CN113670844A - Method for detecting content of ferric chloride in high-temperature alloy corrosive liquid - Google Patents
Method for detecting content of ferric chloride in high-temperature alloy corrosive liquid Download PDFInfo
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- 229910021578 Iron(III) chloride Inorganic materials 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000007788 liquid Substances 0.000 title claims abstract description 29
- 239000000956 alloy Substances 0.000 title claims abstract description 21
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 20
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 title claims description 22
- 239000000243 solution Substances 0.000 claims abstract description 151
- 239000012086 standard solution Substances 0.000 claims abstract description 54
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910001447 ferric ion Inorganic materials 0.000 claims abstract description 36
- 238000002835 absorbance Methods 0.000 claims abstract description 34
- 238000001514 detection method Methods 0.000 claims abstract description 33
- 239000011550 stock solution Substances 0.000 claims abstract description 31
- 238000002360 preparation method Methods 0.000 claims abstract description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 141
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 96
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 62
- 238000007865 diluting Methods 0.000 claims description 43
- 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 32
- ZNNZYHKDIALBAK-UHFFFAOYSA-M potassium thiocyanate Chemical compound [K+].[S-]C#N ZNNZYHKDIALBAK-UHFFFAOYSA-M 0.000 claims description 32
- 239000012085 test solution Substances 0.000 claims description 29
- 239000012490 blank solution Substances 0.000 claims description 23
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 18
- 229910052742 iron Inorganic materials 0.000 claims description 18
- 235000010323 ascorbic acid Nutrition 0.000 claims description 16
- 229960005070 ascorbic acid Drugs 0.000 claims description 16
- 239000011668 ascorbic acid Substances 0.000 claims description 16
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 13
- 229910052804 chromium Inorganic materials 0.000 claims description 13
- 239000011651 chromium Substances 0.000 claims description 13
- 229910017052 cobalt Inorganic materials 0.000 claims description 9
- 239000010941 cobalt Substances 0.000 claims description 9
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 9
- 229910052759 nickel Inorganic materials 0.000 claims description 9
- 239000012088 reference solution Substances 0.000 claims description 9
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 8
- 229910052750 molybdenum Inorganic materials 0.000 claims description 8
- 239000011733 molybdenum Substances 0.000 claims description 8
- 229910052720 vanadium Inorganic materials 0.000 claims description 8
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 229910052758 niobium Inorganic materials 0.000 claims description 7
- 239000010955 niobium Substances 0.000 claims description 7
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 7
- 239000003153 chemical reaction reagent Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 238000011161 development Methods 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 230000001502 supplementing effect Effects 0.000 claims description 2
- DKAGJZJALZXOOV-UHFFFAOYSA-N hydrate;hydrochloride Chemical compound O.Cl DKAGJZJALZXOOV-UHFFFAOYSA-N 0.000 claims 1
- 230000035945 sensitivity Effects 0.000 abstract 1
- 238000002156 mixing Methods 0.000 description 26
- 238000012360 testing method Methods 0.000 description 14
- 238000005259 measurement Methods 0.000 description 9
- 238000005260 corrosion Methods 0.000 description 7
- 230000007797 corrosion Effects 0.000 description 7
- DXTCFKRAUYBHRC-UHFFFAOYSA-L iron(2+);dithiocyanate Chemical compound [Fe+2].[S-]C#N.[S-]C#N DXTCFKRAUYBHRC-UHFFFAOYSA-L 0.000 description 7
- 229910000831 Steel Inorganic materials 0.000 description 6
- 239000010959 steel Substances 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- ZMZDMBWJUHKJPS-UHFFFAOYSA-N hydrogen thiocyanate Natural products SC#N ZMZDMBWJUHKJPS-UHFFFAOYSA-N 0.000 description 4
- 229910021645 metal ion Inorganic materials 0.000 description 4
- 238000004448 titration Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- ZMZDMBWJUHKJPS-UHFFFAOYSA-M Thiocyanate anion Chemical compound [S-]C#N ZMZDMBWJUHKJPS-UHFFFAOYSA-M 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 239000003518 caustics Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012776 electronic material Substances 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 2
- 238000002798 spectrophotometry method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910000601 superalloy Inorganic materials 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910001448 ferrous ion Inorganic materials 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 235000019345 sodium thiosulphate Nutrition 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 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
- G01N21/17—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
- 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
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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- 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
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- 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
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- 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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Abstract
The invention discloses FeCl in a high-temperature alloy corrosive liquid3The content detection method is implemented by the following steps: step 1, preparing a simulated solution; step 2, preparation of Fe3+A standard solution; step 3, drawing a standard working curve; step 4, measuring the stock solution, measuring the absorbance, substituting the measured absorbance value of the stock solution into the standard working curve drawn in the step 3, and calculating to obtain FeCl3And (4) content. The invention realizes FeCl in the corrosive liquid sample3And (4) accurately measuring the content. Determination of FeCl by the method of the invention3The sensitivity and stability of the content determination result are optimal.
Description
Technical Field
The invention belongs to the technical field of chemical analysis and detection, and relates to FeCl in a high-temperature alloy corrosive liquid3And (3) a content detection method.
