CN102519997A - Automatic sampling and analyzing method of 4 types of slag samples in front of steel smelting furnace - Google Patents
Automatic sampling and analyzing method of 4 types of slag samples in front of steel smelting furnace Download PDFInfo
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Abstract
The invention discloses an automatic sampling and analyzing method of blast furnace slag, converter slag, refining slag and protecting slag in front of a steel smelting furnace. The method comprises steps that: (1) a sample requiring analysis is roughly crushed; (2) the roughly-crushed sample is washed, and is subject to slag-iron separation; a bonding agent is added to the separated slag sample, and the mixture is grinded; the grinded slag sample is washed, and is preserved for later use; (3) with an automatic wafer pressing machine, the sample is pressed into a wafer used in fluorescence analysis; and components in the slag sample are analyzed by using X-fluorescence spectrum. According to the invention, through experiments, optimal grinding parameters in the slag sample automatic sampling and analyzing method are obtained by screening. A cross-contamination problem possible to be caused by various steps such as grinding and pressing is avoided by ways of air cleaning, sample washing, bonding agent washing, and the like, such that analysis precision is ensured. Also, with the method, parameters such as optimal pressing pressure and pressure maintaining time are determined, such that slag samples can be successfully pressed into wafers. The prepared samples are uniform, complete, and firm. Data analysis is in time and accurate. With the method, automatic sampling and analyzing of the four slag samples are realized.
Description
Technical field
The present invention relates to 4 kinds of full-automatic sample preparations of slag specimen in smelting iron and steel stokehold and analytical approach; Relate in particular to the full-automatic sample preparation of slag specimen and the analytical approach of blast furnace slag, vessel slag, refining slag and covering slag before the steel-making, iron-smelting furnace, belong to the sample preparation and the analysis field of smelting iron and steel stokehold slag specimen.
Background technology
At present, Chinese home and abroad iron and steel enterprise adopts automatical analysis to accomplish the full-automatic specimen preparation of stokehold slag, scum and analyze to guarantee the promptness of sample analysis more.But owing to before steel-making, the iron-smelting furnace polytypes such as blast furnace slag, vessel slag, refining slag, covering slag being arranged; The difference of its chemical composition content is big; Make full-automatic slag specimen preparation system have the problem of cross pollution, the precision of slag specimen analysis and accuracy have all received influence, simultaneously because the type of slag specimen is different; The broken problem of print in the imperfect or analytic process of compressing tablet can appear in the part slag specimen when pressing appearance, can not realize the automatical analysis of same the multiple slag specimen of production line.
Summary of the invention
Technical matters to be solved by this invention is to overcome defectives such as precision that the existing automatical analysis that can not realize same the multiple slag specimen of production line in 4 kinds of full-automatic sample preparations of slag specimen in existing smelting iron and steel stokehold and the analytical approach and slag specimen analyze and accuracy be lower; A kind of full-automatic sample preparation of slag specimen and analytical approach of new smelting iron and steel stokehold blast furnace slag, vessel slag, refining slag and covering slag are provided; Imperfect, the print of existing compressing tablet is prone to problems such as fragmentation when cross pollution that this method has solved four kinds of slags when alternately analyzing and four kinds of slag specimens of a production flow analysis, realizes the automatical analysis of smelting iron and steel blast furnace slag, vessel slag, refining slag, four kinds of slag specimens of covering slag.
Technical problem to be solved by this invention realizes by the following technical programs:
The full-automatic sample preparation and the analytical approach of a kind of smelting iron and steel stokehold blast furnace slag, vessel slag, refining slag and covering slag may further comprise the steps:
(1) four kinds of slag specimen samples to be analyzed is slightly broken into particle;
(2) carrying out slag iron after the material after will slightly breaking cleans separates; Adding for the first time in the slag specimen sample after the separation, cementing agent grinds; Adding for the second time after the cleaning again, cementing agent grinds; Slag specimen after the grinding cleans, and is subsequent use;
(3) the resulting sample of step (2) is pressed into fluorescence analysis with full-automatic sheeter and uses disk; With SiO in the X-fluorescent spectroscopy slag specimen
2, CaO, MgO, AL
2O
3Or MnO composition.
In order to reach better technique effect, thick the breaking described in the step (1) is to adopt full-automatic disintegrating machine under following condition, to carry out fragmentation: the broken quantitatively volume 200-500ml of slag specimen, and broken time 5-10s, disintegrating machine is dry-cleaned time 5-10s.
