CN103344636A - Method for determination of aluminum and alumina in steel slag - Google Patents
Method for determination of aluminum and alumina in steel slag Download PDFInfo
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- CN103344636A CN103344636A CN2013102419551A CN201310241955A CN103344636A CN 103344636 A CN103344636 A CN 103344636A CN 2013102419551 A CN2013102419551 A CN 2013102419551A CN 201310241955 A CN201310241955 A CN 201310241955A CN 103344636 A CN103344636 A CN 103344636A
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- edta
- standard solution
- alundum
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Abstract
The invention discloses a method for determination of aluminum and alumina in steel slag. The method comprises the following steps of 1, dissolving steel slag in hydrochloric acid, adding sodium hydroxide solids into the filtered solution so that other metal ions form hydroxide precipitates and the precipitates are separated from the solution, adding an excess amount of an EDTA standard solution into the subacid solution, carrying out boiling in the presence of acetic acid-ammonium acetate so that aluminum and EDTA fully form a complex, carrying out back titration of the residual EDTA by a copper sulfate standard solution in the presence of PAN as an indicator until the solution has a purplish red color or a blue color, and calculating an aluminum mass fraction, and 2, ashing the filter paper in the residual residues obtained by step 1, carrying out fusion of a sample by a mixed solvent, carrying out leaching by hydrochloric acid, adding sodium hydroxide solids into the leaching solution, carrying out separation and adding an EDTA standard solution into the separated solution. The method for detection utilizes the characteristic that aluminum can be dissolved in hydrochloric acid easily and cannot dissolve alumina, realizes simultaneous detection of aluminum and alumina content, has simple processes and can produce an accurate detection result.
Description
Technical field
The invention belongs to chemical analysis field, particularly the mensuration of metallic aluminium and alundum (Al in the slag.
Background technology
Slag also is the important auxiliary material of steel-making, not only can adsorb the molten steel snotter and steel quality is provided, and can strengthen deoxidation, desulfurization, dephosphorization, prevents that molten steel is air-breathing, reduces the temperature of molten steel and scatters and disappears.Along with providing day by day of steel-making level, slag material market demand also increases day by day.Therefore the setting of the steel performance that the accurate analysis of the chemical constitution of slag is conducive to refine reaches desirable steel performance easilier.
Summary of the invention
The purpose of this invention is to provide a kind of method of measuring metallic aluminium and alundum (Al in the slag simply, accurately.
Technical scheme of the present invention is achieved in that the mensuration of metallic aluminium and alundum (Al in the slag, it is characterized in that:
Step 1: use the dissolving with hydrochloric acid slag, in the solution after filtration, add sodium hydrate solid, aluminium is sodium metaaluminate, and other metallic ions are precipitation of hydroxide and separate; In slightly acidic solution, add excessive EDTA standard solution, then in the presence of acetic acid-ammonium acetate, boil and make aluminium and EDTA all form complex, be indicator with PAN, with the EDTA of copper sulphate standard solution residual titration surplus to aubergine or blueness be terminal point, calculate the massfraction of metallic aluminium;
Step 2: with the residual residue after the step 1 filtration, behind ashing filter paper, sample mixed solvent fusion, hydrochloric acid leaching is after hydro-oxidation sodium solid separates, add excessive EDTA standard solution, then in the presence of acetic acid-ammonium acetate, boil and make aluminium and EDTA all form complex, be indicator with PAN, with the excessive EDTA of copper sulphate standard solution residual titration, calculate the massfraction of alundum (Al.
Nearly step ground, the method for making of described EDTA standard solution: take by weighing 93gEDTA in the 10000ml volumetric flask, be diluted to scale with water, shake up
Nearly step ground, acetic acid-ammonium acetate method for making takes by weighing the 77g ammonium acetate, is dissolved in water, and adds the 5ml glacial acetic acid, is diluted to 1000ml with water.
Further, PAN is 0.1% ethanolic solution.
Nearly step ground, the method for making of copper sulphate standard solution takes by weighing 65g copper sulphate in the 10000ml volumetric flask, adds 5mL sulfuric acid, is diluted to scale with water, shakes up.
Nearly step ground, described mixed solvent is: 1.5 parts of natrium carbonicum calcinatums, the sodium tetraborate of 1.5 parts of sal tartari and 0.7 part.
