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CN110346314A - The rapid detection method of micro chromium content in a kind of steel - Google Patents

The rapid detection method of micro chromium content in a kind of steel Download PDF

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Publication number
CN110346314A
CN110346314A CN201910744485.8A CN201910744485A CN110346314A CN 110346314 A CN110346314 A CN 110346314A CN 201910744485 A CN201910744485 A CN 201910744485A CN 110346314 A CN110346314 A CN 110346314A
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Prior art keywords
chromium content
steel
sample
color development
chromium
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Inventor
王岩
孟洋
刘淑影
王莉
郭景喻
郭思维
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Jianlong Beiman Special Steel Co Ltd
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Jianlong Beiman Special Steel Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry

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Abstract

The present invention relates to a kind of rapid detection methods of micro chromium content in steel, belong to chromium content detection method technical field.It is easily splashed and detection time length to emit sulfuric acid cigarette when solving the problems, such as existing national standard method dissolved samples, the present invention provides a kind of rapid detection methods of micro chromium content in steel, draw standard curve including sample treatment, diphenylcarbazide colour developing, with the absorbance of chromium standard solution, measure the absorbance of sample color development treatment liquid and substitute into micro chromium content in standard curve calculating steel.Rapid detection method of the present invention changes dissolved samples method, has both been able to satisfy the accuracy of inspection result, moreover it is possible to eliminate the security risk in detection process;This invention simplifies detecting steps not only to shorten round of visits without filtering, but also saves testing cost.Detection method provided by the invention has preferable stability, is applied to steelmaking technical field, can smelt steel grade standard sample in time for stokehold and carry out definite value, plays the role of for stokehold steel-making guiding.

Description

The rapid detection method of micro chromium content in a kind of steel
Technical field
The invention belongs to a kind of quick detections of micro chromium content in chromium content detection method technical field more particularly to steel Method.
Background technique
Currently, the measuring method of chromium content mainly uses GB/T233.11-2008 " visual titration or electricity in steel and alloy Position titration " " steel and alloy analysis method sodium carbonate separate-diphenylcarbazide luminosity with GB/T233.12-1991 Method measures chromium content ".
The content of chromium, can only survey in GB/T233.11-2008 " visual titration or potentiometric titration " measurement steel and alloy Steel and alloy of the chromium content 0.1% or more are tried, when chromium content is less than 0.1%, test result deviation is larger, and the party The valuableness of reagent price needed for method, complex steps, time are long, and titration end-point is not easy to control.And GB/T233.12-1991 " steel and Alloy analysis method sodium carbonate separation-diphenylcarbazide Spectrophotometric Determination of Chromium amount " sample to be tested dissolution after send out sulfuric acid Cigarette easily splashes, and has not only extended analytical cycle but also has been easy to hurt sb.'s feelings, there are security risks;And potassium permanganate oxygen is separated using sodium carbonate A large amount of precipitatings are generated after change, then are filtered, it is more and sticky due to precipitating, so filter cycle is longer, it is not able to satisfy big life Production demand.
Summary of the invention
It is grown to emit sulfuric acid cigarette when solving the problems, such as existing national standard method dissolved samples and easily splashing with detection time, the present invention mentions A kind of rapid detection method of micro chromium content in steel is supplied.
Technical solution of the present invention:
The rapid detection method of micro chromium content, includes the following steps: in a kind of steel
Step 1: sample treatment:
0.1000-0.2000g sample is weighed, is added what 20mL was prepared according to a certain volume by sulfuric acid, phosphoric acid, nitric acid and water Nitration mixture dissolves by heating sample, sends out film after sample dissolution completely, observe to smolder to remove and be cooled to room temperature system, add Salt in the water-soluble enzymatic hydrolysis system of 50mL, it is in stable aubergine that potassium permanganate to system is added dropwise after system is boiled, and continues to boil It is cooled to room temperature after 2min, system is settled to 100mL and obtains test solution;
Step 2: colour developing:
It takes the conduct point of 10mL test solution to take test solution, the aubergines of 10mL urea, 5~6 drop sodium nitrite to potassium permanganate is added to take off It goes, adds water to 70mL, add 10mL phosphoric acid, 3mL diphenylcarbazide is settled to 100mL with water and shakes even;
Step 3: drawing standard curve:
It pipettes different volumes chromium standard solution to be respectively placed in 100mL volumetric flask, by step 2 operating method to DIFFERENT Cr The standard solution of content carries out color development treatment, then the standard solution of different chromium contents is obtained with water constant volume, to be not added with chromium mark The blank color development treatment liquid of quasi- solution is reference, and the absorbance of each standard solution color development treatment liquid is measured under 540nm wavelength, with The absorbance of each standard solution color development treatment liquid is ordinate, and each standard solution institute's chrome content is abscissa, draws standard curve;
Step 4: calculating micro chromium content in steel:
Using water as reference, measure that treated point takes the extinction of test solution color development treatment liquid through step 2 under 540nm wavelength Degree, while the absorbance of the color development treatment liquid for sample blank reagent of not adding an examination of is measured, divide and the absorbance of test solution color development treatment liquid is taken to subtract The absorbance resulting value of color development treatment liquid of sample blank reagent of going not add an examination of substitutes into the standard curve that step 3 is drawn, and is calculated The chromium content of sample.