Background
Rough cast or forged superalloys and finish forged superalloys are often used made of FeCl3And performing macroscopic corrosion inspection on the corrosion solution consisting of HCl, wherein the potential of ferric ions in the corrosion solution is higher than that of iron in the alloy, ferric ions oxidize the iron into ferrous ions to be dissolved, and hydrochloric acid inhibits the ferric ionsThe iron is hydrolyzed, so that the passivation layer on the surface of the noble metal such as chromium, nickel and the like is corroded. FeCl in the corrosive liquid along with the increase of the corrosion times3And the HCl content is continuously reduced, the original Fe3+Will be partially converted into Fe2+Meanwhile, a large amount of other metal ions are introduced into the corrosive liquid, the metal ions are increased continuously, and the corrosion effect is reduced, so that the control of the component concentration of the corrosive is particularly critical. In the prior art, a titration method is adopted to determine FeCl in high-temperature alloy corrosive liquid3But because the titration solution has darker color, cations in the corrosion solution are complex, anions are single, and the introduced metal ions give FeCl3The content measurement brings great trouble, the judgment of the end point is seriously influenced, and the detection repeatability is poor.
Disclosure of Invention
The invention aims to provide FeCl in high-temperature alloy corrosive liquid3The method for detecting the content solves the problem of FeCl in the high-temperature alloy corrosive liquid in the prior art3The accuracy of component content detection is poor.
The invention adopts the technical scheme that a method for detecting the content of FeCl3 in high-temperature alloy corrosive liquid is implemented according to the following steps:
step 2, preparation of Fe3+A standard solution;
step 4, measuring the absorbance of the stock solution, substituting the measured absorbance of the stock solution into the standard working curve drawn in the step 3, and calculating to obtain FeCl3And (4) content.
The present invention is also characterized in that,
the step 1 specifically comprises the following steps: step 1.1, 71.6g of FeCl is weighed3·6H2O, adding FeCl36H2O dissolved in hydrochloric acid and water in a volume ratio of 1: 9, and then adding hydrochloric acid and water in a volume ratio of 1: 9 to a 100ml volumetric flask, 430g/L ferric chloride solution was obtained. Taking 1.00ml of 430g/L ferric trichloride solution, putting the solution into a volumetric flask of 1000ml, diluting the solution to the scale with water, shaking up,the obtained solution contains FeCl30.43g/L is the test solution I;
step 1.2, measuring 3.35ml of high-grade pure hydrochloric acid, diluting the high-grade pure hydrochloric acid into a 100ml volumetric flask with water, and shaking up to obtain 39.9g/L hydrochloric acid solution; dividing and taking 10.00ml of 39.9g/L hydrochloric acid solution into a 100ml volumetric flask, diluting the solution to a scale with water, shaking up to obtain a solution containing 3.99g/L hydrochloric acid, namely a test solution II;
step 1.3, preparing a single element interference standard solution; the single element interference standard solution comprises a nickel standard solution, a molybdenum standard solution, a chromium standard solution, a niobium standard solution, a vanadium standard solution and a cobalt standard solution.
The specific steps of the step 2 are as follows: weighing 2.000g of high-purity iron into a 250ml conical flask, and adding 20ml of hydrochloric acid and water in a volume ratio of 1: 9 hydrochloric acid solution, heating and dissolving at low temperature in a flat electric furnace, placing a glass triangular funnel at the opening of the conical flask in the process of relieving heat, taking down the conical flask after high-purity iron is completely dissolved, and dropwise adding H2O2Until brown solution is generated and color is not deepened any more, cooling, transferring into 200ml volumetric flask, diluting to line, shaking to obtain Fe with concentration of 10.0mg/ml3+Standard solution A, adding Fe3+Diluting the standard solution A to the required concentration to obtain Fe3+Standard solution B:
step 3.1, transferring 0.00ml, 1.00ml, 2.00ml, 3.00ml, 4.00ml and 5.00ml of Fe in the step 2 respectively3+The standard solution B is placed in a 6-100 ml volumetric flask, and the volume ratio of hydrochloric acid to water is 1: 4, 20% of KSCN solution and 10% of ascorbic acid solution, respectively supplementing about 10ml of water along the bottle wall by using a washing bottle, and then adding 15.0ml of hydrochloric acid and water in a volume ratio of 1: 4, adding 10.00ml of 20% KSCN solution into hydrochloric acid solution, adding 2.0ml of 10% ascorbic acid solution, shaking uniformly when adding each reagent, finally diluting with water to a scribed line, and shaking uniformly to obtain blank solution;
step 3.2, transferring 0.00ml, 1.00ml, 2.00ml, 3.00ml, 4.00ml and 5.00ml of Fe in the step 2 respectively3+Dropping 1-2 drops of H into 6 100ml volumetric flasks2O2And (3) adding 10ml of water along the bottle wall by using a washing bottle, adding 15.0ml of hydrochloric acid and water according to the volume ratio of 1: 4 hydrochloric acidAdding 10.00ml of 20% KSCN solution into the solution, shaking uniformly when each reagent is added, diluting the solution to a scribed line by water, and shaking uniformly to prepare a color developing solution:
step 3.3, taking the blank solution in the step 3.1 as a reference solution, measuring the absorbance of the color development solution in the step 3.2, and taking Fe3+The mass of (A) is abscissa and the absorbance is ordinate, and a standard working curve is drawn by an absorptiometry.
