BS ISO 18073:2004

Foreword
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 Water sample containers
   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/quality control
   9.1 General
   9.2 Initial precision and recovery (IPR)
   9.3 Spiking
   9.4 Method blanks
   9.5 Quality control check sample
   9.6 Method precision
10 Calibration
   10.1 Operating conditions
   10.2 Mass spectrometer (MS) resolution
   10.3 QC limits and theoretical ion abundance ratios for
        standards
   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 suspended solids
   11.3 Preparation of aqueous samples containing 1% or less
        by mass suspended solids
12 Extraction and concentration
   12.1 Extraction of samples with no visible particulates
   12.2 Soxhlet extraction of filters and/or disks
   12.3 Back-extraction with acid and base
   12.4 Macro-concentration
   12.5 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 Florisil clean-up
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 Concentration calculations for isotope dilution
   17.2 Internal standard recovery and concentration calculations
   17.3 Concentration in the aqueous sample
   17.4 Toxicity equivalents (TEQs)
18 Analysis of complex samples
   18.1 General
   18.2 Recovery of internal standards
19 Results and reporting
Annex A (informative) - Application of HRGC/HRMS
Annex B (informative) - Interlaboratory trial data
Annex C (informative) - Pollution prevention and waste management
Annex D (informative) - Additional extraction and clean up techniques
Bibliography

Describes a method for the determination of tetra- to octa-chlorinated dibenzo-p-dioxins ((PCDDs) and dibenzofurans (PCDFs) in waters and waste waters (containing less than 1% by mass solids) using high-resolution gas chromatography/high-resolution mass spectrometry (HRGC/HRMS).

This International Standard specifies a method for the determination of tetra- to octa-chlorinated dibenzo-p-dioxins (PCDDs) and dibenzofurans (PCDFs) in waters and waste waters (containing less than 1%by mass solids) using high-resolution gas chromatography/high-resolution mass spectrometry (HRGC/HRMS).

This International Standard is applicable to the seventeen 2,3,7,8-substituted PCDDs/PCDFs specified in Table1.

The detection limits and quantitation levels in this method are usually dependent on the level of interferences rather than instrumental limitations. The minimum levels (MLs) specified in Table2 are the levels at which the PCDDs/PCDFs can be determined with no interferences present. The method detection limit (MDL) for 2,3,7,8-TCDD has been determined as 4,4pg/l based on this method using a sample volume of 1l. Lower detection limits may be achieved by using a larger sample volume.

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 International Standard are met. The requirements for establishing method equivalency are given in 9.1.2.