CN112162057A - Method for measuring total iron content in converter fly ash pressure ball - Google Patents
Method for measuring total iron content in converter fly ash pressure ball Download PDFInfo
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- CN112162057A CN112162057A CN202010829395.1A CN202010829395A CN112162057A CN 112162057 A CN112162057 A CN 112162057A CN 202010829395 A CN202010829395 A CN 202010829395A CN 112162057 A CN112162057 A CN 112162057A
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- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
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Abstract
The invention relates to a method for measuring the content of total iron in converter fly ash pressure balls, which comprises the following steps: step one, putting a converter fly ash sample with mass m into a conical flask, sequentially adding hydrochloric acid and a sodium fluoride solution, and heating at high temperature until the sample is dissolved to form a test solution; continuously dropwise adding stannous chloride and replenishing hydrochloric acid in the dissolving process to keep the test solution yellowish, concentrating the volume of the test solution, taking down and cooling to room temperature; step two, sequentially adding water and a sodium tungstate solution into the test solution, and immediately adding a titanium trichloride solution under continuous shaking until the sample is blue; titrating by using a potassium dichromate standard titration solution until the test solution is changed from light green to blue green to purple red by the last drop; and step three, calculating the total iron content in the sample according to the following formula. The method has the advantages of simple steps, high analysis precision, good repeatability and higher accuracy, effectively reduces the complexity of the experiment, shortens the detection period and reduces the experiment cost.
Description
Technical Field
The invention relates to a method for measuring the content of total iron in converter fly ash pressure balls, and belongs to the technical field of steelmaking raw and auxiliary material detection.
Background
The converter fly ash pressed ball is mainly applied to the technical field of steel making, contains about 45 to 60 percent of total iron, and has high recycling value. The converter fly ash pressing balls can replace sinter, can replace part of waste steel in the smelting process of the converter, can keep the heat balance of the whole converter, can flexibly adjust the adding amount and adding time of cold burden according to the condition of the molten pool of the converter, plays an important role in stabilizing the production of the converter, and can effectively reduce the consumption of metal materials, improve the oxygen supply strength and shorten the smelting period. Therefore, the accurate determination and detection timeliness of the total iron content in the fly ash pressure ball are extremely important, and the total iron content has direct influence on smelting. At present, the determination of the total iron content comprises an oxidation-reduction titration method, a melting sample preparation-X-ray fluorescence spectrometry method and the like. The latter method has the disadvantages of complicated steps, long detection period, high reagent use cost, high analysis skill requirement and unsuitability for single element detection. How to improve the determination and analysis efficiency of the total iron in the converter fly ash pressure ball and reduce the detection cost becomes a main problem to be solved in the field of chemical analysis.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for measuring the content of total iron in converter fly ash pressure balls in the prior art, and can solve the problems of complicated steps, long detection period, high laboratory cost and high requirement on operation skills of the conventional measuring method.
The technical scheme adopted by the invention for solving the problems is as follows: a method for measuring the content of total iron in converter fly ash pressed balls comprises the following steps:
step one, putting a converter fly ash sample with mass m into a conical flask, sequentially adding hydrochloric acid and a sodium fluoride solution, and heating at high temperature until the sample is dissolved to form a test solution; continuously dropwise adding stannous chloride and replenishing hydrochloric acid in the dissolving process to keep the test solution yellowish, concentrating the volume of the test solution, taking down and cooling to room temperature;
step two, sequentially adding water and a sodium tungstate solution into the test solution, and immediately adding a titanium trichloride solution under continuous shaking until the sample is blue; dripping potassium dichromate solution until the blue color disappears, or slightly waiting until the oxygen in the air is oxidized until the blue color disappears, immediately adding sulfuric acid-phosphoric acid mixed acid, and adding sodium diphenylamine sulfonate indicator solution; titrating by using a potassium dichromate standard titration solution until the test solution is changed from light green to blue green to purple red by the last drop;
step three, calculating the total iron content in the sample according to the following formula:
in the formula:
c-potassium dichromate standard titration solution concentration in moles per liter (mol/L);
v-volume of potassium dichromate solution consumed by titrating the sample solution in milliliters (mL);
V0-titrating the blank test solution to consume the volume of potassium dichromate solution in milliliters (mL);
m-mass of the sample in grams (g);
55.85-molar mass of iron in grams per mole (mol/L).
Optionally, in step one, the sample is taken in the conical flask, and then a small amount of water is added to wet along the wall of the conical flask.
Optionally, in the step one, if the stannous chloride is excessive and the solution is transparent, the potassium permanganate solution is dripped to be yellowish.
Optionally, hydrochloric acid and sodium fluoride are used for decomposing the sample in the step one.
Optionally, the stannous chloride used in the step one is not added with tin particles and is prepared for use.
Optionally, in the second step, a titanium trichloride solution is adopted to reduce ferric iron into ferrous iron, and the pH value is adjusted by using a sulfuric acid-phosphoric acid mixed acid.
Optionally, the sodium fluoride solution in step one is stored in a plastic bottle.
