CN104422685A - Method for determining content of metal aluminum in ladle slag modifying agent - Google Patents
Method for determining content of metal aluminum in ladle slag modifying agent Download PDFInfo
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- CN104422685A CN104422685A CN201310388452.7A CN201310388452A CN104422685A CN 104422685 A CN104422685 A CN 104422685A CN 201310388452 A CN201310388452 A CN 201310388452A CN 104422685 A CN104422685 A CN 104422685A
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Abstract
The invention relates to a method for determining the content of metal aluminum in a ladle slag modifying agent, which mainly aims at solving the technical problems in the prior art that the precision of detection on the content of the metal aluminum in the ladle slag modifying agent is low and the time for detecting the content of the metal aluminum in the ladle slag modifying agent is long. According to the technical scheme, the method for determining the content of the metal aluminum in the ladle slag modifying agent comprises the following steps: measuring a test sample of a fixed quantity, placing the test sample into a tapered bottle with a copper sulfate leaching solution, and heating and boiling the copper sulfate leaching solution by utilizing an electric heating plate so as to selectively dissolve metal aluminum in the test sample, thereby separating the metal aluminum from other elements and aluminum in other forms in the test sample, and preparing a solution to be detected; determining spectral intensity of the aluminum in the solution to be detected by adopting an inductance coupling plasma emission spectrometer; and calculating the content of the metal aluminum in the test sample. By adopting the determination method, the content of the metal aluminum in the ladle slag modifying agent can be accurately measured, and the detection time is short and only needs 2 to 3 hours.
Description
Technical field
The present invention relates to steel-making raw and auxiliary material chemical analysis technology field, particularly the assay method of metal aluminum content in a kind of ladle dreg modifying agent.
Background technology
What require steel product quality along with user improves constantly, and inclusion content of steel must be fewer and feweri, and granularity also must be more and more less, and this just requires that ladle is in refining process, and the deoxidation products of molten steel will float in time.In prior art, iron and steel enterprise adopts process to be the ladle dreg modifying agent added in steel-making ladle molten steel refining process containing metallic aluminium usually, to reach the cleanliness factor that absorption foreign substance in molten steel improves molten steel, ladle dreg modifying agent has good deoxidation, desulfurized effect to molten steel simultaneously.
Along with improving constantly of requiring Cleanliness of Molten Steel, also higher requirement to be had to the requirement of process for making and steel-making raw and auxiliary material accordingly.Ladle dreg modifying agent containing metallic aluminium is more prevalent at refining application of RE in the steel as a kind of slag making materials.China Patent No. is ZL200810024566.2, disclosed a kind of modifier for ladle top slag modification, be made up of active lime, pre-melted slag, fluorite, aluminum shot, pre-melted slag major component is calcium aluminate system (CaO-Al2O3), and the percentage by weight of its chemical composition is: CaO:57 ~ 70%; Al2O3:15 ~ 28%; Al:3.5 ~ 7%; CaF2:6 ~ 10%; MgO:1.5 ~ 5%; SiO2:<3%; C≤0.01%; Control moisture≤0.3%.Metal aluminum content is one of ladle dreg modifying agent important indicator, and its height directly has influence on the quality of metallurgical effect and steel.
In prior art, assay method for metallic aluminium in ladle dreg modifying agent does not also have corresponding national standard method at present, although some traditional analytical approach is by highly basic fusion and decomposition sample, aluminium content in disodium ethylene diamine tetraacetate (EDTA) titration measuring sample, this kind of method is Holo-Al content in working sample (metallic aluminium and other chemical combination state aluminium resultant), instead of metal aluminum content, if make the detection data that can only provide mistake in this way, economic loss can be caused to smelter.