Step 4.1, dividing the stock solution Vml into 100ml volumetric flasks, adding 10ml of water into the flask wall by using a wash flask, adding 15.0ml of hydrochloric acid and adding water according to the volume ratio of 1: 4, adding 10.00ml of 20% KSCN solution and 2.0ml of 10% ascorbic acid solution, diluting the mixture with water to a scribed line, and shaking up to obtain a stock solution blank solution.
And 4.2, dividing the stock solution Vml into 100ml volumetric flasks, adding about 10ml of water into the flask wall by using a wash bottle, adding 15.0ml of hydrochloric acid and adding water according to the volume ratio of 1: 4, adding 10.00ml of 20 percent KSCN solution, diluting the solution to the scribed line by water, and shaking up to obtain a stock solution color developing solution.
Step 4.3, taking the stock solution blank solution prepared in the step 4.1 as a reference solution and the stock solution developing solution prepared in the step 4.2 as a solution to be detected, measuring the absorbance at 480nm of a spectrophotometer, and checking Fe on the working curve in the step 33+The concentration of FeCl3 was calculated.
FeCl in step 4.33Is passed through
Is calculated to obtain d in the formula(FeCl3)Indicating FeCl3The unit of (a) is g/L grams per liter; m is(Fe3+)Shows that the work curve is searched for Fe3+In mg; m is(FeCl3)Indicating FeCl3The unit of mass of (2) is g; m(FeCl3)Indicating FeCl3The relative molecular mass is 162.5; m(Fe3+)Represents Fe3+The relative atomic mass takes the value 56; v represents the volume of the stock solution to be aliquoted in ml.
In the step 1.2, the mass fraction of the superior grade pure hydrochloric acid is 36-38%, and d is 1.19 g/ml.
And in the step 2, the mass fraction of the high-purity iron is not less than 99.99%.
The invention has the beneficial effects that: the invention adopts thiocyanate and Fe3+The particularity of the reaction to generate the blood red iron thiocyanate avoids the interference of cations in the developing solution, anions do not participate in the reaction, and FeCl is carried out by a spectrophotometry3Detecting the content; realizes the detection of FeCl in the high-temperature alloy corrosive liquid3The content of the sodium hydroxide is not interfered by the dark color of the solution, and the method is simple, convenient, accurate and reliable to operate, can be used for daily detection work, and is worthy of popularization.
Drawings
FIG. 1 is a graph of the absorption of iron thiocyanate at different wavelengths according to example 1 of the present invention;
FIG. 2 is a graph showing stability tests of iron thiocyanate in example 2 of the present invention;
FIG. 3 is a graph showing the results of measurement of the amount of the developer used in example 3 of the present invention;
FIG. 4 is a graph showing the results of measurement of the amount of hydrochloric acid added in example 4 of the present invention;
FIG. 5 is H in example 5 of the present invention202Influence graph of addition amount corresponding to absorbance;
FIG. 6 is a linear range diagram in example 7 of the present invention;
fig. 7 is a linear graph of the operating curve in example 8 of the present invention.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
The FeCl in the high-temperature alloy corrosive liquid3The content detection method is implemented according to the following steps:
step 1.1, 71.6g of FeCl is weighed3·6H2Dissolving FeCl3 & 6H2O in hydrochloric acid and water at a volume ratio of 1: 9, and then adding hydrochloric acid and water in a volume ratio of 1: 9, diluting the hydrochloric acid solution into a 100ml volumetric flask to obtain 430g/L ferric trichloride solution: dividing 430g/L ferric trichloride solution 1.00ml into 1000ml volumetric flasks, diluting with water to scale, shaking up to obtainContaining FeCl3The concentration of the solution is 0.43g/L, namely the test solution I;
step 1.2, measuring 3.35ml of high-grade pure hydrochloric acid, wherein the mass fraction of the high-grade pure hydrochloric acid is 36-38%, and d is 1.19 g/ml; diluting with water to 100ml volumetric flask, shaking up to obtain 39.9g/L hydrochloric acid solution; and (3) dividing 39.9g/L of hydrochloric acid solution 10.00ml into 100ml volumetric flasks, diluting with water to the scale, shaking up to obtain a solution containing 3.99g/L of hydrochloric acid, namely a test solution II.
Step 1.3, preparing a single element interference standard solution; the single element interference standard solution comprises a nickel standard solution, a molybdenum standard solution, a chromium standard solution, a niobium standard solution, a vanadium standard solution and a cobalt standard solution.
Configuring corresponding FeCl3The corrosion solution comprises a hydrochloric acid solution, a single element interference standard solution and a simulated corrosive solution, so that the components of the test solution and the corrosive solution used under the later test condition are consistent, and the test solution I, the test solution II and the single element interference standard solution form the corrosive solution with known chemical component concentration.