Carry out calculating as a result then:
One, is calculated as follows the percentage composition of aluminium
In the formula: C-copper sulphate concentration of standard solution, mol/L;
V
1The volume of-adding EDTA standard solution, ml;
V
2Consume the volume of copper sulphate standard solution during-titration, ml;
G-take by weighing sample mass, g;
F-separatory rate;
26.98 the molal weight of-aluminium, g/mol;
Two, be calculated as follows the percentage composition of alundum (Al
In the formula: the concentration of C-EDTA standard solution, mol/L;
V
1The volume of-adding EDTA standard solution, ml;
V
2The excessive EDTA of-residual titration consumes the volume of copper sulphate standard solution, ml;
V
3-minute get the volume of test solution, ml;
V
4The volume of-constant volume, ml;
M-sample size, g.
Beneficial effect of the present invention is: detection method of the present invention has utilized aluminium to be soluble in hydrochloric acid, and must dissolve the characteristic of alundum (Al, detects the content of metallic aluminium and alundum (Al simultaneously, and detection method is simpler, and testing result is more accurate.
Embodiment
Below in conjunction with specific embodiment the present invention is further explained explanation.
One, chemical reagent
1.1 NaOH: solid.
1.2 hydrochloric acid solution: (2+3).
1.3 hydrochloric acid solution: (1+1).
1.4 phenolphthalein indicator: 1% ethanolic solution.
1.5 PAN indicator: 0.1% ethanolic solution.
1.6 acetic acid-ammonium acetate buffer solution (PH=4.5): take by weighing the 77g ammonium acetate, be dissolved in water, add the 5ml glacial acetic acid, be diluted to 1000ml with water.
1.7 sodium fluoride: solid.
1.8 EDTA standard solution (0.025mol/L): take by weighing 93gEDTA in the 10000ml volumetric flask, be diluted to scale with water, shake up.
1.9 copper sulphate standard solution (0.025mol/L): take by weighing 65g copper sulphate in the 10000ml volumetric flask, add 5mL sulfuric acid, be diluted to scale with water, shake up.
1.10 mixed solvent: 1.5 parts of natrium carbonicum calcinatums, the sodium tetraborate mixing of 1.5 parts of sal tartari and 0.7 part, porphyrize is preserved in port grinding bottle.
1.11 the demarcation of EDTA standard solution: benchmark copper solution (C=0.025 mol/L): accurately take by weighing the 0.3971g fine copper in the 300ml beaker, add 10mL nitric acid (1+1), after the dissolving, be diluted in the 250ml volumetric flask, shake up.
Accurately pipette four parts of EDTA solution that 20.0ml configures in the 250mL conical flask, add 60mL water, 20ml buffer solution, heating is boiled, and takes off, and add PAN indicator 4-6 and drip, be terminal point with benchmark copper solution titration to purple immediately.
Calculate:
C-EDTA concentration of standard solution, mol/L;
C
1The accurate concentration of-benchmark copper solution, mol/L;
V
1The accurate volume of-benchmark copper solution, ml;
V
2The accurate volume of the EDTA standard solution of-adding, ml
The demarcation of copper sulphate standard solution: accurately pipette EDTA standard solution 20.0mL, four parts in the 250ml conical flask, add buffer solution 20ml, about thin up 100ml, heating is boiled, and takes off, add PAN indicator 4-6 and drip, copper-bath titration to the rose of demarcating with desire is terminal point.
Calculate:
C-copper sulphate concentration of standard solution, mol/L;
C
1The accurate concentration of-EDTA standard solution, mol/L;
V
1The accurate volume of-EDTA standard solution, ml;
V
2The accurate volume of-copper sulphate standard solution, ml
Two, chemical analysis:
(1) mensuration of metallic aluminium
Take by weighing the 0.2000g sample in the 300ml beaker, add 50ml hydrochloric acid (1.2), sample is placed be heated to the reaction end on the electric furnace pan, take off immediately, filter 1. in the 400ml beaker 1. with quick filter paper, after washing precipitation three times with water, in solution, add NaOH (1.1) when precipitation of hydroxide occurring, after amount 6g, boil, be cooled to room temperature, move in 200 milliliters of volumetric flasks, filter in former beaker with quick filter paper.
