ISO 13110:2012 PDF

Overview - ISO 13110:2012 (menthol determination in cigarette smoke condensates)

ISO 13110:2012 specifies a gas‑chromatographic (GC) method to determine menthol in the total particulate matter (TPM) of mainstream cigarette smoke condensates. Smoking and collection of mainstream smoke are carried out in accordance with ISO 4387 with specific exceptions (Annex A). The standard covers sample preparation, choice of reagents and internal standard, GC operating conditions, calibration, result expression and reporting. It also highlights limitations (e.g., machine smoking is not a measure of human exposure) and special handling considerations for encapsulated menthol.

Key topics and technical requirements

• Scope: quantitative determination of menthol in TPM from mentholated cigarettes using GC.
• Sampling and smoking: follow ISO 4387 and ISO 8243 sampling with Annex A exceptions for menthol loss and conditioning.
• Reagents and internal standard:
  • Extraction solvents: propan‑2‑ol, ethanol or methanol are acceptable after validation.
  • Internal standard typically n‑heptadecane (≥99 %); alternatives allowed after assessment.
  • Reference substance: menthol (>99 % purity) with recommended cool, dark storage.
• Test portion and extraction:
  • TPM dissolved in extraction solvent (20 ml for 44 mm filter pads, 50 ml for 92 mm pads), shaken ≥20 min.
• Gas chromatography:
  • Column example: DB‑WAX, 0.53 mm ID, 1 µm film, ~30 m (or equivalent).
  • Detector: flame ionization detector (FID); carrier gases include helium, nitrogen or hydrogen.
  • Example operating conditions provided (e.g., injector ~200 °C, 1 µl injection, split ≈10:1; oven program 100→150→200 °C; detector ~250 °C).
• Calibration and QC:
  • At least four calibration standards (typical range 0.02–1.0 mg/ml).
  • Full calibration daily; inject intermediate standard every ~20 samples - if >3 % deviation, recalibrate.
• Results:
  • Report menthol yield in mg per cigarette to 0.01 mg.
• Performance:
  • Repeatability and reproducibility estimates based on a 17‑lab study are provided in the standard.

Applications and practical use

• Quality control and production testing in tobacco R&D laboratories.
• Regulatory and compliance testing for menthol yields in cigarette products.
• Contract analytical laboratories performing routine menthol analysis.
• Product characterization, formulation development and comparative emissions studies. Note: Users should be aware machine measurements characterize emissions for design/regulatory purposes but are not direct measures of human exposure.

Related standards

• ISO 4387 - determination of TPM using a routine analytical smoking machine (primary smoking regimen reference).
• ISO 8243 - cigarettes sampling.
• ISO 3308, ISO 3402 - referenced in related bibliographic material for smoking machine and conditioning atmospheres.

Keywords: ISO 13110:2012, menthol determination, gas‑chromatographic method, cigarettes, smoke condensates, total particulate matter, GC‑FID, n‑heptadecane, ISO 4387.