Step 2, preparation of Fe3+A standard solution;
the specific steps of the step 2 are as follows: weighing 2.000g of high-purity iron in a 250ml conical flask, wherein the mass fraction of the high-purity iron is not less than 99.99%, and adding 20ml of hydrochloric acid and water in a volume ratio of 1: 9 hydrochloric acid solution, heating and dissolving at low temperature of a flat electric furnace, in order to prevent the acid mist from evaporating too fast, placing a glass triangular funnel at the conical bottle mouth in the process of relieving heat, taking down the glass triangular funnel after the high-purity iron is completely dissolved, and dropwise adding H2O2Until brown solution is generated and color is not deepened any more, cooling, transferring into 200ml volumetric flask, diluting to line, shaking to obtain Fe with concentration of 10.0mg/ml3+Standard solution A, adding Fe3+Diluting the standard solution A to the required concentration to obtain Fe3+Standard solution B:
step 3.1, transferring 0.00ml, 1.00ml, 2.00ml, 3.00ml, 4.00ml and 5.00ml of Fe in the step 2 respectively3+The standard solution B is placed in a 6-100 ml volumetric flask, and the volume ratio of hydrochloric acid to water is 1: 4 hydrochloric acid solution, 20% KSCN solution, 10% ascorbic acid solution, about 10ml water is added along the bottle wall by a washing bottle, and then 15.0ml hydrochloric acid and water are added in a volume ratio of 1: 4, adding 10.00ml of 20% KSCN solution into hydrochloric acid solution, adding 2.0ml of 10% ascorbic acid solution, shaking uniformly when adding each reagent, finally diluting with water to a scribed line, and shaking uniformly to obtain blank solution;
step 3.2, transferring 0.00ml, 1.00ml, 2.00ml, 3.00ml, 4.00ml and 5.00ml of Fe in the step 2 respectively3+Dropping 1-2 drops of H into 6 100ml volumetric flasks2O2And (3) adding 10ml of water along the bottle wall by using a washing bottle, adding 15.0ml of hydrochloric acid and water according to the volume ratio of 1: 4, adding 10.00ml of 20% KSCN solution, shaking up when adding each reagent, diluting the mixture with water to a scribed line, and shaking up to prepare a color developing solution:
step 3.3, taking the blank solution in the step 3.1 as a reference solution, measuring the absorbance of the color development solution in the step 3.2, and taking Fe3+The mass of (A) is abscissa and the absorbance is ordinate, and a standard working curve is drawn by an absorptiometry.
Step 4, measuring the absorbance of the stock solution, substituting the measured absorbance of the stock solution into the standard working curve drawn in the step 3, and calculating to obtain FeCl3And (4) content.
Step 4.1, dividing the stock solution Vml into 100ml volumetric flasks, adding 10ml of water into the flask wall by using a wash flask, adding 15.0ml of hydrochloric acid and adding water according to the volume ratio of 1: 4, adding 10.00ml of 20% KSCN solution and 2.0ml of 10% ascorbic acid solution, diluting the mixture with water to a scribed line, and shaking up to obtain a stock solution blank solution.
And 4.2, dividing the stock solution Vml into 100ml volumetric flasks, adding about 10ml of water into the flask wall by using a wash bottle, adding 15.0ml of hydrochloric acid and adding water according to the volume ratio of 1: 4, adding 10.00ml of 20 percent KSCN solution, diluting the solution to the scribed line by water, and shaking up to obtain a stock solution color developing solution.
Step 4.3, taking the stock solution blank solution prepared in the step 4.1 as a reference solution and the stock solution developing solution prepared in the step 4.2 as a solution to be detected, measuring the absorbance at 480nm of a spectrophotometer, and checking Fe on the working curve in the step 33+The concentration of FeCl3 was calculated.
FeCl in step 4.33Is passed through
Is calculated to obtain d in the formula(FeCl3)Indicating FeCl3The unit of (a) is g/L grams per liter; m is(Fe3+)Shows that the work curve is searched for Fe3+In mg; m is(FeCl3)Indicating FeCl3The unit of mass of (2) is g; m(FeCl3)Indicating FeCl3The relative molecular mass is 162.5; m(Fe3+)Represents Fe3+The relative atomic mass takes the value 56; v represents the volume of the stock solution to be aliquoted in ml.
In the examples, the spectrophotometer used was a UV-2100 type UV/visible spectrophotometer manufactured by Longnike instruments Inc., and the plasma emission spectrometer used was an Optima 5300DV plasma emission spectrometer manufactured by Perkin Elmer, USA.
Example 1
This example analyzes the absorption of iron thiocyanate at different wavelengths
2.00ml of the test solution I is dispensed into a 100ml volumetric flask, 10ml of water is added into the flask by a wash bottle and the flask wall is filled with 15.0ml of hydrochloric acid, and the volume ratio of the water is 1: 4, adding 10.00ml of 20% KSCN solution, adding 2.0ml of 10% ascorbic acid solution, diluting the solution to a scribed line by using water, and shaking up to prepare a blank solution of a test solution I:
2.00ml of the test solution I is dispensed into a 100ml volumetric flask, about 10ml of water is added to the flask wall by means of a wash flask, 15.0ml of 1+4 hydrochloric acid is added, and the volume ratio of water is 1: 4, adding 10.00ml of 20% KSCN solution, diluting the solution to the scribed line with water, and shaking up to prepare a test solution I color developing solution:
the absorbance is measured, the wavelength is used as an abscissa, the absorbance is used as an ordinate, a curve is drawn, as shown in figure 1, and as can be seen from figure 1, the absorption peak of the iron thiocyanate is between 470nm and 485nm, and the peak is preferably 480nm, namely the highest point of the peak in the invention.
