CN1556401A - Special steel protective slag fusion point, fusion speed full fluorine analysis technology - Google Patents
Special steel protective slag fusion point, fusion speed full fluorine analysis technology Download PDFInfo
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- CN1556401A CN1556401A CNA2004100258170A CN200410025817A CN1556401A CN 1556401 A CN1556401 A CN 1556401A CN A2004100258170 A CNA2004100258170 A CN A2004100258170A CN 200410025817 A CN200410025817 A CN 200410025817A CN 1556401 A CN1556401 A CN 1556401A
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Abstract
Procedure for determining melting point and speed is as following: two samples in 10g each are prepared as column shape in 33mm; heating up one sample in high heat furnace in 5 deg.C, when the sample is in hemispherical molten state, the temperature is melting point; putting another sample into high heat furnace in 1350deg.C, when the sample is in hemispherical molten state, the time needed is melting speed. Procedure for determining whole content of fluorin is as following: putting dried sample 0.4g into 250ml distillation flask, adding 15m1 perchloric acid in 70%, 5 drops of dense phosphoric acid etc. till color of test solution is not non fading; distilling for half hour at 140 deg.C; then adding proper amount of alizarin red, NaOH, hydrochloric acid, methylene blue etc. determined by color of solution. Standard solution of zirconia is added till the solution is turned to tea-red so as to calculate whole fluorin.
Description
Affiliated technical field the present invention relates to a kind of analytical technology of special steel covering slag, belongs to the metallurgical analysis technical field.
The physical and chemical index of background technology special steel covering slag is its most basic attribute.Can it is related to form suitable slag structure, and a series of performance, as the ability of heat-insulating property, absorption foreign material, improves Ingot Surface Quality, prevents secondary oxidation etc.At present; domestic steel mill: as neat steel, comfort producers such as steel, Wuhan Iron and Steel Plant, Xixia covering slag factory; all adopt different sensing equipments and method to survey the fusing point of covering slag, molten speed, perfluor; the method of each producer and standard disunity; this has just caused covering slag of the same race different with analysis result under the diverse ways in different factories, and people urgently wish to have the standard analytical techniques of easy, accurate, the unified special steel covering slag of a kind of method.
Summary of the invention purpose of the present invention is exactly the standard analytical techniques that a kind of easy, accurate, fusing point of special steel covering slag that cost is low, molten speed, perfluor will be provided, and it is workable, adaptability is strong.
For achieving the above object, the technical scheme that the present invention takes is: a kind of special steel covering slag fusing point, molten speed, the perfluor analytical technology, it is characterized in that: its analysis test method is: take by weighing two parts of special steel covering slag sample 10g behind the calcination de-carbon respectively, be placed in 850 ℃-900 ℃ the muffle furnace calcination respectively 30 minutes, take out cooling back porphyrize to 180 order, add the water mixing, make how much shapes of φ 3 * 3mm then, 1. get a copy of it sample, put into high temperature furnace, the speed of heating by 5 ℃/min is heated, and till sample became hemispherical molten condition, the temperature of this moment was the fusing point of this covering slag; 2. get a duplicate samples in addition high temperature furnace is warming up to 1350 ℃ by the speed of heating of 5 ℃/min.And remain on 1350 ℃, and then sample is put into high temperature furnace, till sample is hemispherical molten condition, puts into high temperature furnace to sample from sample and be the required time of hemispherical molten condition, be the molten speed of this covering slag; 3. get the sample after a dried, insert in the 250ml cucurbit water, add the perchloric acid of 15ml70%, Dropwise 5 drips strong phosphoric acid again; Add again the potassium permanganate saturated solution to the test solution look colour-fast till, rubber stopper jam-pack bottleneck with the band thermometer, again with the blowhole on the rubber tube connection distilled water bottle and the venthole of steam bottle, and the venthole of cucurbit and condenser pipe, the end of condenser pipe is accepted distillate with triangular flask, heating also is controlled at 130 ℃-140 ℃ with the melt temperature in the cucurbit, distilled 20-30 minute, when distillate approximately remains the 150-200ml left and right sides, taking off triangular flask adds 1-2 and drips the sodium alizarinsulfonate indicator, NaOH liquation with 2% is neutralized to and is rose-colored, adding concentration then and be 1: 9 hydrochloric acid liquation neutralization is lemon yellow and crosses and add 3ml, add 4 sodium alizarinsulfonate indicator again, add 2-3 and drip the methine orchid, with the titration of zirconia standard liquation to test solution by the emerald green congo red that becomes; Can calculate the content of fluorine this moment.