Further, the volume ratio of sulfuric acid, phosphoric acid described in step 1, nitric acid and water is 4:3:1:23;The wherein sulfuric acid Mass concentration be 1.84g/mL, the mass concentration of phosphoric acid is 1.69g/mL, and the mass concentration of nitric acid is 1.42g/mL.
Further, the mass concentration of potassium permanganate described in step 1 is 40g/L.
Further, the mass concentration of urea described in step 2 is 50g/L, and the mass concentration of the sodium nitrite is 5g/ L。
Further, the volumetric concentration of phosphoric acid described in step 2 is 50%;The mass concentration of the diphenylcarbazide is 2.5g/L。
Further, the concentration of chromium standard solution described in step 3 is 2 μ g/mL.
Further, chromium standard solution described in step 3 be added volumetric flask amount be respectively as follows: 1.00mL, 2.00mL, 4.00mL, 7.00mL and 10.00mL.
Further, the chromium content detection range of standard curve described in step 3 is 0.005%~0.5%.
Further, the calculation formula of chromium content described in step 4 are as follows: Cr%=[(m1×V)/(m×V1)]×100;Formula In: m1: the chromium content checked in from standard curve, g;M: sample size, g;V: test solution total volume, mL;V1: divide and takes test solution volume, mL.
Beneficial effects of the present invention:
The rapid detection method of micro chromium content changes dissolved samples method in a kind of steel provided by the invention, is both able to satisfy The accuracy of inspection result, moreover it is possible to eliminate the security risk in detection process;With constant volume after potassium permanganate oxidation, sodium carbonate is not had to Separation, does not precipitate generation, without filtering, not only shortens round of visits, but also save testing cost.
Detection method provided by the invention has preferable stability, using standard sample as analysis sample and standard value It compares, within the scope of tolerance, greatly shortens detection cycle, micro addition chromium content is in 0.005%-0.5% in completion steel Quick analysis, can in time for stokehold smelt steel grade standard sample carry out definite value, for stokehold steel-making play the role of it is guiding.
Detailed description of the invention
Fig. 1 is the standard curve that embodiment 5- embodiment 8 is drawn according to the chromium content and absorbance of chromium standard solution.
Specific embodiment
Below with reference to embodiment, the following further describes the technical solution of the present invention, and however, it is not limited to this, all right Technical solution of the present invention is modified or replaced equivalently, and without departing from the spirit and scope of the technical solution of the present invention, should all be contained Lid is within the protection scope of the present invention.
Embodiment 1
The rapid detection method of micro chromium content, includes the following steps: in a kind of steel
Step 1: sample treatment:
0.1000-0.2000g sample is weighed, is added what 20mL was prepared according to a certain volume by sulfuric acid, phosphoric acid, nitric acid and water Nitration mixture dissolves by heating sample, sends out film after sample dissolution completely, observe to smolder to remove and be cooled to room temperature system, add Salt in the water-soluble enzymatic hydrolysis system of 50mL, it is in stable aubergine that potassium permanganate to system is added dropwise after system is boiled, and continues to boil It is cooled to room temperature after 2min, system is settled to 100mL and obtains test solution;
Step 2: colour developing:
It takes the conduct point of 10mL test solution to take test solution, the aubergines of 10mL urea, 5~6 drop sodium nitrite to potassium permanganate is added to take off It goes, adds water to 70mL, add 10mL phosphoric acid, 3mL diphenylcarbazide is settled to 100mL with water and shakes even;
Step 3: drawing standard curve:
It pipettes different volumes chromium standard solution to be respectively placed in 100mL volumetric flask, by step 2 operating method to DIFFERENT Cr The standard solution of content carries out color development treatment, then the standard solution of different chromium contents is obtained with water constant volume, to be not added with chromium mark The blank color development treatment liquid of quasi- solution is reference, and the absorbance of each standard solution color development treatment liquid is measured under 540nm wavelength, with The absorbance of each standard solution color development treatment liquid is ordinate, and each standard solution institute's chrome content is abscissa, draws standard curve;
Step 4: calculating micro chromium content in steel:
Using water as reference, measure that treated point takes the extinction of test solution color development treatment liquid through step 2 under 540nm wavelength Degree, while the absorbance of the color development treatment liquid for sample blank reagent of not adding an examination of is measured, divide and the absorbance of test solution color development treatment liquid is taken to subtract The absorbance resulting value of color development treatment liquid of sample blank reagent of going not add an examination of substitutes into the standard curve that step 3 is drawn, and is calculated The chromium content of sample.
