ISO 22863-2:2020

Overview

ISO 22863-2:2020 defines a laboratory test method for the determination of hexachlorobenzene (HCB) in pyrotechnic compositions using gas chromatography. The procedure covers sample preparation, extraction, purification and GC analysis with a flame ionization detector (FID). Under the specified conditions a limit of detection (LOD) of 1 mg/kg (dry matter) can be achieved.

This part references ISO 22863-1:2020 for general sample preparation requirements and complements it with HCB‑specific procedures and acceptance criteria.

Key Topics

• Analyte: Hexachlorobenzene (HCB), CAS 118-74-1 (purity 99.5% when used as standard).
• Sample size and prep: Typical sample mass is 1 g; extraction is a solid–liquid procedure using chromatographic-grade solvents (n-hexane or preferably ethanol or heptane).
• Extraction steps: Mix sample with solvent, vortex 2 min, centrifuge at 3 000 r/min, repeat extraction twice, combine extracts and evaporate to <1 ml, reconstitute to 1 ml.
• Purification: Treat extract with concentrated sulfuric acid to precipitate impurities, centrifuge and collect the upper solvent layer for GC analysis.
• Chromatography: GC with FID (hydrogen flame), splitless injection, 1 µl injection volume. A typical capillary column given is HP‑5 (30 m × 0.25 mm × 0.25 µm) with a temperature program (start 80 °C, ramp to 230 °C at 20 °C/min, hold 10 min). Reported reference retention time for HCB is approximately 8.2 min.
• Standards and calibration: Prepare primary standard (100 µg/ml), intermediate (10 µg/ml) and working standards (0.5, 1.0, 2.0 and 5.0 µg/ml) to build calibration and verify response.
• Quality control: Recovery check on the 5.0 µg/ml working standard must fall between 84.2 % and 101.6 %. If out of range, repeat the batch.

Applications

• Routine laboratory testing of fireworks and other pyrotechnic compositions for HCB content.
• Regulatory compliance and product safety verification where HCB limits must be monitored.
• Quality control during formulation and raw material inspection to reduce persistent organic pollutant risks.

Benefits include a standardized GC‑FID approach, defined sample handling and validation checks (LOD and recovery) to help laboratories produce reproducible, defensible results.

Related Standards

• ISO 22863-1:2020 - General requirements and sample preparation for test methods on specific chemical substances in fireworks.

Other related laboratory practices referenced in ISO 22863-2:2020 include analytical reagent quality, safe handling of flammable/explosive pyrotechnic samples and use of appropriate personal protective equipment. For reporting, follow the document's minimum data requirements: laboratory identification, sample description, method reference (ISO 22863-2) and results with noted anomalies.

Keywords: ISO 22863-2:2020, hexachlorobenzene, HCB, gas chromatography, GC‑FID, fireworks testing, pyrotechnic compositions, limit of detection, sample extraction, method validation.