Slag iron disengaging time described in the step (2) is preferably 20s; The cleaning time of Measuring glass is elected 10-20s again as; Wherein, cementing agent addition 0-3 grain for the first time, milling time 1-20s, cementing agent addition 0-15 grain for the second time, milling time 60-120s;
Said cleaning way in the step (2) is preferably dry-cleaning and purges, and the time of dry-cleaning purging is preferably 20-100s.
Granularity through the slag specimen after twice grinding in the step (2) is preferably the 120-200 order;
In the step (3) sample is pressed into fluorescence analysis when using disk with full-automatic sheeter, the pressure of sheeter is preferably 60KN-120KN, and the pressure rise time is preferably 5-9s; Dwell time is preferably 10-20s, and pressure is preferably 10-20s fall time, and the pressure range of decrease is preferably 20-50KN; The cleaning pressure head time is preferably 25-50s; The reinforced cup time of cleaning is preferably 25-50s, and the cleaning appearance ring time is preferably 8-16s, and the cleaning appearance cup time is preferably 20-60s.
When carrying out the X-fluorescent spectroscopy in the step (3), adopt all types of slag specimen standard models to do analytic curve separately, set analytical parameters is preferably: pipe stream 50-80KV, pipe is pressed 50-100mA, gate time 120-180s.
The present invention has obtained optimum abrasive parameters through a large amount of experiment screenings, has got rid of the cross-contamination issue that grinding and each step of compressing tablet possibly cause through modes such as air purge, sample cleaning, cementing agent cleanings, has guaranteed the analysis precision; In addition, the present invention has also screened parameters such as optimum film-making pressure, dwell time, makes four types of slag specimens all can accomplish compressing tablet; It is even, complete, firm to make sample; Analyze data in time, accurately, satisfy X-fluorescence spectrum automatical analysis, realized the full-automatic sample preparation and the analysis of smelting iron and steel stokehold blast furnace slag, vessel slag, refining slag, four kinds of slag specimens of covering slag; Four kinds of slag specimens are pressed into print quality height, and failure rate is low.
Description of drawings
Four kinds of slag specimen systems of Fig. 1 compressing tablet qualification rate sequence chart.
Embodiment
Further describe the present invention below in conjunction with specific embodiment, advantage of the present invention and characteristics will be more clear along with description.But these embodiment only are exemplary, scope of the present invention are not constituted any restriction.It will be understood by those skilled in the art that and down can make amendment with form or replace without departing from the spirit and scope of the present invention, but these modifications and replacing all fall within the scope of protection of the present invention the details of technical scheme of the present invention.
(1) slag specimen is carried out slightly breaking.The broken quantitatively volume 200ml of slag specimen is set, broken time 10s, disintegrating machine dry-cleaning time 10s.
(2) carrying out material cleaning → slag iron separation → cementing agent cleaning → improved grinding → grinding back cleans 5 flow processs, guarantees that process of lapping does not have cross pollution.Sample grinding machine tailing milling time 20s is set, Measuring glass cleaning time 20s, magnet disengaging time 20s, the cementing agent addition is 3 for the first time, milling time 20s, the cementing agent addition is 12 for the second time, milling time 120s, dry-cleaning purge time 100s.
(3) sample is carried out compressing tablet.It is 120KN that sheeter compressing tablet pressure is set, and the pressure rise time is 9s, dwell time 20s, pressure 20s fall time, pressure range of decrease 50KN, cleaning pressure head time 50s, the reinforced cup of cleaning time 50s, cleaning appearance ring time 16s, cleaning appearance cup time 60s.
(4) carry out the X-fluorescent spectroscopy.Adopt all types of slag specimen standard models to do analytic curve separately, analytical parameters is set: pipe stream 50KV, pipe is pressed 50mA, gate time 120s.
(5) through 4 kinds of slag specimen crossing operation tests.
After testing, each composition of blast furnace slag can reach following repeatability precision:
When CaO content was 40-50%, repeatability precision (standard deviation) was 0.1-0.3%; When MgO content was 5-10%, repeatability precision (standard deviation) was 0.05-0.15%; SiO
2When content was 30-40%, repeatability precision (standard deviation) was 0.1-0.25%; Al
2O
3When content was 10-20%, repeatability precision (standard deviation) was 0.05-0.15%.
After testing, each composition of vessel slag can reach following repeatability precision:
When CaO content was 40-50%, repeatability precision (standard deviation) was 0.06-0.25%; When MgO content was 10-20%, repeatability precision (standard deviation) was 0.08-0.20%; SiO
2When content was 10-20%, repeatability precision (standard deviation) was 0.05-0.20%; When TFe content was 10-20%, repeatability precision (standard deviation) was 0.08-0.15%.