In prior art, also have on a small quantity about the report of metal aluminum content assay method in aluminium slag making materials, as Determination of Al Metal in Slag-Modifier Agent for Molten Steel Refining with Iron Sulfate Leaching Method, " special steel technology ", Gan Guojian, 50-52 in 2007.The method adopts iron sulfate leaching, and its metallic aluminium leaching effect is bad, and sense cycle is long, the alundum (Al2O3) of part chemical combination state also can be caused simultaneously to dissolve, cause testing result error larger.Chinese patent publication No. CN102269708A, name is called, the assay method of metallic aluminium in a kind of aluminium slag making materials, disclose a kind of ferric trichloride-ammonium chloride mixed solution that adopts to leach, disodium ethylene diamine tetraacetate (EDTA) Complexometric B ack-Titration method measures the method for aluminium content in leaching liquid, this mensuration mode poor operability, the analyst needing more rich working experience can complete, careless slightly, cause testing result mistake, also be applicable to low content (<5%) metallic aluminium to measure simultaneously, be mainly manifested in following several respects: (1) adopts ferric trichloride-ammonium chloride mixed solution leaching metallic aluminium, leaching speed is slow, general needs 30 ~ 120min can leach completely, (2) a large amount of ferric ion in leaching liquid, interference aluminium measures, and needs precipitate and separate, causes operation quite complicated, and the ferric hydroxide simultaneously precipitated to a certain extent can Al adsorption, causes Al-single crystal error larger, (3) adopt traditional EDTA Complexometric B ack-Titration method to measure aluminium content in solution, need fine adjustment solution condition, and then adopt manual titration measuring aluminium content.Chinese patent publication No. CN102507853A, name is called, metallic aluminium assay method in steel-making exothermic mixture, disclose a kind of NaOH that adopts and belong to aluminium as leaching liquid leaching Gold Samples, disodium ethylene diamine tetraacetate (EDTA) Complexometric B ack-Titration method measures aluminium content in leaching liquid, and this method exists following problem: (1) adopts NaOH to belong to aluminium as leaching liquid leaching Gold Samples, and leaching speed is slow, chemical combination state aluminium also can be caused simultaneously to dissolve, cause testing result distortion; (2) adopt traditional EDTA Complexometric B ack-Titration method to measure aluminium content in solution, need fine adjustment solution condition, and then adopt manual titration measuring aluminium content.
In prior art, the disclosed ladle dreg modifying agent containing metallic aluminium, metal aluminum content detection method is also in traditional manual inspection technological layer, operation is quite complicated, labour intensity is large, poor operability, estimating precision is low, and detection time is long, whole analysis needs 6 ~ 8 hours, are difficult to meet the production requirement of modern steel enterprise; Meanwhile, these class methods need chemical reagent kind how large with amount of reagent, can bring the problems such as certain environment pollution.
Summary of the invention
The object of this invention is to provide the assay method of metal aluminum content in a kind of ladle dreg modifying agent, solve the technical matters that accuracy of detection is low, detection time is long of metal aluminum content in ladle dreg modifying agent in prior art.
The technical solution used in the present invention is:
An assay method for metal aluminum content in ladle dreg modifying agent, comprises the following steps:
A, take quantitative sample and be placed in the conical flask filling copper sulphate leaching liquid, boil optionally metallic aluminium in dissolved samples with electric hot plate heating, metallic aluminium is separated with the aluminium of other element and other form in sample, is prepared into solution to be measured;
The spectral intensity of aluminium in b, use inductance Coupled Plasma-Emission spectrophotometer solution to be measured;
C, calculate metal aluminum content in sample.
Further, in step a of the present invention, leaching liquid is prepared from 100ml dilution heat of sulfuric acid (1+4) for taking 15 ~ 20g copper sulphate dissolves, during leaching sample, in leaching liquid, concentration of copper sulfate is 15 ~ 20%, leaching liquid addition is 40 ~ 60ml, and leaching the time of boiling with the electric hot plate of power 2.4KW is 20 ~ 30min.
Again, according to chemical characteristic and the spectra1 interfer-of aluminium element, Inductively coupled plasma optical emission spectrometer spectral intensity I of aluminium in solution to be measured in wavelength 396.15nm or 308.22nm determination step a in step b
alshi Xiaoguo is good.
Further, step c, calculates metal aluminum content in sample by formula one:
in formula one,
for metallic aluminium mass percent in sample;
for sample sample weighting amount, unit is g; A is background equipotent concentration, and unit is ug; B be the spectral intensity of aluminium to mass conversion, unit is ug/cps; I
alfor the spectral intensity of aluminium in solution, unit is cps.
In formula one, the spectral intensity of background equipotent concentration a and aluminium is determined by the working curve equation of the spectral intensity relation of aluminium content and aluminium in solution mass conversion b, be specially: accurately pipette 0 respectively with pipette, 1.00, 3.00, 5.00, 7.00, 9.00, 10.00ml aluminum standard solution (1000ug/ml) is in 100ml volumetric flask, add the 50ml leaching liquid that concentration of copper sulfate is 20%, be diluted with water to scale, shake up solution, aluminium ion intensity in above-mentioned solution is measured respectively at wavelength 396.15nm or 308.22nm place with Inductively coupled plasma optical emission spectrometer, the unary linear regression equation of the working curve of the spectral intensity relation of aluminium content and aluminium in solution is calculated by Computer
(formula two) determines a and b value; In formula two, m is aluminium content in solution, and unit is ug; A is background equipotent concentration, and unit is ug; B be the spectral intensity of aluminium to mass conversion, unit is ug/cps; I
alfor the spectral intensity of aluminium in solution, unit is cps.
