CR 10322:2003

Overview

CR 10322:2003 - Chemical analysis of ferrous materials - Operational guidelines for the application of flame atomic absorption spectrometry (FAAS) in standard methods for the chemical analysis of iron and steel (CEN report). This document provides practical, instrument-level guidance to ensure reliable, comparable results when FAAS is used for analysing iron, steel and cast irons. It focuses on operational parameters, verification procedures, and common error sources to optimize sensitivity, detection limits and precision. The report is confined to the flame technique (not flameless AA) and is intended as a working reference for laboratories and method developers.

Key topics and technical requirements

• Instrument components and optimisation
  • Radiation source: use of hollow cathode lamps (single- or multi-element); lamp current adjustment affects sensitivity, linearity and lamp life; recommended performance check - signal deviation ≤ 0.5% over 15 minutes.
  • Monochromator: set slit width first, then wavelength; choose largest slit compatible with spectral interferences; re-check wavelength before measurements.
  • Detector & signal processing: implications of scale expansion, concentration read-out, curvature correction, damping and integration times (integration < ~30 s to avoid drift).
• Atomization and sample introduction
  • Nebulization: aspiration rate and nebulizer efficiency affect fraction of sample reaching flame; match physical properties (density, viscosity, temperature) of calibration and sample solutions.
  • Flame atomization: fuel/oxidant ratio (air–acetylene or nitrous oxide–acetylene) and measuring height influence atomic population and matrix effects. Nitrous oxide/acetylene flames require special burners (slot ≈ 5 cm) or higher gas flow; air/acetylene commonly uses a 10 cm burner.
• Gases & safety
  • Acetylene purity and pressure (avoid < 600 kPa) to prevent contamination; compressed clean air recommended; nitrous oxide regulators must be protected against freezing.
  • Annex C provides safety directions (flammable gases, flashback risk, salt deposits).
• Errors, verification and reporting
  • Discussion of systematic vs random errors, performance checks, calibration practice (curved calibration graphs), and reporting measurement results (Annex B).
• Informative annexes
  • Annex A: instrumental settings and optimisation
  • Annex B: reporting format
  • Annex C: safety
  • Annex D: instrument parameter determination

Applications and users

• Analytical laboratories performing routine or standards-based chemical analysis of iron, steel and cast iron
• Quality control and metallurgical labs requiring trace and major element determinations by FAAS
• Standards writers and method developers drafting or validating standard methods that incorporate FAAS
• Instrument technicians responsible for optimisation, verification and troubleshooting

Related standards

• CR 10321 (related recommendations for drafting FAAS standard methods)
• ISO 6955:1982 and ISO/DIS 6956:1981 (general AA references cited in the report)

Keywords: CR 10322:2003, flame atomic absorption spectrometry, FAAS, chemical analysis of ferrous materials, iron and steel analysis, CEN, instrument optimisation, calibration, analytical quality.