GB2186686A - Method and apparatus for determination of soluble aluminium in steel - Google Patents

Method and apparatus for determination of soluble aluminium in steel Download PDF

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Publication number
GB2186686A
GB2186686A GB08630256A GB8630256A GB2186686A GB 2186686 A GB2186686 A GB 2186686A GB 08630256 A GB08630256 A GB 08630256A GB 8630256 A GB8630256 A GB 8630256A GB 2186686 A GB2186686 A GB 2186686A
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GB
United Kingdom
Prior art keywords
sample
aluminium
steel
cell
soluble aluminium
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Granted
Application number
GB08630256A
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GB2186686B (en
GB8630256D0 (en
Inventor
Carlos Augusto Coutinho
Elpidio Cosenza Arruda
Edouard Hugues Braun
Wilton Pachaco De Araujo
Elias Ayras Guidetti Zagatto
Henrique Filho Bergami
Francisco Jose Krug
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MINAS GERAIS SIDERURG
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MINAS GERAIS SIDERURG
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Publication of GB8630256D0 publication Critical patent/GB8630256D0/en
Publication of GB2186686A publication Critical patent/GB2186686A/en
Application granted granted Critical
Publication of GB2186686B publication Critical patent/GB2186686B/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/416Systems
    • G01N27/42Measuring deposition or liberation of materials from an electrolyte; Coulometry, i.e. measuring coulomb-equivalent of material in an electrolyte
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/20Metals
    • G01N33/205Metals in liquid state, e.g. molten metals

Abstract

According to the invention a steel sample (1) connected as anode is dissolved in an electrochemical cell (2) a sample of the solution is analysed in a spectrophotometry system (3) and the analysis results processed in a microcomputer (4) to provide better accuracy and reliability than conventionally obtainable. <IMAGE>

Description

SPECIFICATION Method and apparatus for determination of soluble aluminium in steel This invention relates to the determination of soluble aluminium in steel.
The analysis of soluble aluminium in solid samples of steel usually starts with acid solubilization of the sample, followed by determination of aluminium by molecular absorption or atomic absorption spectrophotometry or by inductively coupled plasma techniques. The average time taken for aluminium determination by these methods is in excess of 20 minutes, which is unacceptable for use in monitoring metallurgical processes. The basic reason for this long analysis time is the time taken to prepare the sample, i.e. withdrawing filings of the metal, weighing them and solubilizing them in hot mineral acid.
Another technique for aluminium determination uses optical emission spectrometry which determines only the total aluminium content, the soluble aluminium content then being estimated on the basis of correlation between total aluminium and soluble aluminium determined by the methods described above. However, optical emission spectrometry, although having an appropriate response time, does not give an accurate estimate of soluble aluminium due to the presence of heterogeneously distributed aluminium particles in the sample affecting determination of total aluminium content.
This invention was developed in order to obviate various disadvantages of the conventional processes which make it impossible to determine the soluble aluminium content in a time compatible with metallurgical process control requirements.
In accordance with the invention, there is provided a method for determining soluble aluminium in steel comprising the steps of dissolving a sample of steel containing soluble aluminium in an electrochemical cell analysing spectrophotometrically a sample of the solution from the cell and generating an output signal indicative of dissolved aluminium in the sample of solution and processing the data contained in the output signal and displaying the processed data in visual form as the content of soluble aluminium in the sample of steel.
The present invention provides also apparatus for the determination of soluble aluminium in steel comprising an electrochemical cell for dissolving a sample of steel containing soluble aluminium a spectrophotometer operatively connected to the cell for spectrophotometrically analysing a sample of solution from the cell and for generating an output signal indicative of dissolved aluminium in the sample of solution and means for processing the data contained in the output signal and for displaying the processed data in visual form as the content of soluble aluminium in the sample of steel.
Suitably, the electrochemical cell is capable of dissolving the steel sample without the sample having been subjected to any prior treatment, in iess than 60 seconds.
In this respect, the cell is preferably one in which the steel sample is connected as anode and which operates continuously with an electrolyte solution flowing continuously through the cell. An example of such a cell, which may be used in practicing the invention, is described in greater detail in Brazilian Patent Application Pl 8500929. The electrolyte from the cell, after having been degassed to remove dissolved or entrained gases produced during electrolysis, is then passed to the spectrophotometry system.
The spectrophotometry system is preferably a flux injection spectrophotometry system which quantifies the aluminium present in the solution provided by the cell, and is suitably associated with a microcomputer operative to check the cell and spectrophotometry system and to process the resulting data so as to provide the analysis results directly as a percentage of soluble aluminium in the metal sample through the agency of an indicator and/or a printer.
The apparatus according to the invention is illustrated diagramatically in the accompanying drawing. With reference to the drawing, a sample of steel to be analysed is connected as anode 1 in an electrochemical cell 2 provided with a DC power source, and the resulting solution, after being degassed, is passed to a spectrophotometer 3. An output signal from the spectrophotometer is passed to a microcomputer 4 and is processed to provide a direct indication of soluble aluminium content of the original steel sample, which is displayed on indicator 5 and/or printer 6.
Determination of soluble aluminium by the method according to the invention is more accurate and sensitive than that provided by conventional methods and takes at most 60 seconds; it is therefore very well suited to metallurgical process control requirements.
1. A method for determining soluble aluminium in steel comprising the steps of dissolving a sample of steel containing soluble aluminium in an electrochemical cell analysing spectrophotometrically a sample of the solution from the cell and generating an output signal indicative of dissolved aluminium in the sample of solution and processing the data contained in the output signal and displaying the processed data in visual form as the content of soluble aluminium in the sample of steel.
2. A method according to claim 1, wherein the sample of steel is dissolved in a period of
**WARNING** end of DESC field may overlap start of CLMS **.