The present invention is owing to adopt technique scheme, so make analytic process more easy, the result is more accurate, can realize the standardized work of special steel covering slag analytical technology, can measure the fusing point of special steel covering slag, molten speed, perfluor fast and accurately.Embodiment:
Embodiment 1: a kind of special steel covering slag fusing point, molten speed, perfluor technology, take two parts of special steel covering slag sample 10g behind the calcination de-carbon respectively, be placed in 850 ℃-900 ℃ the muffle furnace calcination respectively 30 minutes, take out cooling, porphyrize to 180 order, add mixing, after make the column of φ 3 * 3mm, 1. get a copy of it sample, put into high temperature furnace, the speed of heating by 5 ℃/min is heated, and till sample became hemispherical molten condition, the temperature of this moment was the fusing point of this covering slag; 2. get a duplicate samples in addition high temperature furnace is warming up to 1350 ℃ by the speed of heating of 5 ℃/min.And remain on 1350 ℃, then sample is put into high temperature furnace, until sample be hemispherical till, put into high temperature furnace to sample from sample and be the required time of hemispherical molten condition, be the molten speed of this covering slag; 3. get the sample after a dried, insert in the 250ml cucurbit water, add the perchloric acid of 15ml70%, Dropwise 5 drips strong phosphoric acid again; Add again the potassium permanganate saturated solution to the test solution look colour-fast till, rubber stopper jam-pack bottleneck with the band thermometer, again with the blowhole on the rubber tube connection distilled water bottle and the venthole of steam bottle, and the venthole of cucurbit and condenser pipe, the end of condenser pipe is accepted distillate with triangular flask, heating also is controlled at 130 ℃-140 ℃ with the melt temperature in the cucurbit, distilled 20-30 minute, about the approximately surplus 150-200ml of distillate, taking off triangular flask adds 1-2 and drips the sodium alizarinsulfonate indicator, NaOH liquation with 2% is neutralized to and is rose-colored, the hydrochloric acid liquation neutralization that adds concentration then and be 1: 9 is lemon yellow and adds 3ml, add 4 sodium alizarinsulfonate indicator again, add 2-3 and drip the methine orchid, with the titration of zirconia standard liquation to test solution by the emerald green congo red that becomes; Can calculate the content of perfluor this moment.
Embodiment 2: 1. preceding step partly reach, 2. with embodiment 1,3. gets the sample 0.3g after a drying is handled, and inserts in the 250ml distilled water bottle, adds the perchloric acid of 15ml70%, and Dropwise 5 drips strong phosphoric acid again; Add again the potassium permanganate saturated solution to the test solution look colour-fast till, rubber stopper jam-pack bottleneck with the band thermometer, again with the blowhole on the rubber tube connection distilled water bottle and the venthole of steam bottle, and the venthole of cucurbit and condenser pipe, the end of condenser pipe is accepted distillate with triangular flask, heating also is controlled at 130 ℃-140 ℃ with the melt temperature in the cucurbit, distilled 20-30 minute, about the approximately surplus 150-200ml of distillate, taking off triangular flask adds 1-2 and drips the sodium alizarinsulfonate indicator, NaOH liquation with 2% is neutralized to and is rose-colored, adding concentration then and be 1: 9 hydrochloric acid liquation neutralization is lemon yellow and crosses and add 3ml, add 4 sodium alizarinsulfonate indicator again, add 2-3 and drip the methine orchid, with the titration of zirconia standard liquation to test solution by the emerald green congo red that becomes; Can calculate the content of perfluor this moment.
This analysis technology has wide application value at covering slag factory, special steel plant.