Example 2
This example was conducted to test the stability of iron thiocyanate
2.00ml of the test solution I is dispensed into a 100ml volumetric flask, 10ml of water is added into the flask by a wash bottle and the flask wall is filled with 15.0ml of hydrochloric acid, and the volume ratio of the water is 1: 4, adding 10.00ml of 20% KSCN solution, adding 2.0ml of 10% ascorbic acid solution, diluting the solution to a scribed line by using water, and shaking up to prepare a blank solution of a test solution I:
2.00ml of the test solution I is dispensed into a 100ml volumetric flask, about 10ml of water is added to the flask wall by means of a wash flask, 15.0ml of 1+4 hydrochloric acid is added, and the volume ratio of water is 1: 4, adding 10.00ml of 20% KSCN solution, diluting the solution to the scribed line with water, and shaking up to prepare a test solution I color developing solution:
and (3) drawing a curve by taking the developing time as an abscissa and the absorbance as an ordinate, as shown in fig. 2, as can be seen from fig. 2, after ferric ions and thiocyanate radicals generate iron thiocyanate, the absorbance is in a descending trend along with the increase of the standing time, and is stable when the ferric ions and the thiocyanate radicals are placed for 5-20 min, so that the absorbance determination is completed within 20min after the developing is completed.
Example 3
Effect of amount of color developing agent used in the present example on the measurement results
Seven parts of 2.00ml test solution I are respectively taken and placed in seven 100ml volumetric flasks, about 10ml water is added into the flask wall by a wash bottle, 15.0ml hydrochloric acid is added, and the volume ratio of the water is 1: 4, uniformly mixing, respectively and sequentially adding 2.00ml, 4.00ml, 6.00ml, 8.00ml, 10.00ml, 12.00ml and 14.00ml of 20% KSCN solution, uniformly mixing, adding 2.0ml of 10% ascorbic acid solution, diluting to a scribed line by using water, and shaking uniformly to obtain a blank solution of the test solution I;
seven parts of 2.00ml test solution I are respectively taken and placed in seven 100ml volumetric flasks, about 10ml water is added into the flask wall by a wash bottle, 15.0ml hydrochloric acid is added, and the volume ratio of the water is 1: 4, uniformly mixing, respectively and sequentially adding 2.00ml, 4.00ml, 6.00ml, 8.00ml, 10.00ml, 12.00ml and 14.00ml of 20% KSCN solution, uniformly mixing, diluting with water to be scribed, and shaking uniformly to obtain a test solution I developing solution;
the curve is drawn by taking the KSCN addition amount as an abscissa and the absorbance as an ordinate, as shown in FIG. 3, as can be seen from FIG. 3, the addition amount of the 20% KSCN tends to be stable between 8.00ml and 12.00ml, and 10.00ml is preferred in the invention, as the absorbance increases with the increase of the usage amount of the 20% KSCN developer solution.
Example 4
This example analyzes the influence of the amount of hydrochloric acid on the measurement results
Seven parts of 2.00ml test solution I are respectively taken and placed in seven 100ml volumetric flasks, 10ml water is added into the flask wall by a wash flask, and 5.0ml, 8.0ml, 10.0ml, 12.0ml, 15.0ml, 20.0ml, 25.0ml hydrochloric acid and water are respectively added in the volumetric ratio of 1: 4, uniformly mixing, adding 10.00ml of 20% KSCN solution, uniformly mixing, adding 2.0ml of 10% ascorbic acid solution, diluting with water to a scribed line, and shaking uniformly to obtain a blank solution of a test solution I;
seven parts of 2.00ml test solution I are respectively taken and placed in seven 100ml volumetric flasks, 10ml water is added into the flask wall by using a wash flask, and 0.0ml, 5.0ml, 8.0ml, 10.0ml, 12.0ml, 15.0ml, 20.0ml hydrochloric acid and water are respectively added in the volumetric ratio of 1: 4, uniformly mixing, adding 10.00ml of 20% KSCN solution, uniformly mixing, diluting with water to a scribed line, and shaking uniformly to obtain a test solution I color developing solution:
the curve is plotted with the addition of hydrochloric acid as abscissa and the absorbance as ordinate, as shown in fig. 4, which can be seen from fig. 4: the addition amount of the hydrochloric acid is between 5.0ml and 20.0ml, the absorbance tends to be stable, and the invention prefers 15.0 ml.
Example 5
Example H2O2Influence of the amount of addition on the assay results
5 portions of 2.00ml of 0.1mg/ml Fe are divided3+The solution is put into a 6 100ml volumetric flask, about 5ml of water is added to wash the wall of the flask, 15.0ml of hydrochloric acid is added, and the volume ratio of the water to the hydrochloric acid is 1: 4, mixing uniformly, adding 10.00ml of 20% KSCN solution, mixing uniformly, adding 2.0ml of 10% ascorbic acid solution, mixing uniformly, diluting with water to a scribed line, shaking uniformly to obtain a blank solution of a test solution I:
6 portions of 2.00ml of 0.1mg/ml Fe are divided3+The solution is put into 6 100ml volumetric flasks, about 5ml of water is added to wash the walls of the flasks, and the solution is respectively dripped into the 6 100ml volumetric flasksH added with 0d, 1d, 2d, 3d, 4d and 5d2O2Adding about 5ml of water to wash the bottle wall, adding 15.0ml of 1+4 HCl solution, mixing uniformly, adding 10.00ml of 20% KSCN solution, mixing uniformly, diluting with water to a scribed line, shaking uniformly to prepare a test solution I color developing solution:
with H202The amount of addition was plotted on the abscissa and the absorbance on the ordinate, as shown in FIG. 5, from which it can be seen from FIG. 5 that H was added in 1d202Fe can be ensured2+All conversion to Fe3+In the invention, 2d of H is preferably added202。
Example 6
This example was conducted to conduct a coexisting element test
The field corrosive agent is detected by adopting an inductively coupled plasma emission spectrometer, and the corrosive agent mainly contains elements such as chromium, nickel, molybdenum, vanadium, aluminum, titanium, manganese, cobalt and the like. According to the characteristic that thiocyanate reacts with metal ions, the interference test is carried out on elements such as nickel, molybdenum, chromium, niobium, vanadium, cobalt and the like.