After testing, each composition of refining slag can reach following repeatability precision:
When CaO content was 50-60%, repeatability precision (standard deviation) was 0.01-0.25%; When MgO content was 1-10%, repeatability precision (standard deviation) was 0.03-0.10%; SiO
2When content was 1-10%, repeatability precision (standard deviation) was 0.02-0.10%; Al
2O
3When content was 10-20%, repeatability precision (standard deviation) was 0.05-0.15%.
After testing, each composition of covering slag can reach following repeatability precision:
When CaO content was 30-40%, repeatability precision (standard deviation) was 0.05-0.25%; When MgO content was 5-15%, repeatability precision (standard deviation) was 0.05-0.15%; SiO
2When content was 30-40%, repeatability precision (standard deviation) was 0.06-0.30%; Al
2O
3When content was 10-20%, repeatability precision (standard deviation) was 0.06-0.20%.
(6) through test, the automatic compressing tablet accuracy of analysis of standard model situation is seen table 1.
The automatic compressing tablet accuracy of analysis of 4 kinds of standard models of table 1
(7) automatic compressing tablet running situation
Through test, stable being controlled at more than 99% of slag specimen system compressing tablet serviceability rate in year June in July, 2010-2011,12 monthly average reach 99.39%, and concrete condition is seen shown in Figure 1.
(1) slag specimen is carried out slightly breaking.The broken quantitatively volume 500ml of slag specimen is set, broken time 5s, disintegrating machine dry-cleaning time 5s.
(2) carrying out material cleaning → slag iron separation → cementing agent cleaning → improved grinding → grinding back cleans 5 flow processs, guarantees that process of lapping does not have cross pollution.Sample grinding machine tailing milling time 10s is set, Measuring glass cleaning time 10s, magnet disengaging time 20s, the cementing agent addition is 2 for the first time, milling time 10s, the cementing agent addition is 5 for the second time, milling time 80s, dry-cleaning purge time 40s.
(3) sample is carried out compressing tablet.It is 60KN that sheeter compressing tablet pressure is set, and the pressure rise time is 5s, dwell time 10s, pressure 10s fall time, pressure range of decrease 20KN, cleaning pressure head time 25s, the reinforced cup of cleaning time 25s, cleaning appearance ring time 8s, cleaning appearance cup time 20s.
(4) carry out the X-fluorescent spectroscopy.Adopt all types of slag specimen standard models to do analytic curve separately, analytical parameters is set: pipe stream 50KV, pipe is pressed 50mA, gate time 120s.
(5) through 4 kinds of slag specimen crossing operation tests,
After testing, each composition of blast furnace slag can reach following repeatability precision:
When CaO content was 40-50%, repeatability precision (standard deviation) was 0.1-0.31%; When MgO content was 5-10%, repeatability precision (standard deviation) was 0.04-0.15%; SiO
2When content was 30-40%, repeatability precision (standard deviation) was 0.1-0.26%; Al
2O
3When content was 10-20%, repeatability precision (standard deviation) was 0.04-0.15%.
After testing, each composition of vessel slag can reach following repeatability precision:
When CaO content was 40-50%, repeatability precision (standard deviation) was 0.06-0.26%; When MgO content was 10-20%, repeatability precision (standard deviation) was 0.09-0.20%; SiO
2When content was 10-20%, repeatability precision (standard deviation) was 0.04-0.20%; When TFe content was 10-20%, repeatability precision (standard deviation) was 0.09-0.16%.
After testing, each composition of refining slag can reach following repeatability precision:
When CaO content was 50-60%, repeatability precision (standard deviation) was 0.012-0.26%; When MgO content was 1-10%, repeatability precision (standard deviation) was 0.032-0.10%; SiO
2When content was 1-10%, repeatability precision (standard deviation) was 0.025-0.10%; Al
2O
3When content was 10-20%, repeatability precision (standard deviation) was 0.04-0.152%.
After testing, each composition of covering slag can reach following repeatability precision:
When CaO content was 30-40%, repeatability precision (standard deviation) was 0.05-0.27%; When MgO content was 5-16%, repeatability precision (standard deviation) was 0.053-0.15%; SiO
2When content was 30-40%, repeatability precision (standard deviation) was 0.055-0.30%; Al
2O
3When content was 10-20%, repeatability precision (standard deviation) was 0.05-0.20%.