Embodiment 2
The rapid detection method of micro chromium content, includes the following steps: in a kind of steel
Step 1: sample treatment:
It weighs 0.1000-0.2000g sample to be placed in 250mL conical flask, it is 1.84g/mL that 20mL, which is added, by mass concentration Sulfuric acid, mass concentration be 1.69g/mL phosphoric acid, mass concentration be 1.42g/mL nitric acid and water 4:3:1:23 by volume The nitration mixture of preparation, being heated to 40~90 DEG C makes dissolved samples, sends out film after sample dissolution completely, observes to smolder and remove body System is cooled to room temperature, and adds the salt in the water-soluble enzymatic hydrolysis system of 50mL, and potassium permanganate is added dropwise after system is boiled to system in stable Aubergine continues to be cooled to room temperature after boiling 2min, system is settled to 100mL and obtains test solution;
Step 2: colour developing:
It takes the conduct point of 10mL test solution to take test solution, the aubergines of 10mL urea, 5~6 drop sodium nitrite to potassium permanganate is added to take off It goes, adds water to 70mL, add 10mL phosphoric acid, 3mL diphenylcarbazide is settled to 100mL with water and shakes even;
Step 3: drawing standard curve:
It pipettes different volumes chromium standard solution to be respectively placed in 100mL volumetric flask, by step 2 operating method to DIFFERENT Cr The standard solution of content carries out color development treatment, then the standard solution of different chromium contents is obtained with water constant volume, to be not added with chromium mark The blank color development treatment liquid of quasi- solution is reference, and the absorbance of each standard solution color development treatment liquid is measured under 540nm wavelength, with The absorbance of each standard solution color development treatment liquid is ordinate, and each standard solution institute's chrome content is abscissa, draws standard curve;
Step 4: calculating micro chromium content in steel:
Using water as reference, measure that treated point takes the extinction of test solution color development treatment liquid through step 2 under 540nm wavelength Degree, while the absorbance of the color development treatment liquid for sample blank reagent of not adding an examination of is measured, divide and the absorbance of test solution color development treatment liquid is taken to subtract The absorbance resulting value of color development treatment liquid of sample blank reagent of going not add an examination of substitutes into the standard curve that step 3 is drawn, and is calculated The chromium content of sample.
Hair sulfuric acid cigarette is changed to hair phosphoric acid cigarette in the case where not impact analysis result by the present embodiment, solves security risk, With constant volume after potassium permanganate oxidation, do not have to sodium carbonate and separate, do not precipitate generation, without filtering, guarantees result accuracy Under the conditions of not only shorten round of visits, but also save inspection cost.Since ingredient is single in general steel, noiseless element, therefore this implementation Also the requirement of analysis precision is able to satisfy while example Simplified analysis step.
Embodiment 3
The rapid detection method of micro chromium content, includes the following steps: in a kind of steel
Step 1: sample treatment:
It weighs 0.1000-0.2000g sample to be placed in 250mL conical flask, it is 1.84g/mL that 20mL, which is added, by mass concentration Sulfuric acid, mass concentration be 1.69g/mL phosphoric acid, mass concentration be 1.42g/mL nitric acid and water 4:3:1:23 by volume The nitration mixture of preparation, being heated to 40~90 DEG C makes dissolved samples, sends out film after sample dissolution completely, observes to smolder and remove body System is cooled to room temperature, and adds the salt in the water-soluble enzymatic hydrolysis system of 50mL, and the permanganic acid that mass concentration is 40g/L is added dropwise after system is boiled Potassium to system is in stable aubergine, continues to be cooled to room temperature after boiling 2min, system is settled to 100mL and obtains test solution;
Step 2: colour developing:
It takes 10mL test solution as point test solution is taken, adds the drop mass concentration of urea, 5~6 that 10mL mass concentration is 50g/L to be The aubergine of the sodium nitrite of 5g/L to potassium permanganate is taken off, and 70mL is added water to, and adding 10mL volumetric concentration is 50% phosphoric acid, 3mL mass concentration is the diphenylcarbazide of 2.5g/L, is settled to 100mL with water and shakes even;
Step 3: drawing standard curve:
It pipettes different volumes chromium standard solution to be respectively placed in 100mL volumetric flask, by step 2 operating method to DIFFERENT Cr The standard solution of content carries out color development treatment, then the standard solution of different chromium contents is obtained with water constant volume, to be not added with chromium mark The blank color development treatment liquid of quasi- solution is reference, and the absorbance of each standard solution color development treatment liquid is measured under 540nm wavelength, with The absorbance of each standard solution color development treatment liquid is ordinate, and each standard solution institute's chrome content is abscissa, draws standard curve;
Step 4: calculating micro chromium content in steel:
Using water as reference, measure that treated point takes the extinction of test solution color development treatment liquid through step 2 under 540nm wavelength Degree, while the absorbance of the color development treatment liquid for sample blank reagent of not adding an examination of is measured, divide and the absorbance of test solution color development treatment liquid is taken to subtract The absorbance resulting value of color development treatment liquid of sample blank reagent of going not add an examination of substitutes into the standard curve that step 3 is drawn, and is calculated The chromium content of sample.
