BS ISO 16000-39:2019 pdf download – Indoor air Part 39: Determination of amines — Analysis of amines by (ultra-) high-performance liquid chromatography coupled to high resolution or tandem mass spectrometry
This document, along with ISO 16000‑38, specifies the measurement method for determining the mass concentration of primary, secondary and tertiary aliphatic and aromatic amines in indoor air using accumulated sampling and high-performance liquid chromatography (HPLC) coupled with tandem mass spectrometry (MS-MS) or high-resolution mass spectrometry (HRMS). The analytical procedure is covered by this document. The sampling procedure and the manufacturing of the samplers are covered by ISO 16000-38.
This document describes specifications for the chromatography and the mass spectroscopy for the amines. Measurement results are expressed in µg/m 3 . Although primarily intended for the measurement of amines listed in Tables A.1 and A.2, it can also be used for the measurement of other amines in indoor air. This document gives instructions and describes procedures for the inclusion of other amines.
The range of application of this document concerning the concentrations of amines in indoor air depends on the linear range of the calibration line and hence on the gas sample volume (here: from 5 l up to 100 l), the eluate volume (from 1 ml up to 5 ml), the injection volume (from 1 µl up to 10 µl) and the sensitivity of the analytical equipment (e.g. linear range from 2 pg up to 2 ng amine). The range of application can be expected to be from approximately 0,002 µg/m 3 (100 l sample) up to 2 000 µg/m 3 (5 l sample) for a common analytical equipment (e.g. Waters „TQD“) for the majority of the amines listed in Tables A.1 and A.2.
The analysis of derivatives of ethanolamine is usually about 10 times more sensitive and the analysis of short-chained aliphatic amines is usually about 10 times less sensitive than the analysis of an average amine. The performance data of the analytical method is given in Annex B, particularly in Tables B.1 and B.2. This document can be used also for the determination of amines in water if the detection limit is sufficient. This document does not cover the determination of isocyanates in indoor air (nor in water samples) as corresponding amines (covered by ISO 17734-1 and ISO 17734-2).
2 Normative references The following documents are referred to in the text in such a way that some or all of their content constitutes requirements of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.
ISO 16000-38, Indoor air — Part 38: Determination of amines in indoor and test chamber air — Active sampling on samplers containing phosphoric acid impregnated filters
— column temperature: 40 °C;
— injection volume: 1 µl to 10 μl;
— mobile phase: acetonitrile and water with each 0,02 % formic acid (500 µl formic acid in 2,5 l
acetonitrile or 2,5 l water, respectively);
— mobile phase composition: 28 % acetonitrile/72 % water, isocratic.
5.3 Tandem mass spectrometry
— ionisation: electrospray ionisation, positive mode (ESI + );
— source temperature: 120 °C;
— desolvation gas: nitrogen, 900 l/h;
— desolvation temperature: 420 °C;
— cone gas: nitrogen, 50 l/h;
— precursor ion: M+1;
— collision gas: argon;
— calibration: external and additionally with Pyridine-d5 as internal standard.
5.4 High resolution mass spectrometry
— ionisation: electrospray ionisation, positive mode (ESI + ).
5.5 Sample sequence and external calibration
— external calibration: run calibration standards at least at the beginning and at the end of a sample sequence;
— every 25 samples or less and at the beginning and end, run a calibration blank and a calibration check solution of an independent source;
— every 50 samples (for example) and at the end of a run, analyse an interference check solution (ICS).
6 Testing of the suitability of the equipment and the instrumental analysis
6.1 General
In Table A.3, several amines are listed which can interfere with another amine in the instrumental analysis. In order to check and confirm the suitability of the selected system and procedure following issues have to be tested.
6.2 High-performance or ultra-performance liquid chromatography (HPLC or UHPLC)
The chromatographic separation of following compounds has to be tested and confirmed:
a) Diethylamine (11) and N,N‑Dimethylethylamine (24);
b) Isobutylamine (2) and n‑Butylamine (10);
c) 2‑(Dimethylamino)ethanol (8) and 2‑(Ethylamino)ethanol (25);
d) Diisobutylamine (14) and Di-n-butylamin (16).BS ISO 16000-39 pdf download.