ISO 22863-5:2021

Overview

ISO 22863-5:2021 - Fireworks - Test methods for determination of specific chemical substances - Part 5: Analysis of lead and lead compounds by inductively coupled plasma spectrometry (ICP) - specifies a validated laboratory method to determine lead (Pb) content in pyrotechnic compositions. The standard defines sample preparation (acid digestion), instrumental analysis by ICP-OES, calibration, quality controls and reporting requirements to produce reproducible results expressed in mg/kg.

Key topics and technical requirements

• Scope: Determination of lead and lead compounds in fireworks and pyrotechnic compositions using ICP spectrometry after acid digestion.
• Sample prep:
  • Dry sample at (105 ± 5) °C to constant mass.
  • Digest representative aliquots with nitric acid (HNO3) (three separate digestions; microwave digestion is optional following manufacturer guidance).
  • Filter, combine aliquots and make up to volume (typically 100.0 ml).
• Instrumentation and consumables:
  • ICP-OES (argon plasma) with manufacturer-recommended accessories.
  • Analytical balance (±0.1 mg), oven, crucible (25 ml), volumetric flasks.
• Calibration:
  • External calibration series recommended: 0.00, 0.25, 0.50, 1.00, 5.00 and 10.0 μg/ml Pb (prepared from a 1 000 μg/ml stock).
  • Optional internal standard: yttrium (Y) at 2 μg/ml (Y line cited at 324.228 nm).
  • Typical instrument settings are specified (e.g., plasma flow 15.0 L/min, nebulizer 0.75 L/min, power ~1.30 kW).
  • Primary analytical line recommended for Pb (220.353 nm); an alternate line is suggested to check spectral interferences.
• Quality control:
  • Analyze at least one certified reference material (CRM) per batch; recovery expected within ±15%.
  • Instrument calibration check tolerances: calibration points within ±5%; sample concentrations within ±10% of true value or require re-calibration.
  • Typical method precision targets indicated (relative standard deviation ~10%, recovery ~90%) and note potential spectral bias from aluminum levels >1% w/w.
• Reporting:
  • Results reported in mg/kg with method reference ISO 22863-5:2021 and full sample description per ISO 22863-1.

Applications and users

This standard is intended for:

• Test laboratories analyzing fireworks, pyrotechnic formulations, regulatory compliance testing and safety assessment.
• Manufacturers performing incoming quality control and formulation verification to limit Pb content.
• Regulators and certification bodies enforcing limits on toxic metals in consumer pyrotechnics. Practical uses include contamination assessment, pre-market testing, batch release testing and inter-laboratory method harmonization.

Related standards

• ISO 22863-1 - Artifices de divertissement - Test methods for determination of specific chemical substances - Part 1: Generalities (terminology, sampling and general requirements).
• Other parts of the ISO 22863 series covering analyses of different substances in fireworks.

Keywords: ISO 22863-5:2021, fireworks testing, lead analysis, ICP-OES, pyrotechnic compositions, nitric acid digestion, certified reference material, calibration, laboratory method.