ISO 22863-12:2022

Overview

ISO 22863-12:2022 specifies a validated test method for the determination of picrates and picric acid in fireworks and pyrotechnic compositions using high performance liquid chromatography (HPLC). The standard describes sample preparation, extraction, chromatographic conditions, qualitative identification by retention time, and quantitative determination with an external standard calibration curve. It is part of the ISO 22863 series developed by ISO/TC 264 (Fireworks).

Key topics and requirements

• Scope: Determination of picric acid and picrates in firework compositions by HPLC.
• Principle: Hot-water extraction of picrate anions followed by HPLC under acidic conditions; detection by UV (350 nm) and comparison to external picric acid standards.
• Sample preparation:
  • Sample mass: 0.5 g
  • Extraction: 5 ml hot deionized water, ultrasonic mixing 40 min, centrifuge 2 min at 3 000 r/min; repeat three times and combine to 25 ml.
  • Filtration through 0.45 µm organic Millipore device.
• HPLC settings (specified):
  • Column: C18 (4.6 × 250 mm, 5 µm) or equivalent
  • Mobile phase: Methanol : 0.1% glacial acetic acid = 55:45 (v/v)
  • Flow rate: 0.8 ml/min, injection volume 10 µl
  • Detection wavelength: 350 nm
• Calibration and quantification:
  • External standard (picric acid, ≥99% purity) reserve solution (100 µg/ml), prepare diluted standards to build a linear response curve.
  • Calculate sample concentration from peak area and standard curve; blank and parallel tests required.
• Performance:
  • Reported recovery: ~89.4%–96.4% in the 0.5–20 mg/kg range
  • Relative standard deviation (RSD) < 10%
• Reporting: Test report must include laboratory ID, reference to ISO 22863-12, sample description per ISO 22863-1, qualitative/quantitative results, and anomalies.

Applications and users

ISO 22863-12 is relevant for:

• Fireworks and pyrotechnic manufacturers performing quality control and formulation safety checks.
• Accredited testing laboratories and forensic labs analyzing seized fireworks for hazardous picrates/picric acid.
• Regulatory and customs authorities enforcing explosives and consumer safety regulations.
• Research groups studying pyrotechnic chemistry and decomposition products.

Keywords: ISO 22863-12:2022, picrates, picric acid, HPLC, fireworks testing, pyrotechnic compositions, high performance liquid chromatography, analytical method.

Related standards

• ISO 22863-1:2020 - Fireworks - Test methods for determination of specific chemical substances - Part 1: General (referenced for sample preparation and general requirements).
• Series: Other parts of ISO 22863 cover additional target substances and test procedures for fireworks.