Overview
EN ISO 23649:2025 - Chemicals for the leather tanning industry: Determination of cyclosiloxanes (ISO 23649:2025) specifies a standardized analytical method for measuring the total content of three cyclosiloxanes - octamethylcyclotetrasiloxane (D4), decamethylcyclopentasiloxane (D5) and dodecamethylcyclohexasiloxane (D6) - in chemicals used in leather tanning (for example, silicone-based waterproofing fatliquors and finishing agents). The method uses gas chromatography with a single quadrupole mass spectrometer (GC‑MS) following sample solubilisation and liquid–liquid extraction.
Key topics and requirements
- Analytes: D4, D5, D6 (cyclosiloxanes) - all noted in the document as classified in the EU as persistent, bioaccumulative and toxic (PBT).
- Analytical technique: Gas chromatography (GC) coupled with a single quadrupole mass spectrometer (MS) for identification and quantification.
- Sample preparation:
- Solubilise the chemical specimen in water (water grade 1, ISO 3696).
- Perform liquid–liquid extraction using an n‑hexane : ethyl acetate (50:50 v/v) mixture.
- Use internal standardisation to compensate for matrix effects and recovery.
- Annex C covers sample preparation for non‑water‑soluble chemicals.
- Calibration and quantification:
- External calibration with correction for the internal standard recovery.
- Stock solutions and internal standards (examples: Naphthalene‑D8 or Tetrakis(trimethylsilyloxy)silane) are specified.
- Apparatus and reagents: Ultrasonic bath, shaker, centrifuge, syringe membrane filters (e.g., 0.2 µm), GC vials, analytical balance, n‑hexane, ethyl acetate, sodium chloride, anhydrous MgSO4, and certified reference cyclosiloxanes.
- Supporting information:
- Annex A: recommended chromatographic operating parameters for GC‑MS.
- Annex B: method precision / reliability data.
- Annex C: normative sample prep for non‑water‑soluble matrices.
Applications and users