detecting content of ferric chloride in high-temperature alloy corrosive liquid |
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