Optionally, in the step one, the mass m of the sample is 0.2g, the rho of hydrochloric acid added for the first time is 1.19g/mL, the concentration of the sodium fluoride solution is 50g/L, the concentration of stannous chloride added dropwise in the dissolving process is 60g/mL, and the added hydrochloric acid is 1+ 1.
Optionally, in the second step, the concentration of the sodium tungstate solution is 250g/mL, the titanium trichloride solution is 1+14 titanium trichloride solution, the concentration of the potassium dichromate solution is 1g/L, the sulfuric acid-phosphoric acid mixed acid is 3+3+4 sulfuric acid-phosphoric acid mixed acid, the concentration of the sodium diphenylamine sulfonate indicator solution is 4g/L, and the concentration of the potassium dichromate titration solution is labeled as c (1/6K)2Cr2O7)＝0.05000moL/L。
Compared with the prior art, the invention has the advantages that:
the method for measuring the content of the total iron in the converter fly ash pressure ball is simple and convenient in steps, high in analysis precision, good in repeatability and high in accuracy, effectively reduces the complexity of an experiment, shortens the detection period, timely provides accurate detection data for an enterprise steelmaking technology, and reduces the experiment cost.
Detailed Description
The present invention will be described in further detail with reference to examples.
In this embodiment, a method for determining the content of total iron in converter fly ash pressure balls includes the following steps:
step one, preparing a reagent: the hydrochloric acid rho is 1.19 g/mL; 1+1 of hydrochloric acid; sulfuric acid-phosphoric acid mixed acid 3+3+ 4; 50g/L of sodium fluoride solution; stannous chloride 60 g/mL; 250g/mL of sodium tungstate solution; 1g/L of potassium dichromate solution; 1+14 parts of a titanium trichloride solution; potassium dichromate standard titration solution c (1/6K)2Cr2O7) ═ 0.05000 moL/L; 4g/L of diphenylamine sodium sulfonate indicator solution; 4g/L of potassium permanganate solution;
weighing a converter fly ash sample with the mass of 0.2g into a 300 mL conical flask, adding a small amount of water to soak along the wall of the conical flask, adding 20 mL of hydrochloric acid (rho is 1.19g/mL), adding 15 mL of sodium fluoride solution (50g/L), and heating at high temperature until the sample is dissolved to form a test solution; continuously dropwise adding stannous chloride (60g/mL) and supplemented hydrochloric acid (1+1) according to the change of the test solution in the dissolving process, wherein if the stannous chloride is excessive, the solution is transparent, a potassium permanganate solution (4g/L) can be dropwise added to be slightly yellow, the test solution is kept slightly yellow, the concentration volume is about 20 mL, and the test solution is taken down and cooled to room temperature;
step two, adding about 150 mL of water and 1 mL of sodium tungstate solution (250g/mL), and immediately adding a titanium trichloride solution (1+14) under continuous shaking until the sample is blue; dripping potassium dichromate solution (1g/L) until the blue color disappears, or slightly waiting until the oxygen in the air is oxidized until the blue color disappears, immediately adding 20 ml sulfuric acid-phosphoric acid mixed acid (3+3+4), and adding 5 drops of sodium diphenylamine sulfonate indicator solution (4 g/L); titration of solution c with potassium dichromate Standard (1/6K)2Cr2O7) ═ 0.05000moL/L, titrate until the end point when the test solution changes from light green to blue green to purple red, and the volume of potassium dichromate solution consumed at this time is 39.4 ml;
step three, calculating the content of total iron in the sample by the following formula:
in the formula:
c-potassium dichromate standard titration solution concentration in moles per liter (mol/L);
v-the volume of potassium dichromate standard titration solution consumed by titrating the sample solution, in milliliters (mL);
V0-titrating the blank test solution to consume the volume of the standard titration solution of potassium dichromate in milliliters (mL);
m-mass of the sample in grams (g);
55.85-molar mass of iron in grams per mole (mol/L)
The determination of total iron content is 55.01% according to the calculation of the formula.
Three sets of standards H51, H52 were tested in multiple runs according to the analytical procedure of the present invention and the results are shown in Table 1, with the measured values being very close to the standard values.
Table 1: analysis results of Standard samples GBW07218a, GSB03-184-
According to the invention, the sample samples Y1, Y2 and Y3 are respectively measured and compared with the results of the melting sample preparation-X-ray fluorescence spectrometry, the comparison results are shown in Table 2, and the accuracy of the results detected by the method is not lower than that of the melting sample preparation-X-ray fluorescence spectrometry through the Table 2;
table 2: comparison of analysis results of hydrochloric acid-sodium fluoride decomposition method and melting sample preparation-X-ray fluorescence spectrometry
The experiments show that the method has high analysis precision, good repeatability and good accuracy, effectively reduces the complexity of the experiment and greatly reduces the analysis cost.
In addition to the above embodiments, the present invention also includes other embodiments, and any technical solutions formed by equivalent transformation or equivalent replacement should fall within the scope of the claims of the present invention.
