ISO 15318:1999 PDF

Overview

ISO 15318:1999 specifies a laboratory test method for the determination of seven specified polychlorinated biphenyls (PCBs) in pulp, paper and board. The method targets congeners 18, 28, 52, 101, 138, 153 and 180, and describes sample preparation, extraction, cleanup, chromatographic analysis and result expression. Annexes provide a procedure to estimate total PCB from these congeners, a design for the extraction reservoir, and graphical interpretation guidance.

Key topics and requirements

• Analytes covered: Seven PCB congeners (18, 28, 52, 101, 138, 153, 180) used to identify PCB contamination patterns from sources such as historical carbonless copy paper.
• Sampling: Follow EN ISO 186 (paper and board sampling) or EN 27213 (pulp sampling). Samples should be protected (e.g., wrapped in aluminium foil) between acquisition and testing.
• Sample size and preparation: Typical test portions are ~2.00 g (paper/board) or 1.80 g (pulp, oven-dry basis), homogenised and cut to ~1 cm pieces.
• Extraction: Reflux with ethanolic (or methanolic) potassium hydroxide (2 % w/v) for 60 minutes; aliquot diluted with water prior to solid-phase cleanup.
• Clean-up: Liquid–solid partitioning using a disposable C18 solid-phase extraction cartridge (3.0 ml / 200 mg) conditioned with methanol/water; elution with n-hexane (or ISO-octane).
• Post‑treatment: Hexane extract washed with concentrated sulphuric acid to remove interfering colour and matrix components.
• Instrumental determination: Capillary gas chromatography with an electron capture detector (GC‑ECD) or mass selective detector (GC‑MS/MS or MSD). Recommended column: 5% phenylmethyl silicone, 50–60 m, 0.2–0.35 mm ID, 0.1–0.3 µm film. Example oven and detector temperature programs are provided.
• Standards and controls: Use individual and combined reference standard solutions, internal standards (PCB 30 or 2,4,6‑tribromobiphenyl), and technical mixture comparison samples (e.g., Chlophen/Arochlor) to verify congener pattern and allow estimation of total PCB.
• Quality elements: Method blank, sample blanks, calibration (spiked) samples, and triplicate analysis are specified. Annex A gives an approach to estimate total PCB from the seven congeners.

Applications and users

This standard is intended for:

• Environmental and analytical testing laboratories performing PCB residue analysis in paper products.
• Paper, board and pulp manufacturers and recyclers conducting quality control and contamination screening.
• Regulatory and compliance testing where identification of PCB contamination from recycled materials (e.g., carbonless copy paper) is required.
• Research labs studying PCB congener patterns and contamination pathways in paper recycling streams.

Related standards

• EN ISO 186 - Paper and board: sampling to determine average quality
• EN 27213 - Pulps: sampling for testing

Keywords: ISO 15318, polychlorinated biphenyls, PCB congeners, pulp paper board, GC‑ECD, solid‑phase extraction, paper recycling, analytical method, PCB determination.