Nickel standard solution: 1000. mu.g/ml, Medium C (HNO)3) 1.0mol/L, numbered: 198039-2. national center for analyzing and testing nonferrous metals and electronic materials, 5.00ml of the solution is divided into 100ml volumetric flasks, diluted to the scale and shaken up, and the solution contains 0.05mg/ml of nickel.
Molybdenum standard solution: 1000. mu.g/ml, medium 5% H2SO4Number: 4201. the national iron and steel materials testing center iron and steel research institute, divide and fetch 5.00ml in 100ml volumetric flask, dilute to the scale, shake, this solution contains molybdenum 0.05 mg/ml.
Chromium standard solution: 1000 mug/ml, 5% HCl as medium, 0.1000g high purity chromium (mass fraction: 99.999%) is weighed into 150ml conical flask, 1+1HCl10ml is added, the flask is placed in a low temperature furnace and heated until the chromium is completely dissolved, in order to prevent the acid from evaporating too fast, a glass triangular funnel is placed at the conical flask mouth, the flask is moved into a 100ml volumetric flask, the flask is diluted to scale and shaken up, the solution contains 1mg/ml chromium, 5.00ml chromium standard solution 1000 mug/ml is dispensed into a 100ml volumetric flask, the flask is diluted to scale with water and shaken up, the solution contains 0.05mg/ml chromium.
Niobium standard solution: 1000 μ g/ml, medium 5% HF, No.: 4101. the national iron and steel materials testing center iron and steel research institute, divide and fetch 5.00ml in 100ml plastic volumetric flasks, dilute to the scale, shake, this solution contains niobium 0.05 mg/ml.
Vanadium standard solution: 1000 μ g/ml, medium 10% HCl, No.: 2302. the national iron and steel materials testing center iron and steel research institute. 2.00ml is divided into 200ml volumetric flasks, diluted to the scale and shaken up, and the solution contains 0.01mg/ml vanadium.
Cobalt standard solution: 1000. mu.g/ml, Medium C (HNO)3) 1.0mol/L, numbered: 198010-1, national center for analyzing and testing nonferrous metals and electronic materials, 1.00ml of 1000. mu.g/ml standard cobalt solution is dispensed into a 100ml volumetric flask, diluted to the scale with water and shaken up, and the solution contains 0.01mg/ml cobalt.
Under the test conditions, the content of nickel, molybdenum, chromium, niobium and vanadium in the color development liquid is below 0.25mg, and the content of cobalt is below 50 mu g, so that the measurement is not influenced.
Example 7
Linear range of the present example
0.20mg/ml Fe was separately extracted3+Putting standard solutions B0.00ml, 2.00ml, 4.00ml, 5.00ml, 6.00ml, 7.50ml, 10.00ml, 12.50ml and 15.00ml in 9 100ml volumetric flasks, adding about 10ml of water to the walls of the flasks by using wash bottles, uniformly mixing, adding 15.0ml of 1+4 HCl solution, uniformly mixing, adding 10.00ml of 20% KSCN solution, uniformly mixing, adding 2.0ml of 10% ascorbic acid solution, diluting the mixture with water to a scribed line, and uniformly shaking to obtain a blank solution:
0.20mg/ml Fe was separately extracted3+Standard solution B0.00ml, 2.00ml, 4.00ml, 5.00ml, 6.00ml, 7.50ml, 10.00ml, 12.50ml and 15.00ml is added into a 9-100 ml volumetric flask dropwise with 2 drops of H2O2Adding about 10ml of water into the bottle wall of the bottle by washing the bottle, mixing the solution evenly, adding 15.0ml of 1+4 HCl solution, mixing the solution evenly, adding 10.00ml of 20% KSCN solution, mixing the solution evenly, diluting the solution with water to be scribed, shaking the solution evenly to prepare a color developing solution:
using blank solution as reference solution, measuring absorbance of the chromogenic solution, and using Fe3+Mass of (2) is plotted on the abscissa and absorbance is plotted on the ordinate, as shown in FIG. 6As can be seen in fig. 6: determination of Fe in accordance with the invention3+Linear range of (i.e. Fe in developing solution)3+The amount of Fe is 0.0mg to 2.0mg, and therefore, Fe is measured by the method3+When Fe is controlled in the developing solution3+Within 2.0mg, i.e. FeCl3Control within 5.8 mg.