Claims (9)
1. A method for measuring the content of total iron in converter fly ash pressed balls is characterized by comprising the following steps:
step one, putting a converter fly ash sample with mass m into a conical flask, sequentially adding hydrochloric acid and a sodium fluoride solution, and heating at high temperature until the sample is dissolved to form a test solution; continuously dropwise adding stannous chloride and replenishing hydrochloric acid in the dissolving process to keep the test solution yellowish, concentrating the volume of the test solution, taking down and cooling to room temperature;
step two, sequentially adding water and a sodium tungstate solution into the test solution, and immediately adding a titanium trichloride solution under continuous shaking until the sample is blue; dripping potassium dichromate solution until the blue color disappears, or slightly waiting until the blue color disappears after oxidation in the air, immediately adding sulfuric acid-phosphoric acid mixed acid, and adding sodium diphenylamine sulfonate indicator solution; titrating by using a potassium dichromate standard titration solution until the test solution is changed from light green to blue green to purple red by the last drop;
step three, calculating the total iron content in the sample according to the following formula:
in the formula:
c-potassium dichromate standard titration solution concentration in moles per liter (mol/L);
v-volume of potassium dichromate solution consumed by titrating the sample solution in milliliters (mL);
V0-titrating the blank test solution to consume the volume of potassium dichromate solution in milliliters (mL);
m-mass of the sample in grams (g);
55.85-molar mass of iron in grams per mole (mol/L).
2. The method for measuring the content of the total iron in the converter fly ash pressed ball according to claim 1, which is characterized in that: in the first step, a sample is taken in a conical flask, and then a small amount of water is added to soak along the wall of the conical flask.
3. The method for measuring the content of the total iron in the converter fly ash pressed ball according to claim 1, which is characterized in that: and in the first step, if the stannous chloride is excessive and the solution is transparent, the potassium permanganate solution is dripped to be yellowish.
4. The method for measuring the content of the total iron in the converter fly ash pressed ball according to claim 1, which is characterized in that: and in the first step, hydrochloric acid and sodium fluoride are adopted to decompose the sample.
5. The method for measuring the content of the total iron in the converter fly ash pressed ball according to claim 1, which is characterized in that: the stannous chloride used in the step one is not added with tin particles and is prepared for use.
6. The method for measuring the content of the total iron in the converter fly ash pressed ball according to claim 1, which is characterized in that: and in the second step, reducing ferric iron into ferrous iron by adopting a titanium trichloride solution, and regulating the pH value by using sulfuric acid-phosphoric acid mixed acid.
7. The method for measuring the content of the total iron in the converter fly ash pressed ball according to claim 1, which is characterized in that: the sodium fluoride solution in step one is stored in a plastic bottle.
8. The method for measuring the content of the total iron in the converter fly ash pressed ball according to claim 1, which is characterized in that: in the first step, the mass m of the sample is 0.2g, the rho of hydrochloric acid added for the first time is 1.19g/mL, the concentration of the sodium fluoride solution is 50g/L, the concentration of stannous chloride added dropwise in the dissolving process is 60g/mL, and the added hydrochloric acid is 1+ 1.
9. The method for measuring the content of the total iron in the converter fly ash pressed ball according to claim 1, which is characterized in that: in the second step, the concentration of the sodium tungstate solution is 250g/mL, the titanium trichloride solution adopts a titanium trichloride solution 1+14, the concentration of the potassium dichromate solution is 1g/L, the sulfuric acid-phosphoric acid mixed acid adopts a sulfuric acid-phosphoric acid mixed acid 3+3+4, the concentration of the sodium diphenylamine sulfonate indicator solution is 4g/L, and the concentration of the potassium dichromate label titration solution is c (1/6K)2Cr2O7)＝0.05000moL/L。
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| CN202010829395.1A CN112162057A (en) | 2020-08-18 | 2020-08-18 | Method for measuring total iron content in converter fly ash pressure ball |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103472059A (en) * | 2013-09-30 | 2013-12-25 | 武汉钢铁(集团)公司 | Method for measuring total iron content in fly ash |
| CN109580871A (en) * | 2018-11-26 | 2019-04-05 | 九江萍钢钢铁有限公司 | A kind of method of potassium bichromate standard solution calibration |
-
2020
- 2020-08-18 CN CN202010829395.1A patent/CN112162057A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103472059A (en) * | 2013-09-30 | 2013-12-25 | 武汉钢铁(集团)公司 | Method for measuring total iron content in fly ash |
| CN109580871A (en) * | 2018-11-26 | 2019-04-05 | 九江萍钢钢铁有限公司 | A kind of method of potassium bichromate standard solution calibration |
Non-Patent Citations (4)
| Title |
|---|
| 中华人民共和国工业和信息化部: "《XB/T 617.4-2014 钕铁硼合金化学分析方法 第4部分：铁含量的测定 重铬酸钾滴定法》", 14 October 2014 * |
| 和平使者: "含铁尘泥 全铁含量的测定 三氯化钛还原重铬酸钾滴定法", 《道客巴巴》 * |
| 梁红 等: "《工业分析》", 28 February 2006, 中国环境科学出版社 * |
| 袁奕秋 等: "压片制样X射线荧光光谱法测定除尘灰中全铁含量", 《天津冶金》 * |
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