Embodiment 4
The rapid detection method of micro chromium content, includes the following steps: in a kind of steel
Step 1: sample treatment:
It weighs 0.1000-0.2000g sample to be placed in 250mL conical flask, it is 1.84g/mL that 20mL, which is added, by mass concentration Sulfuric acid, the phosphoric acid that mass concentration is 1.69g/mL, the nitric acid that mass concentration is 1.42 g/mL and water 4:3:1 by volume: 23 nitration mixture prepared, being heated to 40~90 DEG C makes dissolved samples, sends out film after sample dissolution completely, observe smolder remove by System is cooled to room temperature, and adds the salt in the water-soluble enzymatic hydrolysis system of 50mL, and the Gao Meng that mass concentration is 40g/L is added dropwise after system is boiled Sour potassium to system is in stable aubergine, continues to be cooled to room temperature after boiling 2min, system is settled to 100mL and obtains test solution;
Step 2: colour developing:
It takes 10mL test solution as point test solution is taken, adds the drop mass concentration of urea, 5~6 that 10mL mass concentration is 50g/L to be The aubergine of the sodium nitrite of 5g/L to potassium permanganate is taken off, and 70mL is added water to, and adding 10mL volumetric concentration is 50% phosphoric acid, 3mL mass concentration is the diphenylcarbazide of 2.5g/L, is settled to 100mL with water and shakes even;
Step 3: drawing standard curve:
It prepares chromium standard solution: weighing 0.2829g and moved into after 150 DEG C of potassium bichromates that drying to constant weight are dissolved in water in advance In 1000mL volumetric flask, the mother liquor of 100 μ g/mL is obtained with water constant volume;20mL mother liquor is taken to be placed in 1000mL volumetric flask, it is fixed with water Appearance obtains the chromium standard solution of 2 μ g/mL.
It pipettes 1.00mL, 2.00mL, 4.00mL, 7.00mL and 10.00mL chromium standard solution and is respectively placed in 100mL volumetric flask In, color development treatment is carried out by standard solution of the step 2 operating method to different chromium contents, DIFFERENT Cr is then obtained with water constant volume The standard solution of content measures each mark using the blank color development treatment liquid for being not added with chromium standard solution as reference under 540nm wavelength The absorbance of quasi- test solution color development treatment liquid, using the absorbance of each standard solution color development treatment liquid as ordinate, each standard solution institute Chrome content is abscissa, draws standard curve, and the chromium content detection range of the standard curve is 0.005%~0.5%;
Step 4: calculating micro chromium content in steel:
Using water as reference, measure that treated point takes the extinction of test solution color development treatment liquid through step 2 under 540nm wavelength Degree, while the absorbance of the color development treatment liquid for sample blank reagent of not adding an examination of is measured, divide and the absorbance of test solution color development treatment liquid is taken to subtract The absorbance resulting value of color development treatment liquid of sample blank reagent of going not add an examination of substitutes into the standard curve that step 3 is drawn, and is calculated The chromium content of sample.
Embodiment 5
The rapid detection method of micro chromium content, includes the following steps: in a kind of steel
Step 1: sample treatment:
It weighs 0.1000-0.2000g sample to be placed in 250mL conical flask, it is 1.84g/mL that 20mL, which is added, by mass concentration Sulfuric acid, the phosphoric acid that mass concentration is 1.69g/mL, the nitric acid that mass concentration is 1.42 g/mL and water 4:3:1 by volume: 23 nitration mixture prepared, being heated to 40~90 DEG C makes dissolved samples, sends out film after sample dissolution completely, observe smolder remove by System is cooled to room temperature, and adds the salt in the water-soluble enzymatic hydrolysis system of 50mL, and the Gao Meng that mass concentration is 40g/L is added dropwise after system is boiled Sour potassium to system is in stable aubergine, continues to be cooled to room temperature after boiling 2min, system is settled to 100mL and obtains test solution;
Step 2: colour developing:
It takes 10mL test solution as point test solution is taken, adds the drop mass concentration of urea, 5~6 that 10mL mass concentration is 50g/L to be The aubergine of the sodium nitrite of 5g/L to potassium permanganate is taken off, and 70mL is added water to, and adding 10mL volumetric concentration is 50% phosphoric acid, 3mL mass concentration is the diphenylcarbazide of 2.5g/L, is settled to 100mL with water and shakes even;
Step 3: drawing standard curve:
It prepares chromium standard solution: weighing 0.2829g and moved into after 150 DEG C of potassium bichromates that drying to constant weight are dissolved in water in advance In 1000mL volumetric flask, the mother liquor of 100 μ g/mL is obtained with water constant volume;20mL mother liquor is taken to be placed in 1000mL volumetric flask, it is fixed with water Appearance obtains the chromium standard solution of 2 μ g/mL.
