Overview
EN ISO 15320:2011 (CEN adoption of ISO 15320:2011) defines a laboratory test method for the determination of pentachlorophenol (PCP) in an aqueous extract of pulp, paper and board. Originally developed for paper and board intended to contact foodstuffs, the method is applicable to all types of pulp, paper and board. The method uses water extraction (cold or hot), solid‑phase extraction (SPE), chemical derivatization (acetylation) and analysis by gas chromatography with either an electron‑capture detector (ECD) or mass spectrometer (MS). The specified working range for acetylation is 0.05 mg/kg to 0.5 mg/kg (upper limit may be raised if the extract is diluted).
Key Topics and Requirements
- Scope: Quantitative determination of PCP in aqueous extracts of pulp, paper and board, results expressed as mg/kg.
- Sampling: Representative sampling in accordance with relevant standards; minimum sample mass 10 g (oven‑dried).
- Extraction methods:
- Cold‑water extraction: 10 g sample + 200 ml water, stand 24 h at (23 ± 2) °C, occasional shaking.
- Hot‑water extraction: 10 g sample + 200 ml boiling water, stand 2 h in 80 ± 2 °C water bath, washings at 80 °C, cool to 23 ± 2 °C.
- Concentration: Solid‑phase extraction on phenyl silica (e.g., 500 mg/3 ml columns); elution with n‑hexane.
- Derivatization: Formation of an acetylated derivative using acetic anhydride prior to GC analysis.
- Instrumentation:
- Capillary GC column example: polydimethylsiloxane with 5% phenyl, 30 m × 0.32 mm, 0.25 µm film.
- Detectors: ECD or MS (MS example: EI 70 eV, SIM mode).
- Calibration and internal standards:
- ECD: 2,3,6‑trichlorophenol internal standard.
- MS: 13C‑labelled pentachlorophenol internal standard.
- Safety: Method involves hazardous reagents (PCP, methanol, acetic anhydride, acids); follow laboratory safety and environmental practices.
Applications and Users
- Food‑contact materials testing: Compliance testing for paper and board intended to contact food.
- Quality assurance / supplier control: Mill and converter QA labs verifying low PCP content in raw pulp or finished board.
- Regulatory and environmental labs: Monitoring and enforcement of chemical safety limits in paper products.
- R&D and forensic analysis: Method validation, comparative studies, and contaminant source tracking.
Keywords: EN ISO 15320:2011, pentachlorophenol, PCP, aqueous extract, pulp, paper, board, solid‑phase extraction, acetylation, gas chromatography, ECD, mass spectrometry.
Related Standards (normative references)
- ISO 186 - Sampling to determine average quality (paper and board)
- ISO 536 - Determination of grammage
- ISO 638 - Dry matter content (oven‑drying)
- ISO 7213 - Pulps - Sampling for testing
- ISO 3696 - Water for analytical laboratory use
This summary highlights the practical steps and technical elements of EN ISO 15320:2011 for laboratories performing PCP determination in paper and board.