Example 8
This example was tested for accuracy and precision
12 parts of 2.00ml test solution II are divided into two groups in 12 100ml volumetric flasks, and 2.00ml of 0.1mg/ml Fe is added into 6 volumetric flasks3+Standard solution B, 3.00ml of 0.1mg/ml Fe was added to another set of 6 containers3+And (3) washing the bottle wall with about 5ml of water, uniformly mixing, adding 15.0ml of 1+4 HCl solution, uniformly mixing, adding 10.00ml of 20% KSCN solution, uniformly mixing, adding 2.0ml of 10% ascorbic acid solution, uniformly mixing, diluting with water to a scribed line, and shaking uniformly to obtain a blank solution:
12 parts of 2.00ml test solution II are divided into two groups in 12 100ml volumetric flasks, and 2.00ml of 0.1mg/ml Fe is added into 6 volumetric flasks3+A standard solution was prepared by adding 3.00ml of 0.1mg/ml Fe to another 6 containers3+Standard solution, the walls of the flask were rinsed with about 5ml of water, 2d H was added2O2Mixing, adding 15.0ml of 1+4 HCl solution, mixing, adding 10.00ml of 20% KSCN solution, mixing, diluting with water to a scribed line, and shaking to obtain a color development solution:
using blank solution as reference solution, measuring absorbance of the chromogenic solution, and using Fe3+The mass of (a) is plotted on the abscissa and the absorbance is plotted on the ordinate, as shown in FIG. 7, as can be seen from FIG. 7: the linear coefficient of the working curve is infinitely close to 1, which shows that each parameter of the method is well optimized.
Measuring absorbance of the developing solution with the blank solution as reference solution, measuring absorbance at 480nm, and calculating Fe3+The results are shown in Table 1:
TABLE 1 recovery test results
As can be seen from table 1: fe3+The recovery rate of the catalyst is between 97.5 and 102 percent, and the RSD is 1.2 and 1.4 percent. The accuracy is high, the precision is good, and both the accuracy and the precision can meet the daily detection requirements.
Example 9
Detection Limit and detection Limit tests for the present example
According to the analytical method, the blank solution was measured 10 times in parallel, the standard deviation S was calculated, and the detection limit (3S) and the detection lower limit (10S) of the method were calculated as the standard deviation of 3 times and the standard deviation of 10 times, respectively, and the results are shown in Table 2:
TABLE 2 detection Limit (3S) and detection Limit (10S)
As can be seen from table 2: method for detecting Fe3+The detection limit of (2) was 0.0033mg, and the detection limit was 0.011 mg.
Example 10
FeCl in the high-temperature alloy corrosive liquid of the embodiment3The content detection method is compared with the existing method
By adopting the method respectively, the stock solution is diluted and then is detected, and the same corrosive liquid is detected by a sodium thiosulfate titration method, and the measurement results are shown in a table 3:
table 3 comparison of the methods
According to the detection results in Table 3, it can be seen that 79.5g/L and 79.9g/L of suspicious data measured by the two methods are respectively detected by the Graves detection method, and the detection results show that 79.5g/L and 79.9g/L are both normal values and should be reserved; f distribution test is carried out on the two groups of analysis results, and the variance of the two analysis methods is not significantly different; the two groups of measurement means are consistent through t distribution test.
The above examples are based on the absorption of different wavelengths, the amount of developer, the stability of color developing solution, the amount of hydrochloric acid, and H2O2The interference of dosage and coexisting elements is researched and discussed, and the linear range, accuracy and precision, detection limit and detection lower limit tests are carried out, which show that the method uses a spectrophotometry method to measure FeCl in the high-temperature alloy3The linear coefficient of the content of (1) is more than 0.999; fe3+The detection limit of (1) is 0.0033mg, and the detection lower limit is 0.011 mg; fe3+The recovery rate is between 97.5 and 102 percent, and the RSD is less than 5 percent, which indicates that the method is adopted to measure FeCl in the corrosive liquid3The content of the compound has high accuracy and good precision; the method is suitable for low-content FeCl3Content detection, namely measuring FeCl after separating stock solution3Content of (D), determination of FeCl by titration with sodium thiosulfate3The content of (A) is compared and analyzed: f distribution test is carried out on the detection results of the two methods, and the variance of the two analysis methods is not significantly different; the two groups of measurements were found to be in agreement by t-distribution test. Therefore, the detection range can be expanded by separating the original corrosive liquid, so that the test method is reliable and can be applied to daily detection.
Claims (8)
1. FeCl in high-temperature alloy corrosive liquid3The content detection method is characterized by comprising the following steps:
step 1, preparing a simulated corrosive liquid;
step 2, preparation of Fe3+A standard solution;
step 3, drawing a standard working curve;
step 4, measuring the stock solution, measuring the absorbance, substituting the measured absorbance value of the stock solution into the standard working curve drawn in the step 3, and calculating to obtain FeCl3And (4) content.
2. The method of claim 1, wherein the FeCl in the high-temperature alloy corrosive liquid3The method for detecting the content is characterized in that the step 1 specifically comprises
Step 1.1, 71.6g of FeCl is weighed3·6H2O, adding FeCl36H2O dissolved in hydrochloric acid and water in a volume ratio of 1: 9, and then adding hydrochloric acid and water in a volume ratio of 1: 9, diluting the hydrochloric acid solution into a 100ml volumetric flask to obtain 430g/L ferric trichloride solution: dividing 430g/L ferric trichloride solution 1.00ml into 1000ml volumetric flasks, diluting with water to scale, shaking up to obtain solution containing FeCl30.43g/L is the test solution I;
step 1.2, measuring 3.35ml of high-grade pure hydrochloric acid, diluting the high-grade pure hydrochloric acid into a 100ml volumetric flask with water, and shaking up to obtain 39.9g/L hydrochloric acid solution; dividing and taking 10.00ml of 39.9g/L hydrochloric acid solution into a 100ml volumetric flask, diluting the solution to a scale with water, shaking up to obtain a solution containing 3.99g/L hydrochloric acid, namely a test solution II;
step 1.3, preparing a single element interference standard solution; the single element interference standard solution comprises a nickel standard solution, a molybdenum standard solution, a chromium standard solution, a niobium standard solution, a vanadium standard solution and a cobalt standard solution.