It pipettes 1.00mL, 2.00mL, 4.00mL, 7.00mL and 10.00mL chromium standard solution and is respectively placed in 100mL volumetric flask In, color development treatment is carried out by standard solution of the step 2 operating method to different chromium contents, DIFFERENT Cr is then obtained with water constant volume The standard solution of content measures each mark using the blank color development treatment liquid for being not added with chromium standard solution as reference under 540nm wavelength The absorbance of quasi- test solution color development treatment liquid, using the absorbance of each standard solution color development treatment liquid as ordinate, each standard solution institute Chrome content is abscissa, draw standard curve as shown in Figure 1, the chromium content detection range of the standard curve is 0.005%~ 0.5%;
Step 4: calculating micro chromium content in steel:
Using water as reference, measure that treated point takes the extinction of test solution color development treatment liquid through step 2 under 540nm wavelength Degree, while the absorbance of the color development treatment liquid for sample blank reagent of not adding an examination of is measured, divide and the absorbance of test solution color development treatment liquid is taken to subtract The absorbance resulting value of color development treatment liquid of sample blank reagent of going not add an examination of substitutes into the standard curve that step 3 is drawn and obtains point taking Institute's chrome content in test solution, the chromium content of sample is calculated with following formula:
Cr%=[(m1×V)/(m×V1)]×100;In formula:
m1: the chromium content checked in from standard curve, g;
M: sample size, g;
V: test solution total volume, mL;
V1: divide and takes test solution volume, mL.
The tolerance of the present embodiment detection method:
Repeatability limit r:lgr=-1.5589+0.6552lgm
Reproducibility limits R:lgR=-1.3721+0.6245lgm
M is the average value of two measured values, % in formula.
Under the conditions of repeatability, the absolute difference of the result of independent test twice of acquisition is not more than repeatability limit (r).
Under the conditions of reproducibility, the absolute difference of the result of independent test twice of acquisition is no more than repeatability limit (R).
Detection method provided in this embodiment is compared as analysis sample with standard value using standard sample, in tolerance model In enclosing, round of visits is greatly shortened, test of many times confirms that detection method provided in this embodiment has preferable stability.
Embodiment 6
The rapid detection method for present embodiments providing micro chromium content in a kind of steel grade 15MnTi, includes the following steps:
Step 1: sample treatment:
Steel grade 15MnTi sample is drilled through, sample position surface polishing treatment should be subjected to before drilling through, prevent iron oxide Skin enters in sample;Sample after drilling through, it is desirable that for it is oil-free, anhydrous, without decarburization, uniform strip crumbs shape.
0.1000g sample is weighed to be placed in 250mL conical flask, be added 20mL by mass concentration be 1.84g/mL sulfuric acid, 4:3:1:23 is prepared phosphoric acid, the nitric acid that mass concentration is 1.42 g/mL and the water that mass concentration is 1.69g/mL by volume Nitration mixture, being heated to 40 DEG C makes dissolved samples, sends out film after sample dissolution completely, observes to smolder to remove system is cooled to room Temperature adds the salt in the water-soluble enzymatic hydrolysis system of 50mL, and potassium permanganate to the system that mass concentration is 40g/L is added dropwise after system is boiled and is in Stable aubergine continues to be cooled to room temperature after boiling 2min, system is settled to 100mL and obtains test solution;
Step 2: colour developing:
The conduct point of 10mL test solution is taken to take test solution, adding the drop mass concentration of urea, 6 that 10mL mass concentration is 50g/L is 5g/L The aubergine of sodium nitrite to potassium permanganate take off, add water to 70mL, adding 10mL volumetric concentration is 50% phosphoric acid, 3mL matter The diphenylcarbazide that concentration is 2.5g/L is measured, 100mL is settled to water and is shaken even;
Step 3: drawing standard curve:
It prepares chromium standard solution: weighing 0.2829g and moved into after 150 DEG C of potassium bichromates that drying to constant weight are dissolved in water in advance In 1000mL volumetric flask, the mother liquor of 100 μ g/mL is obtained with water constant volume;20mL mother liquor is taken to be placed in 1000mL volumetric flask, it is fixed with water Appearance obtains the chromium standard solution of 2 μ g/mL.