Claims (4)

**WARNING** start of CLMS field may overlap end of DESC **. SPECIFICATION Method and apparatus for determination of soluble aluminium in steel This invention relates to the determination of soluble aluminium in steel. The analysis of soluble aluminium in solid samples of steel usually starts with acid solubilization of the sample, followed by determination of aluminium by molecular absorption or atomic absorption spectrophotometry or by inductively coupled plasma techniques. The average time taken for aluminium determination by these methods is in excess of 20 minutes, which is unacceptable for use in monitoring metallurgical processes. The basic reason for this long analysis time is the time taken to prepare the sample, i.e. withdrawing filings of the metal, weighing them and solubilizing them in hot mineral acid. Another technique for aluminium determination uses optical emission spectrometry which determines only the total aluminium content, the soluble aluminium content then being estimated on the basis of correlation between total aluminium and soluble aluminium determined by the methods described above. However, optical emission spectrometry, although having an appropriate response time, does not give an accurate estimate of soluble aluminium due to the presence of heterogeneously distributed aluminium particles in the sample affecting determination of total aluminium content. This invention was developed in order to obviate various disadvantages of the conventional processes which make it impossible to determine the soluble aluminium content in a time compatible with metallurgical process control requirements. In accordance with the invention, there is provided a method for determining soluble aluminium in steel comprising the steps of dissolving a sample of steel containing soluble aluminium in an electrochemical cell analysing spectrophotometrically a sample of the solution from the cell and generating an output signal indicative of dissolved aluminium in the sample of solution and processing the data contained in the output signal and displaying the processed data in visual form as the content of soluble aluminium in the sample of steel. The present invention provides also apparatus for the determination of soluble aluminium in steel comprising an electrochemical cell for dissolving a sample of steel containing soluble aluminium a spectrophotometer operatively connected to the cell for spectrophotometrically analysing a sample of solution from the cell and for generating an output signal indicative of dissolved aluminium in the sample of solution and means for processing the data contained in the output signal and for displaying the processed data in visual form as the content of soluble aluminium in the sample of steel. Suitably, the electrochemical cell is capable of dissolving the steel sample without the sample having been subjected to any prior treatment, in iess than 60 seconds. In this respect, the cell is preferably one in which the steel sample is connected as anode and which operates continuously with an electrolyte solution flowing continuously through the cell. An example of such a cell, which may be used in practicing the invention, is described in greater detail in Brazilian Patent Application Pl 8500929. The electrolyte from the cell, after having been degassed to remove dissolved or entrained gases produced during electrolysis, is then passed to the spectrophotometry system. The spectrophotometry system is preferably a flux injection spectrophotometry system which quantifies the aluminium present in the solution provided by the cell, and is suitably associated with a microcomputer operative to check the cell and spectrophotometry system and to process the resulting data so as to provide the analysis results directly as a percentage of soluble aluminium in the metal sample through the agency of an indicator and/or a printer. The apparatus according to the invention is illustrated diagramatically in the accompanying drawing. With reference to the drawing, a sample of steel to be analysed is connected as anode 1 in an electrochemical cell 2 provided with a DC power source, and the resulting solution, after being degassed, is passed to a spectrophotometer 3. An output signal from the spectrophotometer is passed to a microcomputer 4 and is processed to provide a direct indication of soluble aluminium content of the original steel sample, which is displayed on indicator 5 and/or printer 6. Determination of soluble aluminium by the method according to the invention is more accurate and sensitive than that provided by conventional methods and takes at most 60 seconds; it is therefore very well suited to metallurgical process control requirements. CLAIMS
1. A method for determining soluble aluminium in steel comprising the steps of dissolving a sample of steel containing soluble aluminium in an electrochemical cell analysing spectrophotometrically a sample of the solution from the cell and generating an output signal indicative of dissolved aluminium in the sample of solution and processing the data contained in the output signal and displaying the processed data in visual form as the content of soluble aluminium in the sample of steel.
2. A method according to claim 1, wherein the sample of steel is dissolved in a period of time of less than 60 seconds.
3. Apparatus for the determination of soluble aluminium in steel comprising an electrochemical cell for dissolving a sample of steel containing soluble aluminium a spectrophotometer operatively connected to the cell for spectrophotometrically analysing a sample of solution from the cell and for generating an output signal indicative of dissolved aluminium in the sample of solution and means for processing the data contained in the output signal and for displaying the processed data in visual form as the content of soluble aluminium in the sample of steel.
4. Apparatus according to claim 3 substantially as herein described with reference to the accompanying drawing.
GB8630256A 1985-12-18 1986-12-18 Method and apparatus for determination of soluble aluminium in steel Expired - Fee Related GB2186686B (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
BR8506355A BR8506355A (en) 1985-12-18 1985-12-18 APPLIANCE FOR FAST DETERMINATION OF ALUMINUM SOLUBLE IN ACOS

