ISO 17734-2:2013
Determination of organonitrogen compounds in air using liquid chromatography and mass spectrometry — Part 2: Amines and aminoisocyanates using dibutylamine and ethyl chloroformate derivatives
Determination of organonitrogen compounds in air using liquid chromatography and mass spectrometry — Part 2: Amines and aminoisocyanates using dibutylamine and ethyl chloroformate derivatives
- Статус документа:
- Действующий
- Формат:
- Электронный (PDF)
- Количество страниц:
- 33
- Дата публикации:
- 27 ноября 2013 г.
- Издание:
- ISO IS 17734 edition 2 version 1
- ICS:
- 13.040.30
ISO 17734-2:2013 gives general guidance for the sampling and analysis of airborne amines and aminoisocyanates in workplace air. It is strongly recommended that the determination of amines and aminoisocyanates is made together with the determination of isocyanates in air, using DBA as a reagent (see ISO 17734-1). The method can be used for simultaneous determinations of amines, such as 4,4'-methylenediphenyldiamine (4,4'-MDA), 2,4- and 2,6-toluenediamine (2,4- and 2,6-TDA), and 1,6-hexamethylenediamine (1,6-HDA), and compounds containing both isocyanate and amine groups, such as 4,4'-methylenediphenyl aminoisocyanate (4,4'-MAI), 2,4-, 4,2-, and 2,6-toluene aminoisocyanate (2,4-, 4,2-, and 2,6-TAI), and 1,6-hexamethylene aminoisocyanate (1,6-HAI). The method is suitable for collecting amines and aminoisocyanates in both the gas and particle phases. The instrumental detection limit for the amines is about 5 nmol/sample and for the aminoisocyanate, it is about 0,3 nmol/sample. For a 15 l air sample, this corresponds to 0,4 ng⋅m?3 for TDA and 0,03 ng⋅m?3 for TAI.
Abstract
Overview
ISO 17734-2:2013 specifies a validated laboratory and field procedure for the sampling and analysis of airborne amines and aminoisocyanates in workplace air. The method uses derivatization with dibutylamine (DBA) and ethyl chloroformate (ET) followed by separation with reversed‑phase liquid chromatography and detection primarily by LC-MS (electrospray, positive ions). It is designed to be used together with ISO 17734‑1 (isocyanates using DBA derivatives) to enable simultaneous determination of isocyanates, aminoisocyanates and amines from a single sampling protocol.
Key topics and technical requirements
- Scope: Collection and analysis of amines (e.g., 4,4'-MDA, 2,4- and 2,6-TDA, 1,6-HDA) and aminoisocyanates (e.g., 4,4'-MAI, TAI isomers, 1,6-HAI) in both gas and particle phases of workplace air.
- Sampling: Draw a known air volume through a midget impinger containing DBA in toluene followed by a glass-fiber filter (no binder). Method supports particles >1.5 µm in impinger and smaller particles on the filter.
- Derivatization & sample prep: Amines derivatized with ET; isocyanate groups reacted with DBA/ethanol to form mixed derivatives. Deuterium‑labelled derivatives are recommended as internal standards.
- Instrumentation & detection:
- Primary: LC-MS (selected ion monitoring of molecular ions) for sensitivity and identification.
- Alternatives: LC‑CLND for nitrogen-specific quantification, LC‑UV for higher concentrations, GC‑TSD for volatile components.
- Analytical performance:
- Instrumental detection limits ≈ 5 nmol/sample for amines and 0.3 nmol/sample for aminoisocyanates.
- Example: for a 15 L air sample, detection corresponds to ≈ 0.4 ng·m‑3 for TDA and 0.03 ng·m‑3 for TAI.
- Quality control: Use of internal standards, blanks, characterized reference solutions, and established calibration procedures.
Practical applications
- Monitoring occupational exposure to amines, aminoisocyanates and isocyanates in industries such as polyurethane manufacturing, thermal decomposition (firefighting/accident assessment), coatings, adhesives and composite production.
- Routine industrial hygiene surveys, incident investigations, regulatory compliance testing and exposure assessment studies.
- Laboratories requiring a sensitive, specific method to quantify low‑level organonitrogen compounds in workplace atmospheres.
Who should use this standard
- Industrial hygienists and occupational health professionals
- Environmental and analytical laboratories performing workplace air monitoring
- Manufacturers and quality/safety teams in industries using isocyanate-containing materials
- Regulators and researchers assessing exposure risks from polyurethane thermal decomposition
Related standards
- ISO 17734-1 - Isocyanates using dibutylamine derivatives (recommended to be used together)
- ISO 16200-1 - Sampling and analysis of volatile organic compounds by solvent desorption/GC (pumped sampling)
- ISO 5725-2 - Accuracy (trueness and precision) of measurement methods
Keywords: ISO 17734-2:2013, airborne amines, aminoisocyanates, dibutylamine DBA, ethyl chloroformate, LC‑MS, workplace air monitoring, isocyanates, occupational exposure.
Технические детали
- Технический комитет
- ISO/TC 146/SC 2 - Workplace atmospheres
- SKU
- ISO 17734-2:2013
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