It pipettes 1.00mL, 2.00mL, 4.00mL, 7.00mL and 10.00mL chromium standard solution and is respectively placed in 100mL volumetric flask In, color development treatment is carried out by standard solution of the step 2 operating method to different chromium contents, DIFFERENT Cr is then obtained with water constant volume The standard solution of content measures each mark using the blank color development treatment liquid for being not added with chromium standard solution as reference under 540nm wavelength The absorbance of quasi- test solution color development treatment liquid, using the absorbance of each standard solution color development treatment liquid as ordinate, each standard solution institute Chrome content is abscissa, draw standard curve as shown in Figure 1, the standard curve chromium content detection range be 0.005%~ 0.5%;
Step 4: calculating micro chromium content in steel:
Using water as reference, measure that treated point takes the extinction of test solution color development treatment liquid through step 2 under 540nm wavelength Degree, while the absorbance of the color development treatment liquid for sample blank reagent of not adding an examination of is measured, divide and the absorbance of test solution color development treatment liquid is taken to subtract The absorbance resulting value of color development treatment liquid of sample blank reagent of going not add an examination of is 0.294, is substituted into the standard that step 3 is drawn It is 10.6 μ g that curve, which obtains point taking institute's chrome content in test solution, and the chromium content of sample is calculated with following formula:
Cr%=[(m1×V)/(m×V1)]×100;In formula:
m1: the chromium content checked in from standard curve, g;
M: sample size, g;
V: test solution total volume, mL;
V1: divide and takes test solution volume, mL.
Cr%=[(m1×V)/(m×V1)] × 100=10.6 × 10-6× 100mL/0.1000g × 10mL= 0.106%.
Embodiment 7
The rapid detection method for present embodiments providing micro chromium content in a kind of steel grade boron steel, includes the following steps:
Step 1: sample treatment:
Steel grade boron steel sample is drilled through, sample position surface polishing treatment should be subjected to before drilling through, prevent iron scale Into in sample;Sample after drilling through, it is desirable that for it is oil-free, anhydrous, without decarburization, uniform strip crumbs shape.
0.1000g sample is weighed to be placed in 250mL conical flask, be added 20mL by mass concentration be 1.84g/mL sulfuric acid, 4:3:1:23 is prepared phosphoric acid, the nitric acid that mass concentration is 1.42 g/mL and the water that mass concentration is 1.69g/mL by volume Nitration mixture, being heated to 40 DEG C makes dissolved samples, sends out film after sample dissolution completely, observes to smolder to remove system is cooled to room Temperature adds the salt in the water-soluble enzymatic hydrolysis system of 50mL, and potassium permanganate to the system that mass concentration is 40g/L is added dropwise after system is boiled and is in Stable aubergine continues to be cooled to room temperature after boiling 2min, system is settled to 100mL and obtains test solution;
Step 2: colour developing:
The conduct point of 10mL test solution is taken to take test solution, adding the drop mass concentration of urea, 6 that 10mL mass concentration is 50g/L is 5g/L The aubergine of sodium nitrite to potassium permanganate take off, add water to 70mL, adding 10mL volumetric concentration is 50% phosphoric acid, 3mL matter The diphenylcarbazide that concentration is 2.5g/L is measured, 100mL is settled to water and is shaken even;
Step 3: drawing standard curve:
It prepares chromium standard solution: weighing 0.2829g and moved into after 150 DEG C of potassium bichromates that drying to constant weight are dissolved in water in advance In 1000mL volumetric flask, the mother liquor of 100 μ g/mL is obtained with water constant volume;20mL mother liquor is taken to be placed in 1000mL volumetric flask, it is fixed with water Appearance obtains the chromium standard solution of 2 μ g/mL.
It pipettes 1.00mL, 2.00mL, 4.00mL, 7.00mL and 10.00mL chromium standard solution and is respectively placed in 100mL volumetric flask In, color development treatment is carried out by standard solution of the step 2 operating method to different chromium contents, DIFFERENT Cr is then obtained with water constant volume The standard solution of content measures each mark using the blank color development treatment liquid for being not added with chromium standard solution as reference under 540nm wavelength The absorbance of quasi- test solution color development treatment liquid, using the absorbance of each standard solution color development treatment liquid as ordinate, each standard solution institute Chrome content is abscissa, draw standard curve as shown in Figure 1, the standard curve chromium content detection range be 0.005%~ 0.5%;
Step 4: calculating micro chromium content in steel:
Using water as reference, measure that treated point takes the extinction of test solution color development treatment liquid through step 2 under 540nm wavelength Degree, while the absorbance of the color development treatment liquid for sample blank reagent of not adding an examination of is measured, divide and the absorbance of test solution color development treatment liquid is taken to subtract The absorbance resulting value of color development treatment liquid of sample blank reagent of going not add an examination of is 0.408, is substituted into the standard that step 3 is drawn It is 14.9 μ g that curve, which obtains point taking institute's chrome content in test solution, and the chromium content of sample is calculated with following formula:
Cr%=[(m1×V)/(m×V1)]×100;In formula:
m1: the chromium content checked in from standard curve, g;
M: sample size, g;
V: test solution total volume, mL;
V1: divide and takes test solution volume, mL.
