BS ISO 17858:2007

Foreword
Introduction
1 Scope
2 Normative references
3 Terms, definitions and abbreviated terms
   3.1 Terms and definitions
   3.2 Abbreviated terms
4 Principle
   4.1 Spiking and extraction
   4.2 Clean-up
   4.3 Concentration
   4.4 Identification
   4.5 Quantification
   4.6 Analytical quality
5 Contamination and interferences
6 Reagents and standards
7 Apparatus and materials
   7.1 Sampling equipment for discrete sampling
   7.2 Equipment for sample preparation
   7.3 Extraction apparatus
   7.4 Filtration apparatus
   7.5 Clean-up apparatus
   7.6 Concentration apparatus
   7.7 Other equipment
8 Sample collection, preservation, storage and holding
   times
9 Quality assurance (QA)/quality control (QC)
   9.1 General
   9.2 Initial precision and recovery (IPR)
   9.3 Spiking
   9.4 Recovery of labelled compounds assessment
   9.5 Method blanks
   9.6 QC check sample
   9.7 Method precision
10 Calibration
   10.1 Operating conditions
   10.2 Mass spectrometer (MS) resolution
   10.3 Ion abundance ratios, minimum levels, signal-to-noise
        ratios, and absolute retention times
   10.4 Retention time
   10.5 Isomer specificity
   10.6 Calibration by isotope dilution
   10.7 Calibration by internal standard
   10.8 Combined calibration
11 Sample preparation
   11.1 General
   11.2 Determination of percent suspended solids
   11.3 Preparation of aqueous samples containing 1%
        of suspended solids or less
12 Extraction and concentration
   12.1 Separatory funnel extraction of filtrates and of
        aqueous samples that are visibly absent of particles
   12.2 Solid-phase extraction (SPE) of samples containing
        less than 1% suspended solids
   12.3 Soxhlet extraction of filters and/or disks
   12.4 Back-extraction with acid and base
   12.5 Macro-concentration
   12.6 Micro-concentration and solvent exchange
13 Extract clean-up
   13.1 General
   13.2 Gel permeation chromatography (GPC)
   13.3 Silica clean-up
   13.4 Alumina clean-up
   13.5 Carbon column
   13.6 High performance liquid chromatography (HPLC)
   13.7 Florisil clean-up
   13.8 Silver nitrate/silica column
14 HRGC/HRMS analysis
15 System and laboratory performance
   15.1 General
   15.2 MS resolution
   15.3 Calibration verification
   15.4 GC resolution
   15.5 Blank
16 Qualitative determination
17 Quantitative determination
   17.1 Isotope dilution quantification
   17.2 Internal standard quantification and labelled-
        compound recovery
   17.3 Concentration in sample
   17.4 Results and reporting
   17.5 Toxic equivalents (TEQ)
18 Analysis of complex samples
   18.1 General
   18.2 Recovery of labelled compounds
19 Pollution prevention
20 Waste management
21 Precision
Annex A (informative) Example chromatograms
Annex B (informative) Use of HRGC/LRMS
Annex C (informative) Precision data
Bibliography

Describes a method for the determination of dioxin-like tetra- to hepta-chlorinated biphenyls (PCBs) in waters and wastewaters (containing less than 1% suspended solids) using high-resolution gas chromatography/high-resolution mass spectrometry (HRGC/HRMS).

This International Standard specifies a method for the determination of dioxin-like tetra- to hepta-chlorinated biphenyls (PCBs) in waters and wastewaters (containing less than 1%suspended solids) using high-resolution gas chromatography/high-resolution mass spectrometry (HRGC/HRMS). The method is optimized for dioxin-like PCBs, but can include other co-planar compounds such as polychlorinated dioxins and furans (PCDDs/PCDFs) and polychlorinated naphthalenes (PCNs). This method can be used to determine dioxin-like PCBs in other matrices (e.g. biota, sediments, air); however, additional clean-up steps and techniques can be required for samples with high organic loadings.

This method is applicable to the twelve non- and mono-ortho PCBs designated by the World Health Organization, as well as to other PCBs and co-planar compounds.

The detection limits and quantification levels in this method are dependent on the level of interferences as well as instrumental limitations. The minimum levels (ML) in Table2 are the levels at which the dioxin-like PCBs can typically be determined with no interferences present.

This method is “performance based”. The analyst is permitted to modify the method to overcome interferences or lower the cost of measurements, provided that all performance criteria in this method are met. The requirements for establishing method equivalency are given in 9.2.