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BSI PD CEN/TR 10362:2014

BSI PD CEN/TR 10362:2014

$142.49

Chemical analysis of ferrous materials. Determination of selenium in steels. Electrothermal atomic absorption spectrometric method

Published By Publication Date Number of Pages
BSI 2014 24
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This Technical Report specifies an electrothermal atomic absorption spectrometric method for the determination of selenium in steels. The method is applicable to selenium contents between 0,000 4 % (m/m) and 0,02 % (m/m).

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PDF Pages PDF Title
4 Contents Page
5 Foreword
6 1 Scope
2 Normative references
3 Principle
4 Reagents
4.1 Nitric acid, HNO3 (ρ20 = 1,40 g/ml)
4.2 Hydrochloric acid, HCl (ρ20 = 1,19 g/ml)
4.3 Matrix modifiers
4.3.1 Palladium-nickel modifier
7 4.3.2 Palladium-magnesium modifier
4.4 Selenium standard solution, 1 g/l
4.5 Selenium standard solution, 0,01 g/l
4.6 Pure iron, containing less than 0,000 1 % (mass fraction) of selenium
5 Apparatus
5.1 Auto sampler equipped with micropipettes of capacity 10 μl to 50 μl
5.2 Atomic absorption spectrometer and electrothermal atomizer
6 Sampling
8 7 Procedure
7.1 Test portion
Table 1 — Mass of the test portion
7.2 Blank test
7.3 Preparation of the test solution
7.4 Preparation of the standard addition solutions for the test solution
Table 2 — Standard addition solutions for the test solution
9 7.5 Preparation of the standard addition solutions for the blank test
Table 3 — Standard addition solutions for the blank test
8 Measurements
9 Expression of results
9.1 Plotting of the standard addition graphs
10 9.2 Method of calculation
10 Precision
11 Test report
11 Annex A (informative) Typical operating parameters
A.1 Typical conditions for the determination of selenium by electrothermal atomic absorption spectrometry
Table A.1 — Instrumental settings
Table A.2 — Typical temperature profile
A.2 Performance criteria
A.3 Criterion for graph linearity
A.3.1 General
12 A.3.2 Linearity of the blank standard addition graph
A.3.3 Linearity of the test standard addition graph
13 Annex B (informative) Instruments and the instrumental conditions used by the participants to the precision test
Table B.1 — Instruments and the instrumental conditions used by the participants to the precision test
14 Annex C (informative) Composition of the samples used for the precision test
Table C.1 — Composition of the samples used for the precision test
15 Table C.1 (cont.)
16 Annex D (informative) Detailed results obtained from the precision test
D.1 Results
Table D.1 — Results obtained from the precision test (µg/g)
17 Table D.1 (cont.)
18 Table D.1 (cont.)
19 Figure D.1 — Selenium — Mandel’s k test for intra laboratory consistency (99 % confidence level)
Figure D.2 — Selenium — Mandel’s h test for between laboratory consistency (99 % confidence level)
D.2 Comments on the suitability of the data
21 Bibliography

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BSI PD CEN/TR 10362:2014
$142.49