(6) through test, the automatic compressing tablet accuracy of analysis of standard model is seen table 2.
The automatic compressing tablet accuracy of analysis of 4 kinds of standard models of table 2
(7) automatic compressing tablet running situation
Through test, stable being controlled at more than 99% of slag specimen system compressing tablet serviceability rate in year June in July, 2010-2011,12 monthly average reach 99.41%.
(1) slag specimen is carried out slightly breaking.The broken quantitatively volume 400ml of slag specimen is set, broken time 8s, disintegrating machine dry-cleaning time 8s.
(2) carrying out material cleaning → slag iron separation → cementing agent cleaning → improved grinding → grinding back cleans 5 flow processs, guarantees that process of lapping does not have cross pollution.Sample grinding machine tailing milling time 15s is set, Measuring glass cleaning time 15s, magnet disengaging time 20s, the cementing agent addition is 1 for the first time, milling time 1s, the cementing agent addition is 1 for the second time, milling time 60s, dry-cleaning purge time 20s.
(3) sample is carried out compressing tablet.It is 90KN that sheeter compressing tablet pressure is set, and the pressure rise time is 7s, dwell time 15s, pressure 15s fall time, pressure range of decrease 40KN, cleaning pressure head time 40s, the reinforced cup of cleaning time 40s, cleaning appearance ring time 12s, cleaning appearance cup time 40s.
(4) carry out the X-fluorescent spectroscopy.Adopt all types of slag specimen standard models to do analytic curve separately, analytical parameters is set: pipe stream 50KV, pipe is pressed 50mA, gate time 120s.
(5) through 4 kinds of slag specimen crossing operation tests,
After testing, each composition of blast furnace slag can reach following repeatability precision:
When CaO content was 40-50%, repeatability precision (standard deviation) was 0.08-0.25%; When MgO content was 5-10%, repeatability precision (standard deviation) was 0.04-0.12%; SiO
2When content was 30-40%, repeatability precision (standard deviation) was 0.12-0.22%; Al
2O
3When content was 10-20%, repeatability precision (standard deviation) was 0.055-0.12%.
After testing, each composition of vessel slag can reach following repeatability precision:
When CaO content was 40-50%, repeatability precision (standard deviation) was 0.05-0.21%; When MgO content was 10-20%, repeatability precision (standard deviation) was 0.07-0.18%; SiO
2When content was 10-20%, repeatability precision (standard deviation) was 0.06-0.19%; When TFe content was 10-20%, repeatability precision (standard deviation) was 0.085-0.14%.
After testing, each composition of refining slag can reach following repeatability precision:
When CaO content was 50-60%, repeatability precision (standard deviation) was 0.012-0.20%; When MgO content was 1-10%, repeatability precision (standard deviation) was 0.03-0.09%; SiO
2When content was 1-10%, repeatability precision (standard deviation) was 0.022-0.14%; Al
2O
3When content was 10-20%, repeatability precision (standard deviation) was 0.04-0.12%.
After testing, each composition of covering slag can reach following repeatability precision:
When CaO content was 30-40%, repeatability precision (standard deviation) was 0.05-0.20%; When MgO content was 5-15%, repeatability precision (standard deviation) was 0.05-0.12%; SiO
2When content was 30-40%, repeatability precision (standard deviation) was 0.06-0.25%; Al
2O
3When content was 10-20%, repeatability precision (standard deviation) was 0.06-0.18%.
(6) through test, the automatic compressing tablet accuracy of analysis of standard model situation is seen table 3.
The automatic compressing tablet accuracy of analysis of 4 kinds of standard models of table 3
(7) automatic compressing tablet running situation
Through test, stable being controlled at more than 99.2% of slag specimen system compressing tablet serviceability rate in year June in July, 2010-2011,12 monthly average reach 99.52%.
Claims (10)
1. the full-automatic sample preparation and the analytical approach of a smelting iron and steel stokehold blast furnace slag, vessel slag, refining slag and covering slag may further comprise the steps:
(1) four kinds of slag specimen samples to be analyzed is slightly broken into particle;
(2) carrying out slag iron after the sample after will slightly breaking cleans separates; Adding for the first time in the slag specimen sample after the separation, cementing agent grinds; Adding for the second time after the cleaning again, cementing agent grinds; Slag specimen after the grinding cleans, and is subsequent use;
(3) the resulting sample of step (2) is pressed into fluorescence analysis with full-automatic sheeter and uses disk; With X-fluorescent spectroscopy SiO wherein
2, CaO, MgO, AL
2O
3Or MnO composition.
