ISO 21863:2020
Water quality — Determination of alkylmercury compounds in water — Method using gas chromatography-mass spectrometry (GC-MS) after phenylation and solvent extraction
This document specifies a method for the determination of alkylmercury compounds in filtered water samples by gas chromatography-mass spectrometry after phenylation and solvent extraction.
This method is applicable to determination of individual methylmercury (MeHg) and ethylmercury (EtHg) compounds in surface water and waste water.
The method can be applied to samples containing 0,2 μg/l to 10 μg/l of each compound as mercury mass. Depending on the matrix, the method may also be applicable to higher concentrations after suitable dilution of the sample or reduction in sample size.
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Foreword
Introduction
1 Scope
2 Normative references
3 Terms and definitions
4 Principle
5 Interferences
5.1 Interferences with sampling, sample storage and sample preparation
5.2 Interferences with GC-MS
6 Reagents and standards
7 Apparatus and materials
8 Sample collection, preservation and storage
9 Procedure
9.1 Sample preparation
9.1.1 pH-adjustment of water sample
9.1.2 Phenylation and solvent extraction
9.1.3 Dehydration of toluene extract
9.2 Preparation of samples for GC‑MS
9.3 Optimization of operating condition for GC‑MS
9.4 Identification of individual substances with GC‑MS
9.5 Blank tests
10 Calibration
10.1 General requirements
10.2 Performance test of GC‑MS
10.3 Calibration with internal standard
10.3.1 General requirement
10.3.2 Procedure of calibration
10.4 Spike recovery test of target substances
11 Calculation
11.1 Calculation of results after calibration with internal standards
11.2 Treatment of results lying outside the calibration range
11.3 Quality checks for internal standardization
12 Expression of results
13 Test report
Annex A (informative) Example of operating condition of GC-MS
Annex B (informative) Examples of mass chromatograms and mass spectra of phenylated alkylmercury by GC-MS
Annex C (informative) The use of sodium tetrapropylborate as an alternative derivatizing agent[4]
Annex D (informative) The use of GC-AFS as an alternative detector
Annex E (informative) Performance data
Bibliography
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Foreword
Introduction
1 Scope
2 Normative references
3 Terms and definitions
4 Principle
5 Interferences
5.1 Interferences with sampling, sample storage and sample preparation
5.2 Interferences with GC-MS
6 Reagents and standards
7 Apparatus and materials
8 Sample collection, preservation and storage
9 Procedure
9.1 Sample preparation
9.1.1 pH-adjustment of water sample
9.1.2 Phenylation and solvent extraction
9.1.3 Dehydration of toluene extract
9.2 Preparation of samples for GC‑MS
9.3 Optimization of operating condition for GC‑MS
9.4 Identification of individual substances with GC‑MS
9.5 Blank tests
10 Calibration
10.1 General requirements
10.2 Performance test of GC‑MS
10.3 Calibration with internal standard
10.3.1 General requirement
10.3.2 Procedure of calibration
10.4 Spike recovery test of target substances
11 Calculation
11.1 Calculation of results after calibration with internal standards
11.2 Treatment of results lying outside the calibration range
11.3 Quality checks for internal standardization
12 Expression of results
13 Test report
Annex A (informative) Example of operating condition of GC-MS
Annex B (informative) Examples of mass chromatograms and mass spectra of phenylated alkylmercury by GC-MS
Annex C (informative) The use of sodium tetrapropylborate as an alternative derivatizing agent[4]
Annex D (informative) The use of GC-AFS as an alternative detector
Annex E (informative) Performance data
Bibliography