Cr%=[(m1×V)/(m×V1)] × 100=14.9 × 10-6× 100mL/0.1000 × 10mL=0.149%.
Embodiment 8
A kind of rapid detection method of micro chromium content in steel grade carbon colorimetric steel is present embodiments provided, including is walked as follows It is rapid:
Step 1: sample treatment:
Steel grade carbon colorimetric steel curved beam is drilled through, sample position should be subjected to surface polishing treatment, anti-block before drilling through Change iron sheet to enter in sample;Sample after drilling through, it is desirable that for it is oil-free, anhydrous, without decarburization, uniform strip crumbs shape.
0.1000g sample is weighed to be placed in 250mL conical flask, be added 20mL by mass concentration be 1.84g/mL sulfuric acid, 4:3:1:23 is prepared phosphoric acid, the nitric acid that mass concentration is 1.42 g/mL and the water that mass concentration is 1.69g/mL by volume Nitration mixture, being heated to 40 DEG C makes dissolved samples, sends out film after sample dissolution completely, observes to smolder to remove system is cooled to room Temperature adds the salt in the water-soluble enzymatic hydrolysis system of 50mL, and potassium permanganate to the system that mass concentration is 40g/L is added dropwise after system is boiled and is in Stable aubergine continues to be cooled to room temperature after boiling 2min, system is settled to 100mL and obtains test solution;
Step 2: colour developing:
The conduct point of 10mL test solution is taken to take test solution, adding the drop mass concentration of urea, 6 that 10mL mass concentration is 50g/L is 5g/L The aubergine of sodium nitrite to potassium permanganate take off, add water to 70mL, adding 10mL volumetric concentration is 50% phosphoric acid, 3mL matter The diphenylcarbazide that concentration is 2.5g/L is measured, 100mL is settled to water and is shaken even;
Step 3: drawing standard curve:
It prepares chromium standard solution: weighing 0.2829g and moved into after 150 DEG C of potassium bichromates that drying to constant weight are dissolved in water in advance In 1000mL volumetric flask, the mother liquor of 100 μ g/mL is obtained with water constant volume;20mL mother liquor is taken to be placed in 1000mL volumetric flask, it is fixed with water Appearance obtains the chromium standard solution of 2 μ g/mL.
It pipettes 1.00mL, 2.00mL, 4.00mL, 7.00mL and 10.00mL chromium standard solution and is respectively placed in 100mL volumetric flask In, color development treatment is carried out by standard solution of the step 2 operating method to different chromium contents, DIFFERENT Cr is then obtained with water constant volume The standard solution of content measures each mark using the blank color development treatment liquid for being not added with chromium standard solution as reference under 540nm wavelength The absorbance of quasi- test solution color development treatment liquid, using the absorbance of each standard solution color development treatment liquid as ordinate, each standard solution institute Chrome content is abscissa, draw standard curve as shown in Figure 1, the standard curve chromium content detection range be 0.005%~ 0.5%;
Step 4: calculating micro chromium content in steel:
Using water as reference, measure that treated point takes the extinction of test solution color development treatment liquid through step 2 under 540nm wavelength Degree, while the absorbance of the color development treatment liquid for sample blank reagent of not adding an examination of is measured, divide and the absorbance of test solution color development treatment liquid is taken to subtract The absorbance resulting value of color development treatment liquid of sample blank reagent of going not add an examination of is 0.270, is substituted into the standard that step 3 is drawn It is 9.7 μ g that curve, which obtains point taking institute's chrome content in test solution, and the chromium content of sample is calculated with following formula:
Cr%=[(m1×V)/(m×V1)]×100;In formula:
m1: the chromium content checked in from standard curve, g;
M: sample size, g;
V: test solution total volume, mL;
V1: divide and takes test solution volume, mL.
Cr%=[(m1×V)/(m×V1)] × 100=9.7 × 10-6× 100mL/0.1000g × 10mL=0.097%.