Claims (1)
1, a kind of special steel covering slag fusing point, molten speed, perfluor analytical technology, it is characterized in that: its analysis test method is, take by weighing two parts of special steel covering slag sample 10g behind the calcination de-carbon respectively, being placed on 850 ℃ respectively---calcination is 30 minutes in 900 ℃ the muffle furnace, take out cooling back porphyrize to 180 order, add the water mixing, make how much shapes of φ 3 * 3mm then, 1. get a copy of it sample, put into high temperature furnace, the speed of heating by 5 ℃/min is heated, and till sample became hemispherical molten condition, the temperature of this moment was the fusing point of this covering slag; 2. get a duplicate samples in addition high temperature furnace is warming up to 1350 ℃ by the speed of heating of 5 ℃/min.And remain on 1350 ℃, and then sample is put into high temperature furnace, till sample is hemispherical molten condition, puts into high temperature furnace to sample from sample and be the required time of hemispherical molten condition, be the molten speed of this covering slag; 3. get the sample after a dried, insert in the 250ml cucurbit water, add the perchloric acid of 15ml70%, Dropwise 5 drips strong phosphoric acid again; Add again the potassium permanganate saturated solution to the test solution look colour-fast till, rubber stopper jam-pack bottleneck with the band thermometer, again with the blowhole on the rubber tube connection distilled water bottle and the venthole of steam bottle, and the venthole of cucurbit and condenser pipe, the end of condenser pipe is accepted distillate with triangular flask, heating also is controlled at 130 ℃ with the melt temperature in the cucurbit---and 140 ℃, distillation 20---30 minutes, distillate approximately remains 150---during the 200ml left and right sides, taking off triangular flask adds 1-2 and drips the sodium alizarinsulfonate indicator, NaOH liquation with 2% is neutralized to and is rose-colored, adding concentration then and be 1: 9 hydrochloric acid liquation neutralization is lemon yellow and crosses and add 3ml, add 4 sodium alizarinsulfonate indicator again, add 2-3 and drip the methine orchid, with the titration of zirconia standard liquation to test solution by the emerald green congo red that becomes; Can calculate the content of perfluor this moment.
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| CNA2004100258170A CN1556401A (en) | 2004-01-06 | 2004-01-06 | Special steel protective slag fusion point, fusion speed full fluorine analysis technology |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100547397C (en) * | 2006-01-18 | 2009-10-07 | 宝山钢铁股份有限公司 | A kind of method and apparatus of measuring the covering slag burn-off rate |
| CN101046456B (en) * | 2006-03-29 | 2010-08-11 | 宝山钢铁股份有限公司 | Process of detecting heat conductivity coefficient of protecting slag |
| CN102495096A (en) * | 2011-12-06 | 2012-06-13 | 首钢总公司 | Method for determining melting behavior and melting point of slag-like material |
| CN102721718A (en) * | 2012-06-11 | 2012-10-10 | 内蒙古包钢钢联股份有限公司 | Method for judging heat transfer property of liquid-state protecting slag in crystallizer |
| CN104407007A (en) * | 2014-12-16 | 2015-03-11 | 中南大学 | Method for determining melting temperature interval and melting behavior of metallurgical slag |
| CN110346508A (en) * | 2019-08-15 | 2019-10-18 | 武汉钢铁有限公司 | Villiaumite measurement device and measuring method in a kind of calcium-based desulfurizing agent |
| CN111721609A (en) * | 2020-05-18 | 2020-09-29 | 包头稀土研究院 | Pretreatment device and method for simultaneously treating multiple samples of hydrothermal distillation fluorine |
| CN112284971A (en) * | 2020-09-01 | 2021-01-29 | 包头钢铁（集团）有限责任公司 | Method for judging physical and chemical property stability of casting powder in casting process |
-
2004
- 2004-01-06 CN CNA2004100258170A patent/CN1556401A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100547397C (en) * | 2006-01-18 | 2009-10-07 | 宝山钢铁股份有限公司 | A kind of method and apparatus of measuring the covering slag burn-off rate |
| CN101046456B (en) * | 2006-03-29 | 2010-08-11 | 宝山钢铁股份有限公司 | Process of detecting heat conductivity coefficient of protecting slag |
| CN102495096A (en) * | 2011-12-06 | 2012-06-13 | 首钢总公司 | Method for determining melting behavior and melting point of slag-like material |
| CN102495096B (en) * | 2011-12-06 | 2013-06-26 | 首钢总公司 | Method for determining melting behavior and melting point of slag-like material |
| CN102721718A (en) * | 2012-06-11 | 2012-10-10 | 内蒙古包钢钢联股份有限公司 | Method for judging heat transfer property of liquid-state protecting slag in crystallizer |
| CN102721718B (en) * | 2012-06-11 | 2014-06-18 | 内蒙古包钢钢联股份有限公司 | Method for judging heat transfer property of liquid-state protecting slag in crystallizer |
| CN104407007A (en) * | 2014-12-16 | 2015-03-11 | 中南大学 | Method for determining melting temperature interval and melting behavior of metallurgical slag |
| CN110346508A (en) * | 2019-08-15 | 2019-10-18 | 武汉钢铁有限公司 | Villiaumite measurement device and measuring method in a kind of calcium-based desulfurizing agent |
| CN111721609A (en) * | 2020-05-18 | 2020-09-29 | 包头稀土研究院 | Pretreatment device and method for simultaneously treating multiple samples of hydrothermal distillation fluorine |
| CN112284971A (en) * | 2020-09-01 | 2021-01-29 | 包头钢铁（集团）有限责任公司 | Method for judging physical and chemical property stability of casting powder in casting process |
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