The present invention is separated metallic aluminium in ladle dreg modifying agent by employing chemical reagent selective dissolution, measures by metal aluminum content in inductance Coupled Plasma-Emission spectrophotometer leaching liquid, solves the accurately quick test problems of metallic aluminium in ladle dreg modifying agent.
The present invention has following good effect compared to existing technology:
1. present invention achieves metal aluminum content rapid and accurate determination in ladle dreg modifying agent, easy and simple to handle, labour intensity is low, workable, detection automaticity is high, avoid the operation steps that complicated Chemical Decomposition, solution condition adjustment, manual titration etc. are complicated, the leaching time of aluminium foreshortens to 20 ~ 30min, and whole minute only needs 2 ~ 3 hours.
2. method of the present invention decreases the use of chemical reagent, only uses copper sulphate, sulfuric acid two kinds of reagent, considerably reduces the discharge of chemical pollutant, reduce human body and environmental hazard.
Embodiment
An assay method for metal aluminum content in ladle dreg modifying agent, comprises the following steps:
A, take 200g copper sulphate dissolves be prepared into the leaching liquid that concentration of copper sulfate is 20% in 1000ml dilution heat of sulfuric acid (1+4), take 0.25g sample and be placed in 300ml conical flask, add 50ml copper sulphate leaching liquid, with model be SC-404, the electric hot plate of power 2.4KW boils about 25min, dissolve completely until solubilisable sample, take off cool to room temperature, constant volume, in 100ml volumetric flask, is done filtration with fast grade filter paper and is obtained filtrate;
B, be aluminium spectrum intensity I in the filtrate that obtains in wavelength 308.22nm determination step a of iCAP6300 Inductively coupled plasma optical emission spectrometer by model
al;
C, calculate metal aluminum content in sample by formula one:
(formula one)
In formula one,
for metallic aluminium mass percent in sample;
for sample sample weighting amount, unit is g; A is background equipotent concentration, and unit is ug; B be the spectral intensity of aluminium to mass conversion, unit is ug/cps; I
alfor the spectral intensity of aluminium in solution, unit is cps.
In formula one, the spectral intensity of background equipotent concentration a and aluminium is determined by the working curve equation of the spectral intensity relation of aluminium content and aluminium in solution mass conversion b, be specially: accurately pipette 0 respectively with pipette, 1.00, 3.00, 5.00, 7.00, 9.00, 10.00ml aluminum standard solution (1000ug/ml) is in 100ml volumetric flask, add the 50ml leaching liquid that concentration of copper sulfate is 20%, be diluted with water to scale, shake up solution, be that iCAP6300 Inductively coupled plasma optical emission spectrometer measures aluminium spectrum intensity in above-mentioned solution respectively at wavelength 308.22nm place by model, the unary linear regression equation of the working curve of the spectral intensity relation of aluminium content and aluminium in solution is calculated by Computer
(formula two) determines a and b value, and in formula two, m is aluminium content in solution, and unit is ug, a is background equipotent concentration, and unit is ug, b be the spectral intensity of aluminium to mass conversion, unit is ug/cps, I
alfor the spectral intensity of aluminium in solution, unit is cps.
The preci-sion and accuracy of the inventive method is confirmed by the recovery testu of sample and Precision Experiment.
Recovery experiment, add a certain amount of metallic aluminium in ladle dreg modifying agent sample after, by the inventive method, the recovery of standard addition of test samples, test findings sees the following form 1.
Table 1 sample recovery testu
| Add metal aluminum amount (g) | Metallic aluminium yield (g) | The recovery (%) |
| 0.1001 | 0.0999 | 99.8 |
| 0.2025 | 0.2030 | 100.2 |
| 0.3005 | 0.2966 | 98.7 |
| 0.4003 | 0.3990 | 99.7 |
| 0.5030 | 0.5080 | 101.0 |
Precision Experiment, carry out 11 Precision Experiments to 2 groups of ladle dreg modifying agents, analysis result sees the following form 2.
Table 2 sample Precision Experiment
Above-mentioned experimental result shows, in the recovery testu of sample, the metallic aluminium recovery is between 98.7 ~ 101.0%, and the recovery is high; In Precision Experiment, RSD is less than 3%, detects data precision good, proves that the inventive method accurately and reliably, meet iron and steel enterprise's production requirement completely.
Claims (5)
1. the assay method of metal aluminum content in ladle dreg modifying agent, is characterized in that, said method comprising the steps of:
A, take quantitative sample and be placed in the conical flask filling copper sulphate leaching liquid, boil optionally metallic aluminium in dissolved samples with electric hot plate heating, metallic aluminium is separated with the aluminium of other element and other form in sample, is prepared into solution to be measured;
The spectral intensity of aluminium in b, use inductance Coupled Plasma-Emission spectrophotometer solution to be measured;
C, calculate metal aluminum content in sample.
