BS/EN 10181-2019 pdf download.Steels-Determination of lead content-Flame atomic absorption spectrometric method ( FAAS).
The following documents are referred to in the text in such a way that some or all of their content constitutes requirements of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.
EN ISO 648, Laboratory glassware — Single-volume pipettes (ISO 648)
EN ISO 1042, Laboratory glassware — One-mark volumetric flasks (ISO 1042)
EN ISO 14284, Steel and iron — Sampling and preparation of samples for the determination of chemical composition (ISO 14284)
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
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4 Principle
Dissolution of a test portion in hydrochloric acid followed by oxidation with nitric acid.
NOTE I Aqua regia can be used (or simultaneous dissolution and oxidation of the test portion.
Nehulization of the test solution into an air/acetylene flame of an atomic absorption spectrometer.
Spectrometric measurement of the atomic absorption of the 283,3 nm spectral line emthed by a lead hollow-cathode lamp.
NOTE 2 Other suitable radiation sources can also be used and measurements can also be carried out at 2 17,0 nm, provided the criteria in 622 and 6.2.3 are still met.
5 Reagents
During the analysis, use only reagents of recognized analytical grade and only distilled water or water of equivalent purity.
The following concentrations and amounts can be modified, provided the changes are taken into account in 8.3 and Clause 9.
5.1 Pure iron, with lead content < 0,00 1 %.
Cover with a watch glass. and, if necessary, heat gently to assist dissolution. When dissolution is complete boil to remove nitrogen oxides.
Allow to cool to room temperature and transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask. Dilute to the mark with water and mix.
1 ml of this solution contains 0,5 mg of lead.
5.5 Lead standard solution, 0.05 g/I.
Transfer 10,0 ml of lead standard solution (5.4) into a 100 ml one-mark volumetric flask. Dilute to the
mark with water and mhc.
Prepare this solution immediately prior to use.
1 ml of this solution contains 0.05 mg of lead.
5.6 Iron base solution, 40 g/1.
Weigh, to the nearest 0,01 g.. 10,00 g of pure iron (5.1) and transfer into a heat-resistant glassware of suitable size. Add 100 ml of hydrochloric acid (5.2). cover the glassware with a watch glass and heat gently until the reaction ceases. Oxidize with 20 ml of nitric acid (5.3). then boil the solution for 5 mm to remove nitrogen oxides.
Allow to cool and transfer the solution quantitatively into a 250 ml one-mark volumetric flask. Dilute to the mark with water and mix.
6 Apparatus
6.1 Ordinary laboratory apparatus
All volumetric glassware shall be class A, in accordance with EN ISO 648 or EN ISO 1042, as appropriate.
6.2 Atomic absorption spectrometer
6.2.1 General
The spectrometer shall be equipped with a lead hollow-cathode lamp or other suitable radiation source and supplied with air and acetylene sufficiently pure to give a steady clear fuel-lean flame, free from water and oil, and free from lead.
The atomic absorption spectrometer used Will be satisfactory if. after optimization according to 8.3.3, the limit of detection and characteristic concentration are in reasonable agreement with the values given by the manufacturer and it meets the performance criteria given in 6.2.2 and 6.2.3.
The standard deviation of 10 measurements of the absorbance of the most concentrated calibration solution shall not exceed 1.5 % of the mean absorbance of this solution.
The standard deviation of 10 measurements of the absorbance of the least concentrated calibration solution (excluding the zero member) shalt not exceed 0.5 % of the mean absorbance of the most concentrated calibration solution.
6.2.3 Additional performance requirements
6.2.3.1 General
The instrument should also conform to the additional performance requirements given in 6.2.3.2 and
6.2.3.3.
6.2.3.2 Characteristic concentration
The characteristic concentration tor lead in a matrix simlar to the fInal test solution shalt be lower than 0,6 ig/ml.
6.2.3.3 Limit of detection
The limit of detection is a number, expressed in units of concentration (or amount) that describes the lowest concentration level (or amount) of an element that can be determined to be statistically different from an analytical blank
The limit of detection of lead in a matrix similar to the final test solution shall be less than 0.3 pg/mI.
7 Sampling
Carry out sampling in accordance with EN ISO 14284 or appropriate national standards for steels.
8 Procedure
NOTE The following concentrations, amounts and glassware volumes can be modified, provided the changes are taken Into account In all appropriate subclauses of Clauses 8 and 9.
8.1 Test portion
Weigh to the nearest I mg,. approximately 2,0 g of the test sample.
8.2 Blank test
In parallel with the determination and following the same procedure, carry out a blank test using the same quantities of all reagents as used for the determination.BS/EN 10181-2019 pdf download.