Publications (3)

Publication Number Publication Date
GB8630256D0 GB8630256D0 (en) 1987-01-28
GB2186686A true GB2186686A (en) 1987-08-19
GB2186686B GB2186686B (en) 1990-04-18

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GB8630256A Expired - Fee Related GB2186686B (en) 1985-12-18 1986-12-18 Method and apparatus for determination of soluble aluminium in steel

Country Status (6)

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JP (1) JPS62195541A (en)
KR (1) KR880008022A (en)
BR (1) BR8506355A (en)
DE (1) DE3643385A1 (en)
FR (1) FR2591749B1 (en)
GB (1) GB2186686B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106769300B (en) * 2016-12-13 2019-07-30 班俊生 The effective measuring method of aluminium and activated silica in a kind of gibbsitic bauxite

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2513345C2 (en) * 1975-03-26 1976-09-30 Kloeckner Werke Ag DEVICE FOR THE SPECTRAL ANALYTICAL DETERMINATION OF THE ALLOY COMPONENTS OF MATERIAL SAMPLES MADE OF METAL
JPS5242190A (en) * 1975-09-30 1977-04-01 Nippon Steel Corp Method and apparatus for automatic electrolysis, extraction and separa tion of nonmetal inclusions in metal
DE3029038C2 (en) * 1980-07-31 1982-06-09 Krupp Stahl Ag, 4630 Bochum Device for the spectral analysis of the chemical composition of metallic workpieces
ATE21559T1 (en) * 1980-10-10 1986-09-15 Cockerill Sambre Sa METHOD OF PREPARATION OF STEEL SAMPLES.
JPS57116253A (en) * 1981-01-10 1982-07-20 Nippon Steel Corp Electrolytic extraction separating method for substance included in metal
BR8204408A (en) * 1982-07-28 1984-03-07 Siderurgica Nacional Sa ELECTROLYTIC DISSOLUTION APPLIANCE FOR ANALYSIS OF SOLUBLE STEEL ALUMINUM
DE3344944C2 (en) * 1983-12-13 1986-06-05 Knieps & Pöckler, 5828 Ennepetal Method for analyzing steel during its manufacture and further processing

Also Published As

Publication number Publication date
GB2186686B (en) 1990-04-18
DE3643385A1 (en) 1987-07-30
BR8506355A (en) 1987-07-07
KR880008022A (en) 1988-08-30
FR2591749A1 (en) 1987-06-19
JPS62195541A (en) 1987-08-28
GB8630256D0 (en) 1987-01-28
FR2591749B1 (en) 1992-09-11

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Effective date: 19961218