Draw the above-mentioned filtrate of 50mL in the 500ml conical flask, add EDTA standard solution (1.8) 40.0ml, add 20ml water, add 2 phenolphthalein indicators (1.4) dripping hydrochloric acid (1.3) and be neutralized to red disappearance just, after 2 of amounts, add 20ml buffer solution (1.6), boil 1min, insulation 2min, add 7 PAN indicator (1.5), by yellow purpling redness, disregard reading with copper sulphate standard solution (1.9) titration, add 1g sodium fluoride (1.7), 1min is boiled in heating, takes off insulation 2min, adding 7 PAN indicator (1.5) again, is terminal point with copper sulphate standard solution (1.9) titration by yellow purpling redness (or blue).
Be calculated as follows the percentage composition of aluminium
In the formula: C-copper sulphate concentration of standard solution, mol/L;
V
1The volume of-adding EDTA standard solution, ml;
V
2Consume the volume of copper sulphate standard solution during-titration, ml;
G-take by weighing sample mass, g;
F-separatory rate;
26.98 the molal weight of-aluminium, g/mol
(2) mensuration of alundum (Al
To analyze the metallic aluminium filtration remaining residue in back and filter paper together moves in the platinum crucible, in high temperature furnace after the ashing, add mixed solvent (1.10) 2 ~ 3g, mixing, cover 1g again, fusion 20 ~ 40min in 1000 ℃ of muffle furnaces places platinum crucible in the beaker that fills 50ml water and 20ml hydrochloric acid, being heated to sample all dissolves, water washes out crucible, adds NaOH (1.1) to precipitation occurring, after amount 6g, boil, be cooled to room temperature, move in the 200ml volumetric flask, be diluted with water to scale, mixing is done filtration with quick filter paper.
Draw filtrate 50ml in the 500ml conical flask, add EDTA(1.8) 30.0ml, drip 2 phenolphthalein (1.4), be neutralized to colourlessly with hydrochloric acid (1.3), after 2 of amounts, add 20ml buffer solution (1.6), boil 1min, insulation 2min drips 7 PAN indicator (1.5), is terminal point with copper sulphate standard solution (1.9) titration to blue (or aubergine).
Be calculated as follows the percentage composition of alundum (Al
In the formula: the concentration of C-EDTA standard solution, mol/L;
V
1The volume of-adding EDTA standard solution, ml;
V
2The excessive EDTA of-residual titration consumes the volume of copper sulphate standard solution, ml;
V
3-minute get the volume of test solution, ml;
V
4The volume of-constant volume, ml;
M-sample size, g.
The above; only be the preferable embodiment of the present invention; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to replacement or change according to technical scheme of the present invention and inventive concept thereof, all should be encompassed within protection scope of the present invention.
Claims (6)
1. the mensuration of metallic aluminium and alundum (Al in the slag is characterized in that:
Step 1: use the dissolving with hydrochloric acid slag, in the solution after filtration, add sodium hydrate solid, aluminium is sodium metaaluminate, and other metallic ions are precipitation of hydroxide and separate; In slightly acidic solution, add excessive EDTA standard solution, then in the presence of acetic acid-ammonium acetate, boil and make aluminium and EDTA all form complex, be indicator with PAN, with the EDTA of copper sulphate standard solution residual titration surplus to aubergine or blueness be terminal point, calculate the massfraction of metallic aluminium;
Step 2: with the residual residue after the step 1 filtration, behind ashing filter paper, sample mixed solvent fusion, hydrochloric acid leaching is after hydro-oxidation sodium solid separates, add excessive EDTA standard solution, then in the presence of acetic acid-ammonium acetate, boil and make aluminium and EDTA all form complex, be indicator with PAN, with the excessive EDTA of copper sulphate standard solution residual titration, calculate the massfraction of alundum (Al.
2. the mensuration of metallic aluminium and alundum (Al in the slag according to claim 1 is characterized in that: the method for making of EDTA standard solution: take by weighing 93gEDTA in the 10000ml volumetric flask, be diluted to scale with water, shake up.
3. the mensuration of metallic aluminium and alundum (Al in the slag according to claim 1 is characterized in that: acetic acid-ammonium acetate method for making, take by weighing the 77g ammonium acetate, and be dissolved in water, add the 5ml glacial acetic acid, be diluted to 1000ml with water.