2. according to described full-automatic sample preparation of claim 1 and analytical approach, it is characterized in that thick the breaking described in the step (1) is to adopt full-automatic disintegrating machine to carry out fragmentation.
3. according to described full-automatic sample preparation of claim 2 and analytical approach; It is characterized in that: described thick breaking is to adopt full-automatic disintegrating machine under following condition, slag specimen sample to be analyzed slightly to be broken into particle: the broken quantitatively volume 200-500ml of slag specimen; Broken time 5-10s, disintegrating machine dry-cleaning time 5-10s.
4. according to described full-automatic sample preparation of claim 1 and analytical approach, it is characterized in that: the slag iron disengaging time described in the step (2) is 20s; The cleaning time of Measuring glass is 10-20s.
5. according to described full-automatic sample preparation of claim 1 and analytical approach, it is characterized in that: the middle cementing agent addition for the first time of step (2) is the 0-3 grain, and milling time is 1-20s, and the cementing agent addition is the 0-15 grain for the second time, and milling time is 60-120s.
6. according to described full-automatic sample preparation of claim 1 and analytical approach, it is characterized in that: the said cleaning in the step (2) is to adopt dry-cleaning to purge.
7. according to described full-automatic sample preparation of claim 6 and analytical approach, it is characterized in that: said dry-cleaning purge time is 20-100s.
8. according to described full-automatic sample preparation of claim 1 and analytical approach, it is characterized in that: the granularity through the slag specimen after twice grinding in the step (2) is the 120-200 order.
9. according to described full-automatic sample preparation of claim 1 and analytical approach, it is characterized in that: in the step (3) sample is pressed into fluorescence analysis when using disk with full-automatic sheeter, the pressure of sheeter is 60KN-120KN; The pressure rise time is 5-9s, and the dwell time is 10-20s, and pressure fall time is 10-20s; The pressure range of decrease is 20-50KN, and the cleaning pressure head time is 25-50s, and the reinforced cup time of cleaning is 25-50s; The cleaning appearance ring time is 8-16s, and the cleaning appearance cup time is 20-60s.
10. according to described full-automatic sample preparation of claim 1 and analytical approach; It is characterized in that: when carrying out the X-fluorescent spectroscopy in the step (3); Adopt all types of slag specimen standard models to do analytic curve separately, wherein, set analytical parameters is: pipe stream 50-80KV; Pipe is pressed 50-100mA, and gate time is 120-180s.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102854210A (en) * | 2012-08-28 | 2013-01-02 | 芜湖新兴铸管有限责任公司 | X fluorescence analysis method of iron ores |
| CN104655516A (en) * | 2015-03-19 | 2015-05-27 | 岑溪市东正动力科技开发有限公司 | Determination method for content of copper in copper smelting furnace slag |
| CN104897444A (en) * | 2015-05-21 | 2015-09-09 | 桂林理工大学 | Pretreatment method used before test of total rock components of basalt |
| CN109342478A (en) * | 2018-11-28 | 2019-02-15 | 南京钢铁股份有限公司 | A kind of method of quick Fabrication clinker tabletting |
| CN112051355A (en) * | 2020-09-07 | 2020-12-08 | 北京首钢股份有限公司 | Detection and analysis method for steel smelting solid waste |
| CN113514487A (en) * | 2021-07-09 | 2021-10-19 | 中国一冶集团有限公司 | X-ray fluorescence analysis method for blast furnace slag, converter slag, electric furnace slag or open slag |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102854210A (en) * | 2012-08-28 | 2013-01-02 | 芜湖新兴铸管有限责任公司 | X fluorescence analysis method of iron ores |
| CN104655516A (en) * | 2015-03-19 | 2015-05-27 | 岑溪市东正动力科技开发有限公司 | Determination method for content of copper in copper smelting furnace slag |
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| CN109342478A (en) * | 2018-11-28 | 2019-02-15 | 南京钢铁股份有限公司 | A kind of method of quick Fabrication clinker tabletting |
| CN112051355A (en) * | 2020-09-07 | 2020-12-08 | 北京首钢股份有限公司 | Detection and analysis method for steel smelting solid waste |
| CN113514487A (en) * | 2021-07-09 | 2021-10-19 | 中国一冶集团有限公司 | X-ray fluorescence analysis method for blast furnace slag, converter slag, electric furnace slag or open slag |
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Application publication date: 20120627 |
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