Overview
EN 13999-4:2007+A1:2009 is a European Standard developed by CEN that defines a short-term method for measuring the emission properties of low-solvent or solvent-free adhesives after application, focusing specifically on the determination of volatile diisocyanates. The standard is essential for testing emissions in the exhaust air of an emission test chamber and is relevant for adhesives containing isocyanate monomers such as toluene diisocyanate (TDI) and methylene bis(4-phenyl isocyanate) (MDI).
The method relies on chemosorption using 1-(2-methoxyphenyl) piperazine (1-2MP) impregnated filters, followed by desorption and analysis via high-performance liquid chromatography (HPLC). It offers a reliable way to measure volatile organic compounds containing isocyanate functional groups (NCO), ensuring accurate monitoring of adhesive emissions for occupational safety, indoor air quality, and regulatory compliance.
Key Topics
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Volatile Isocyanates Detection
EN 13999-4 enables the detection and quantification of volatile diisocyanates such as TDI, MDI, isophorone diisocyanate (IPDI), and 1,6-hexamethylene diisocyanate (HDI).
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Test Chamber Sampling Procedure
The standard specifies sampling in emission test chambers using glass fibre filters impregnated with 1-2MP to capture isocyanates from the air stream. Sampling involves controlled airflow and proper sealing to avoid contamination.
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Analytical Method: Chemosorption and HPLC
Captured isocyanates react with 1-2MP to form non-volatile urea derivatives, which are desorbed using acetic anhydride and analyzed by liquid chromatography using ultraviolet (UV) or diode array detection (DAD).
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Calibration and Quantification
Preparation of calibration standards includes synthetic isocyanate urea derivatives for generating calibration curves, allowing precise quantification of isocyanate concentrations in sampled air.
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Safety and Quality Control
The standard mandates laboratory safety practices and the use of blanks and quality controls to ensure analysis accuracy and reproducibility.
Applications
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Adhesives Industry Compliance
Manufacturers of low-solvent or solvent-free adhesives can use EN 13999-4 to identify volatile diisocyanate emissions during product development and production, ensuring compliance with environmental and health regulations.
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Indoor Air Quality Assessment
Building materials and furnishings utilizing adhesive applications benefit from this standard when assessing potential air contamination from adhesive off-gassing.
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Workplace Exposure Monitoring
Occupational health professionals can monitor air quality in workplaces to assess employee exposure to hazardous diisocyanates, facilitating risk management and compliance with exposure limits.
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Product Certification and Research
Enables laboratories and research institutions to perform standardized analysis for comparative studies or certification purposes related to volatile organic compound emissions from adhesives.
Related Standards
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EN 13999-1 – General procedure for measuring emissions of low-solvent or solvent-free adhesives, providing the foundational test chamber methodology utilized in Part 4.
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ISO 16702 – Specifies the determination of total organic isocyanate groups in air using 1-(2-methoxyphenyl)piperazine and liquid chromatography, offering complementary analytical approaches for isocyanate measurement.
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EN ISO 16000-9 – Defines the emission test chamber method for measuring volatile organic compounds from building products and furnishings, which supports the sampling framework for adhesives emissions.
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EN 1232 – Details requirements and test methods for personal sampling pumps used in workplace atmosphere monitoring, ensuring accurate and reliable air collection.
Conclusion
EN 13999-4:2007+A1:2009 provides a crucial standardized method for determining volatile diisocyanate emissions from low-solvent or solvent-free adhesives. Through its detailed procedures for sample collection, preparation, and chromatographic analysis, this standard supports the adhesive industry and environmental health professionals in monitoring, controlling, and reducing potentially harmful diisocyanate emissions. Adoption of this standard contributes to safer workplaces, improved indoor air quality, and regulatory compliance across Europe and beyond.