4. the mensuration of metallic aluminium and alundum (Al in the slag according to claim 1, it is characterized in that: PAN is 0.1% ethanolic solution.
5. the mensuration of metallic aluminium and alundum (Al in the slag according to claim 1 is characterized in that: the method for making of copper sulphate standard solution, take by weighing 65g copper sulphate in the 10000ml volumetric flask, and add 5mL sulfuric acid, be diluted to scale with water, shake up.
6. the mensuration of metallic aluminium and alundum (Al in the slag according to claim 1, it is characterized in that: described mixed solvent is: 1.5 parts of natrium carbonicum calcinatums, the sodium tetraborate of 1.5 parts of sal tartari and 0.7 part.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104133036A (en) * | 2014-07-31 | 2014-11-05 | 中国冶金地质总局山东局测试中心 | Analysis determining method for aluminium oxide in bauxite |
| CN106248667A (en) * | 2016-08-23 | 2016-12-21 | 内蒙古包钢钢联股份有限公司 | A kind of Al-single crystal method in aluminium bronze |
| CN106323962A (en) * | 2016-08-18 | 2017-01-11 | 内蒙古包钢钢联股份有限公司 | Method for decomposing test sample for measuring aluminum in high-carbon silicon aluminum alloy |
| CN107621519A (en) * | 2017-09-26 | 2018-01-23 | 首钢集团有限公司 | A kind of assay method to metal aluminum content in magnesia carbon brick |
| CN108051542A (en) * | 2017-12-28 | 2018-05-18 | 唐山市德龙钢铁有限公司 | A kind of aluminum content tests method in silico-aluminum, silicon-aluminium-barium alloy |
| CN108152442A (en) * | 2017-12-08 | 2018-06-12 | 中国航发动力股份有限公司 | The method that sodium hydroxide separation-EDTA back titrations measure aluminium element in ferro-aluminum powder |
| CN108613975A (en) * | 2018-04-25 | 2018-10-02 | 山西建龙实业有限公司 | Pure aluminum assay method in a kind of wash heat material |
| CN109406715A (en) * | 2018-12-21 | 2019-03-01 | 鞍钢实业微细铝粉有限公司 | A kind of organic matter passivation aluminium powder active aluminium content detection method |
| CN110082249A (en) * | 2019-03-07 | 2019-08-02 | 中冶节能环保有限责任公司 | A kind of measuring method of steel slag original metal in the dreg iron content |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104133036A (en) * | 2014-07-31 | 2014-11-05 | 中国冶金地质总局山东局测试中心 | Analysis determining method for aluminium oxide in bauxite |
| CN106323962A (en) * | 2016-08-18 | 2017-01-11 | 内蒙古包钢钢联股份有限公司 | Method for decomposing test sample for measuring aluminum in high-carbon silicon aluminum alloy |
| CN106248667A (en) * | 2016-08-23 | 2016-12-21 | 内蒙古包钢钢联股份有限公司 | A kind of Al-single crystal method in aluminium bronze |
| CN107621519A (en) * | 2017-09-26 | 2018-01-23 | 首钢集团有限公司 | A kind of assay method to metal aluminum content in magnesia carbon brick |
| CN108152442A (en) * | 2017-12-08 | 2018-06-12 | 中国航发动力股份有限公司 | The method that sodium hydroxide separation-EDTA back titrations measure aluminium element in ferro-aluminum powder |
| CN108051542A (en) * | 2017-12-28 | 2018-05-18 | 唐山市德龙钢铁有限公司 | A kind of aluminum content tests method in silico-aluminum, silicon-aluminium-barium alloy |
| CN108613975A (en) * | 2018-04-25 | 2018-10-02 | 山西建龙实业有限公司 | Pure aluminum assay method in a kind of wash heat material |
| CN109406715A (en) * | 2018-12-21 | 2019-03-01 | 鞍钢实业微细铝粉有限公司 | A kind of organic matter passivation aluminium powder active aluminium content detection method |
| CN110082249A (en) * | 2019-03-07 | 2019-08-02 | 中冶节能环保有限责任公司 | A kind of measuring method of steel slag original metal in the dreg iron content |
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Application publication date: 20131009 |