Steel - Determination of aluminium content - Flame atomic absorption spectrometric method (ISO 9658:1990)

The method is applicable to the determination of acid-soluble and/or total aluminium content between 0,005 % (m/m) and 0,20 % (m/m). Specifies definition, principle, reagents, apparatus, sampling, procedure, expression of results and test report. The annexes give additional information on the international co-operative tests, a graphical representation of precision data and procedures for the determination of instrumental criteria.

Stahl - Bestimmung des Aluminiumgehalts - Spektralfotometrische Atomabsorptionsmethode (ISO 9658:1990)

Aciers - Dosage de l'aluminium - Méthode par spectrométrie d'absorption atomique dans la flamme (ISO 9658:1990)

La présente Norme internationale prescrit une méthode de dosage par spectrométrie d'absorption atomique dans la flamme, de l'aluminium soluble dans l'acide et/ou l'aluminium total dans les aciers non alliés. La méthode est applicable aux teneurs en aluminium comprises entre 0,005 % (m/m) et 0,20 % (m/m).

Jeklo - Določevanje aluminija - Metoda s plamensko atomsko apsorpcijsko sprektrometrično metodo (ISO 9658:1990)

General Information

Status
Published
Publication Date
19-Dec-1991
Current Stage
9093 - Decision to confirm - Review Enquiry
Start Date
03-Jun-2009
Completion Date
03-Jun-2009

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EN 29658:1997
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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.FLMVNRStahl - Bestimmung des Aluminiumgehalts - Spektralfotometrische Atomabsorptionsmethode (ISO 9658:1990)Aciers - Dosage de l'aluminium - Méthode par spectrométrie d'absorption atomique dans la flamme (ISO 9658:1990)Steel - Determination of aluminium content - Flame atomic absorption spectrometric method (ISO 9658:1990)77.080.20JeklaSteels77.040.30Kemijska analiza kovinChemical analysis of metalsICS:Ta slovenski standard je istoveten z:EN 29658:1991SIST EN 29658:1997en01-december-1997SIST EN 29658:1997SLOVENSKI
STANDARD



SIST EN 29658:1997



SIST EN 29658:1997



SIST EN 29658:1997



SIST EN 29658:1997



SIST EN 29658:1997



SIST EN 29658:1997



SIST EN 29658:1997



SIST EN 29658:1997



IS0 9658:1990(E) 8.3.1.3 Preparation of the test solution for the determination of acid-soluble aluminium If acid-soluble aluminium only is required, add 5,0 ml of fusion mixture solution (5.8) to the 100 ml one-mark volumetric flask, cool, and allow any car- bon dioxide produced to escape, then dilute to the mark with water and mix. Discard the insoluble res- idue and cellulose nitrate filter. Retain this solution for the determination of acid-soluble aluminium. 8.3.1.4 Preparation of the test solution for the determlnatlon of total aluminium Transfer the filter containing the insoluble residue into a platinum crucible (6.4). Char the residue at low temperature and ignite slowly to 1000 “C. Cool the crucible. Add several drops of water, several drops of sulfuric acid (5.5) and 5 ml of hydrofluoric acid (5.2). Evaporate to dryness and again ignite slowly to 1000 “C. Cool the crucible and add I,0 g of the fusion mixture (5.7). Fuse the contents of the crucible in a muffle furnace at 1000 “C for 15 min. Cool the crucible and add 1 ml or 2 ml of hydrochloric acid (5.3) and 8 ml of water to the solidified melt. Heat gently to dissolve the fusion products. Allow the crucible to cool and transfer the solution quantitatively to the filtrate in the 100 ml one-mark volumetric flask. Dilute to the mark with water and mix. Retain this solution for the determination of total aluminium. 8.3.2 Preparation of the calibration solutions 8.3.2.1 Aluminium contents c 0,010 % (m/m) Introduce into a series of five 250 ml beakers (2,00 + 0,Ol) g of the pure iron (5.1). Add 40 ml of acid mixture (5.6) in small portions, to each beaker and cover them with watch-glasses. Heat until the iron is in solution, then boil to eliminate oxides of nitrogen. Cool and transfer the solutions into five 100 ml one-mark volumetric flasks. Using a burette add the volumes of aluminium standard sol- ution B (5.9.3) as indicated in table 1. Add 5,0 ml of fusion mixture solution (5.8) to each flask. Cool and allow any carbon dioxide produced to escape, then dilute to the mark with water and mix. I Table I Volume of alu- Corresponding minium stand- concentration of ard solution B aluminium in (5.9.3) final test sol- ution ml jLg/ml 0 1) 0 295 03 50 190 795 13 IO,0 290 1) Zero member. Corresponding content of alu- minium in test sample O/o (m/m) 0,000 0 0,0025 0,005o 0,0075 0,0100 8.3.2.2 Aluminium content between 0,010 % (m/m) and 0,20 % (m/m) Proceed as specified in 8.3.2.1, using table 2 instead of table 1. Table 2 Volume of alu- Corresponding minium stand- concentration of Corresponding aluminium in content of alu- ard solution A minium in test (5.9.2) final test sol- ution sample ml jlg/mi O/O (m/m) 0 1) 0 0,000 590 IO,0 0,050 IO,0 20,o 0,100 15,o 30,o 0,150 20,o 40,o 0,200 1) Zero member. 8.3.3 Adjustment of atomic absorption spectrometer See table 3. 8.3.4 Optlmlzlng the atomic absorption spectrometer settings Follow the manufacture the instrument for use. r’s instructions for preparing When the current to the lamp, the wavelength and the flow of gas have been adjusted and the burner lit, spray water until the indication has stabilized. 4 SIST EN 29658:1997



IS0 9658:1990(E) Element Type of lamp Wavelength Flame Lamp current Bandwidth Background correction Table 3 Characteristic Aluminium hollow cathode. 309,3 nm Dinitrogen monoxide-acetylene non-luminous oxidizing flame. The height of the red-feather flame shall be 10 mm to 20 mm adjusted for maximum aluminium response. Follow manufacturer’s recommendations. Follow manufacturer’s recommendations. If no recommendation is stated, a bandwidth between 0,2 nm and 0,7 nm is suggested. If the zero member gives an absorbance comparable with the precision of the lowest calibration solution, background correction may be required. WARNING - The manufacturer’s recommendations should be closely followed and particular attention is drawn to the following safety points: a) the explosive nature of acetylene, and regulations concerning its use; b) the need to shield the eyes of the operator from ultraviolet radiation by means of tinted glass; c) the need to keep the burner head clear of deposits because a badly
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