ISO 17734-1:2013
Determination of organonitrogen compounds in air using liquid chromatography and mass spectrometry — Part 1: Isocyanates using dibutylamine derivatives
Determination of organonitrogen compounds in air using liquid chromatography and mass spectrometry — Part 1: Isocyanates using dibutylamine derivatives
- Статус документа:
- Отменён
- Формат:
- Электронный (PDF)
- Количество страниц:
- 38
- Дата публикации:
- 27 ноября 2013 г.
- Издание:
- ISO IS 17734 edition 2 version 1
- ICS:
- 13.040.30
ISO 17734-1:2013 gives general guidance for the sampling and analysis of airborne isocyanates in workplace air. When amines and aminoisocyanates are suspected to be emitted (e.g. from thermal degradation of PUR), it is recommended that, in addition to isocyanates, the amines and aminoisocyanates in the air are determined, using DBA and ethyl chloroformate as reagents (see ISO 17734-2). The method is suitable for the determination of a wide range of different isocyanates in both the gas and particle phases. Typical monofunctional isocyanates that can be determined are isocyanic acid (ICA), methyl isocyanate (MIC), ethyl isocyanate (EIC), propyl isocyanate (PIC), butyl isocyanate (BIC), and phenyl isocyanate (PhI). Typical monomeric diisocyanates include 1,6-hexamethylene diisocyanate (HDI), 2,4- and 2,6-toluene diisocyanate (TDI), 4,4'-methylenediphenyl diisocyanate (MDI), 1,5-naphthyl diisocyanate (NDI), isophorone diisocyanate (IPDI), and 4,4'-dicyclohexylmethane diisocyanate (HMDI). Multifunctional isocyanates that can be determined are typically oligomers in polymeric MDI, biuret-, isocyanurate-, and allophanate-adducts, and prepolymeric forms of isocyanates. The instrumental detection limit for aliphatic isocyanates is about 5 nmol/sample and for aromatic isocyanates, it is about 0,2 nmol/sample. For a 15 l air sample, this corresponds to 0,6 ng∙m?3 for HDI and 0,02 ng∙m?3 for TDI. The useful range, for a 5 l air sample, of the method is approximately 0,001 µg∙m?3 to 200 mg∙m?3 for TDI.
Abstract
ISO 17734-1:2013 - Overview
ISO 17734-1:2013 specifies a validated analytical approach for the sampling and analysis of airborne isocyanates in workplace air using derivatization with di-n‑butylamine (DBA) and detection by liquid chromatography–mass spectrometry (LC‑MS). The standard covers both gas‑phase and particle‑bound isocyanates, including monofunctional isocyanates (ICA, MIC, EIC, PIC, BIC, PhI), common diisocyanates (HDI, TDI, MDI, NDI, IPDI, HMDI) and multifunctional/oligomeric forms (polymeric MDI adducts, biuret, isocyanurate, allophanate, prepolymers).
Key technical topics and requirements
- Sampling principle: Air is drawn through a midget impinger containing DBA in toluene followed by a glass-fibre filter; solvent‑free sampling using DBA‑impregnated filters is an alternative for long sampling times.
- Derivatization: Isocyanates are converted to stable DBA derivatives during sampling to prevent secondary reactions and losses.
- Instrumentation: Analysis is performed by LC‑MS / LC‑MS/MS for selective identification and quantification. A nitrogen‑sensitive detector (LC‑CLND) is referenced for preparing reference solutions.
- Standards and reagents: Use of deuterium‑labelled isocyanate‑DBA internal standards is recommended for accurate quantification and to control recovery.
- Performance characteristics: Instrumental detection limits ≈ 5 nmol/sample for aliphatic isocyanates and 0.2 nmol/sample for aromatic isocyanates. For a 15 L air sample this equals about 0.6 ng·m‑3 (HDI) and 0.02 ng·m‑3 (TDI). Useful range for TDI (5 L sample) is about 0.001 µg·m‑3 to 200 mg·m‑3.
- Data handling: Guidance on identification, calibration curves, quantification, interferences and uncertainty assessment is included.
Practical applications and who uses this standard
ISO 17734-1 is intended for:
- Industrial hygienists and occupational health laboratories monitoring worker exposure to isocyanates.
- Environmental and analytical laboratories performing air monitoring in manufacturing, spray‑coating, foam production and polyurethane (PUR) processing.
- Regulatory bodies and consultants assessing compliance with occupational exposure limits (OELs) and investigating incidents (e.g., thermal degradation of PUR).
- Manufacturers concerned with emissions profiling and process control.
The method is especially valuable where very low detection levels, speciation of multiple isocyanates, or identification of degradation products are required.
Related standards
- ISO 17734-2: Complementary method for amines and aminoisocyanates (DBA + ethyl chloroformate).
- ISO 5725-2: Accuracy (trueness and precision) of measurement methods.
- ISO 16200-1: Sampling and analysis of volatile organic compounds (pumped sampling).
Keywords: ISO 17734-1:2013, isocyanates, dibutylamine (DBA), LC‑MS, workplace air monitoring, sampling and analysis, TDI, HDI, polyurethane.
Технические детали
- Технический комитет
- ISO/TC 146/SC 2 - Workplace atmospheres
- SKU
- ISO 17734-1:2013
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