3. The method of claim 1, wherein the FeCl in the high-temperature alloy corrosive liquid3The content detection method is characterized in that the step 2 comprises the following specific steps: weighing 2.000g of high-purity iron into a 250ml conical flask, and adding 20ml of hydrochloric acid and water in a volume ratio of 1: 9 hydrochloric acid solution, heating and dissolving at low temperature in a flat electric furnace, placing a glass triangular funnel at the opening of the conical flask in the process of relieving heat, taking down the conical flask after high-purity iron is completely dissolved, and dropwise adding H2O2Until brown solution is generated and color is not deepened any more, cooling, transferring into 200ml volumetric flask, diluting to line, shaking to obtain Fe with concentration of 10.0mg/ml3+Standard solution A, adding Fe3+Diluting the standard solution A to the required concentration to obtain Fe3+And (4) standard solution B.
4. The method of claim 1, wherein the FeCl in the high-temperature alloy corrosive liquid3The method for detecting the content is characterized in that in the step 3.1, 0.00ml, 1.00ml, 2.00ml, 3.00ml, 4.00ml and 5.00ml of Fe in the step 2 are respectively transferred and taken3+Standard solution B in 6In a 100ml volumetric flask, preparing a hydrochloric acid-water volume ratio of 1: 4, 20% of KSCN solution and 10% of ascorbic acid solution, respectively supplementing about 10ml of water along the bottle wall by using a washing bottle, and then adding 15.0ml of hydrochloric acid and water in a volume ratio of 1: 4, adding 10.00ml of 20% KSCN solution into hydrochloric acid solution, adding 2.0ml of 10% ascorbic acid solution, shaking uniformly when adding each reagent, finally diluting with water to a scribed line, and shaking uniformly to obtain blank solution;
step 3.2, transferring 0.00ml, 1.00ml, 2.00ml, 3.00ml, 4.00ml and 5.00ml of Fe in the step 2 respectively3+Dropping 1-2 drops of H into 6 100ml volumetric flasks2O2And (3) adding 10ml of water along the bottle wall by using a washing bottle, adding 15.0ml of hydrochloric acid and water according to the volume ratio of 1: 4, adding 10.00ml of 20% KSCN solution, shaking up when adding each reagent, diluting the mixture with water to a scribed line, and shaking up to prepare a color developing solution:
step 3.3, taking the blank solution in the step 3.1 as a reference solution, measuring the absorbance of the color development solution in the step 3.2, and taking Fe3+The mass of (A) is abscissa and the absorbance is ordinate, and a standard working curve is drawn by an absorptiometry.
5. The method of claim 1, wherein the FeCl in the high-temperature alloy corrosive liquid3The content detection method is characterized in that in the step 4.1, stock solution Vml is separated into 100ml volumetric flasks, 10ml of water is added into the flask walls through a wash flask, 15.0ml of hydrochloric acid is added, and the volume ratio of the water is 1: 4, adding 10.00ml of 20% KSCN solution and 2.0ml of 10% ascorbic acid solution, diluting the mixture with water to a scribed line, and shaking up to obtain a stock solution blank solution.
And 4.2, dividing the stock solution Vml into 100ml volumetric flasks, adding about 10ml of water into the flask wall by using a wash bottle, adding 15.0ml of hydrochloric acid and adding water according to the volume ratio of 1: 4, adding 10.00ml of 20 percent KSCN solution, diluting the solution to the scribed line by water, and shaking up to obtain a stock solution color developing solution.
Step 4.3, taking the stock solution blank solution prepared in the step 4.1 as a reference solution and the stock solution developing solution prepared in the step 4.2 as a solution to be detected, measuring the absorbance at 480nm of a spectrophotometer, and in the step 3Finding Fe on working curve3+The concentration of FeCl3 was calculated.
6. The method of claim 5, wherein the FeCl in the high-temperature alloy corrosive liquid3The method for detecting the content is characterized in that FeCl is adopted in the step 4.33Is passed through
Is calculated to obtain d in the formula(FeCl3)Indicating FeCl3The unit of (a) is g/L grams per liter; m is(Fe3+)Shows that the work curve is searched for Fe3+In mg; m is(FeCl3)Indicating FeCl3The unit of mass of (2) is g; m(FeCl3)Indicating FeCl3The relative molecular mass is 162.5; m(Fe3+)Represents Fe3+The relative atomic mass takes the value 56; v represents the volume of the stock solution to be aliquoted in ml.
7. The method of claim 2, wherein the FeCl in the high-temperature alloy corrosive liquid3The method for detecting the content is characterized in that the mass fraction of the high-grade pure hydrochloric acid in the step 1.2 is 36-38%, and d is 1.19 g/ml.
8. The method of claim 3, wherein the FeCl in the high-temperature alloy corrosive liquid3The content detection method is characterized in that the mass fraction of the high-purity iron in the step 2 is not less than 99.99%.
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