2. the assay method of metal aluminum content in a kind of ladle dreg modifying agent as claimed in claim 1, it is characterized in that, in described step a, leaching liquid is prepared from 100ml dilution heat of sulfuric acid (1+4) for taking 15 ~ 20g copper sulphate dissolves, during leaching sample, in leaching liquid, concentration of copper sulfate is 15 ~ 20%, leaching liquid addition is 40 ~ 60ml, and leaching the time of boiling with the electric hot plate of power 2.4KW is 20 ~ 30min.
3. the assay method of metal aluminum content in a kind of ladle dreg modifying agent as claimed in claim 1, it is characterized in that, in described step b Inductively coupled plasma optical emission spectrometer when wavelength 396.15nm or 308.22nm in determination step a in solution to be measured in the spectral intensity I of aluminium
al.
4. the assay method of metal aluminum content in a kind of ladle dreg modifying agent as claimed in claim 1, is characterized in that, calculate metal aluminum content in sample in described step c by formula one:
In formula one,
for metallic aluminium mass percent in sample;
for sample sample weighting amount, unit is g; A is background equipotent concentration, and unit is ug; B: the spectral intensity of aluminium is to mass conversion, and unit is ug/cps; I
al: the spectral intensity of aluminium in solution, unit is cps.
5. the assay method of metal aluminum content in a kind of ladle dreg modifying agent as claimed in claim 4, it is characterized in that, in formula one, the spectral intensity of background equipotent concentration a and aluminium is determined by the working curve equation of the spectral intensity relation of aluminium content and aluminium in solution mass conversion b, be specially and accurately pipette 0 respectively with pipette, 1.00, 3.00, 5.00, 7.00, 9.00, 10.00ml aluminum standard solution (1000ug/ml) is in 100ml volumetric flask, add the 50ml leaching liquid that concentration of copper sulfate is 20%, be diluted with water to scale, shake up solution, aluminium spectrum intensity in above-mentioned solution is measured respectively at wavelength 396.15nm or 308.22nm place with Inductively coupled plasma optical emission spectrometer, the unary linear regression equation of the working curve of the spectral intensity relation of aluminium content and aluminium in solution is calculated by Computer
(formula two) determines a and b value, and in formula two, m is aluminium content in solution, and unit is ug, a is background equipotent concentration, and unit is ug, b be the spectral intensity of aluminium to mass conversion, unit is ug/cps, I
alfor the spectral intensity of aluminium in solution, unit is cps.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104897623A (en) * | 2015-06-12 | 2015-09-09 | 武汉钢铁(集团)公司 | Method for determining aluminium oxide content of aluminous castable |
| CN108120711A (en) * | 2016-11-28 | 2018-06-05 | 广东韶钢松山股份有限公司 | A kind of method that Holo-Al content in steel is measured using inductively coupled plasma atomic emission spectrometer |
| CN108152269A (en) * | 2016-12-02 | 2018-06-12 | 上海梅山钢铁股份有限公司 | The detection method of iron content in a kind of sulfur-iron alloy |
| CN109374597A (en) * | 2018-09-30 | 2019-02-22 | 武钢集团昆明钢铁股份有限公司 | A method of aluminum oxide content in measurement slag iron separation agent |
| CN110554136A (en) * | 2018-06-04 | 2019-12-10 | 上海梅山钢铁股份有限公司 | Method for detecting sulfur content in blast furnace gas |
-
2013
- 2013-08-31 CN CN201310388452.7A patent/CN104422685A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 周桂海: "ICP-AES法测定冶金渣中金属铝含量", 《梅山科技》 * |
| 陈际达 等: "铝渣中铝的价态分析", 《冶金分析》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104897623A (en) * | 2015-06-12 | 2015-09-09 | 武汉钢铁(集团)公司 | Method for determining aluminium oxide content of aluminous castable |
| CN108120711A (en) * | 2016-11-28 | 2018-06-05 | 广东韶钢松山股份有限公司 | A kind of method that Holo-Al content in steel is measured using inductively coupled plasma atomic emission spectrometer |
| CN108152269A (en) * | 2016-12-02 | 2018-06-12 | 上海梅山钢铁股份有限公司 | The detection method of iron content in a kind of sulfur-iron alloy |
| CN110554136A (en) * | 2018-06-04 | 2019-12-10 | 上海梅山钢铁股份有限公司 | Method for detecting sulfur content in blast furnace gas |
| CN109374597A (en) * | 2018-09-30 | 2019-02-22 | 武钢集团昆明钢铁股份有限公司 | A method of aluminum oxide content in measurement slag iron separation agent |
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