The accuracy comparing result of the rapid detection method of micro chromium content is as shown in table 1 in embodiment 6-8 steel:
Table 1
Number Steel grade Standard value % Assay value % Difference % National standard allows reproducibility Accuracy
Embodiment 6 15MnTi 0.100 0.106 0.006 0.0101 It is qualified
Embodiment 7 Boron steel 0.156 0.149 0.007 0.0131 It is qualified
Embodiment 8 Carbon colorimetric steel 0.093 0.097 0.004 0.0096 It is qualified
It can be seen from 1 comparing result of table in steel provided by the invention the rapid detection method of micro chromium content for not With the detection accuracy all with higher and reproducibility of trace chromium in steel grade, it is applied to steelmaking technical field, Neng Gouji When be accurately stokehold smelt steel grade standard sample carry out definite value, for stokehold steel-making play the role of it is guiding.

Claims (9)

1. the rapid detection method of micro chromium content in a kind of steel, which comprises the steps of:
Step 1: sample treatment:
0.1000-0.2000g sample is weighed, 20mL is added and is mixed by what sulfuric acid, phosphoric acid, nitric acid and water were prepared according to a certain volume Acid dissolves by heating sample, sends out film after sample dissolution completely, observe to smolder to remove and be cooled to room temperature system, add 50mL Salt in water-soluble enzymatic hydrolysis system, it is in stable aubergine that potassium permanganate to system is added dropwise after system is boiled, and continues to boil 2min After be cooled to room temperature, system is settled to 100mL and obtains test solution;
Step 2: colour developing:
It takes the conduct point of 10mL test solution to take test solution, adds the aubergines of 10mL urea, 5~6 drop sodium nitrite to potassium permanganate to take off, add Water adds 10mL phosphoric acid, 3mL diphenylcarbazide is settled to 100mL with water and shakes even to 70mL;
Step 3: drawing standard curve:
It pipettes different volumes chromium standard solution to be respectively placed in 100mL volumetric flask, by step 2 operating method to different chromium contents Standard solution carry out color development treatment, the standard solution of different chromium contents is then obtained with water constant volume, it is molten to be not added with chromium standard The blank color development treatment liquid of liquid is reference, measures the absorbance of each standard solution color development treatment liquid, under 540nm wavelength with each mark The absorbance of quasi- test solution color development treatment liquid is ordinate, and each standard solution institute's chrome content is abscissa, draws standard curve;
Step 4: calculating micro chromium content in steel:
Using water as reference, measure that treated point takes the absorbance of test solution color development treatment liquid through step 2 under 540nm wavelength, together When measurement do not add an examination of sample blank reagent color development treatment liquid absorbance, point take the absorbance of test solution color development treatment liquid subtract plus The absorbance resulting value of the color development treatment liquid of sample blank reagent substitutes into the standard curve that step 3 is drawn, and sample is calculated Chromium content.
2. according to claim 1 in a kind of steel micro chromium content rapid detection method, which is characterized in that described in step 1 Sulfuric acid, phosphoric acid, nitric acid and water volume ratio be 4:3:1:23;Wherein the mass concentration of the sulfuric acid is 1.84g/mL, phosphoric acid Mass concentration is 1.69g/mL, and the mass concentration of nitric acid is 1.42g/mL.
3. the rapid detection method of micro chromium content in a kind of steel according to claim 1 or claim 2, which is characterized in that step 1 The mass concentration of the potassium permanganate is 40g/L.
4. according to claim 3 in a kind of steel micro chromium content rapid detection method, which is characterized in that described in step 2 The mass concentration of urea is 50g/L, and the mass concentration of the sodium nitrite is 5g/L.
5. according to claim 4 in a kind of steel micro chromium content rapid detection method, which is characterized in that described in step 2 The volumetric concentration of phosphoric acid is 50%;The mass concentration of the diphenylcarbazide is 2.5g/L.
6. according to claim 5 in a kind of steel micro chromium content rapid detection method, which is characterized in that described in step 3 The concentration of chromium standard solution is 2 μ g/mL.
7. according to claim 6 in a kind of steel micro chromium content rapid detection method, which is characterized in that described in step 3 The amount that volumetric flask is added in chromium standard solution is respectively as follows: 1.00mL, 2.00mL, 4.00mL, 7.00mL and 10.00mL.
8. according to claim 7 in a kind of steel micro chromium content rapid detection method, which is characterized in that described in step 3 The chromium content detection range of standard curve is 0.005%~0.5%.
9. according to claim 8 in a kind of steel micro chromium content rapid detection method, which is characterized in that described in step 4 The calculation formula of chromium content are as follows: Cr%=[(m1×V)/(m×V1)]×100;In formula: m1: the chromium content checked in from standard curve, g;M: sample size, g;V: test solution total volume, mL;V1: divide and takes test solution volume, mL.
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