BS ISO 22032:2006 pdf download

BS ISO 22032:2006 pdf download.Water quality一Determination ofselectedpolybrominateddiphenyl ethers insediment and sewagesludge – – Method usingextraction and gaschromatography/massspectrometry.
5.7 SolutIons of the single reference substanc.s I lrit.rnal standards
Use commercially available solutions (may be in nonane. toluene or iso-octane) or prepare stock solutions. e.g. by dissolving 10mg of each or the reference substances (5.2, 5.3) in toluene (51) in an amber. 10-mi volumetric flask and brig to volume (concentration: I mfml). store at approximately -18 C in the dari.
5.8 Multicomponent stock solution of reference substances.
Accurately transfer between 100 p1 to 500 p1 of each single standard solution (5.7) into an amber. 10-mI volumetric flask and bring to volume with the appropriate solvent. e.g. toluene, or nonane. or iso-octane (5.1). (Concentrations are between 10 iiglml and 50 iiglml per substance.)
5.9 Calibration solutions for multicomponent-muitilevel calibration.
Prepare, e.g. seven calibration solutions with concentrations according to the detection capacity of the mass spectrometer. Combine the multicomponent stock solutions of reference substances (5.8), Internal standards (5.10) and. if necessary, Injection standard (5.12) to produce the solutions (e.g. shown In Table 5) by appropriate dilution with the appropriate solvent. e.g. toluene, or nonane, or Iso-octane (5.1).
in order to avoid potential photodegradation, store the solutions ii the dark. Check the concentrations of calibration solutions before use.
Use one of the calibration solutions to optimize the GC-MS system and to determine the retention times. As an alternative, determine and use relative retention times.
5.10 Stock solution of the internal standards
Prepare a stock solution of the internal standards at an appropriate concentration in. e.g. toluene or iso-octane (2,2,4-trimethlpentane). Dilute thés stock solution. See Table 5 for suggested concentrations of calibration solutions and sample extracts.
5.11 Clean-up material.
See Annex A.
5.12 InjectIon standard
Use an infection standard, e.g. dibrornooctafluorobiphenyl (Ci2Br2F), to determine recovery rates for the internal standard in each sample.
5.13 Baked sand.
Bake sand for at least 81, at 400 C.
6 Apparatus
Clean all glassware b niising with acetone (propanone) (5.1). Heating the glassware to 400 C wifi reduce blanks. Recalibrate volumetric apparatus prior to use If heated.
6.1 Wide-necked bottle, 1 000 ml up to 5 000 ml capacity, for wet sediment or sludge.
6.2 Fr..z. drying apparatus,
63 Deep freezer.
6.4 Mortar and pestle, or a grinding mill
6.5 DryIng ovens, capable of mainta.nang temperatures in the ranges of 100 C to 400 C for baking and
storage of clean-up materials, for bakg of glassware and for dry residue determination of samples.
6.6 Sieve shaker with appropriate sieve meshes (aperture size), e.g. 2 mm.
6.7 DesIccator.
6.8 Soxhlet extraction apparatus, consisting of round bottom flasks (e.g. 250 ml). Soxtilet extractors and Soxhiet thimbles (e.g. 27 mm x 100 mm). vertical condensers (e.g. 300 mm) and heating apparatus.
6.9 Evaporation device. eg. rotary evaporator, turbo evaporator or vacuum concentration device.
6.10 Glass columns for chromatographic clean-up.
6.11 Volumetric cylinders, 250 ml and 500 ml.
6.12 VolumetrIc flasks. I ml, 2 ml, 10 ml. and 25 ml.
6.13 Pasteur pipettes. e.g. 2 mL
6.1 4 SyrInges, 2 p1, 5 p1, 10 p1 and 50 p1, volume precision ± 2 %.
6.15 Sample vials.
Amber glass with fluoropolymer-lined screw-cap is most suitable.
6.16 Gas chromategraph, with either a splittess injection port or an on-column injection port coupled to a mass spectrometer (GC-MS) with electron impact or chemical ionization and appropriate reactant gas (e.g. CH4).
6.17 Analytical column.
Fused silica column with non-polar low bleed separating phase (see Annex B for examples), e.g. inner diameter c 0,25 mm, length 15 m to at maxmium 30 m (shorter columns for higher brominated congeners) A film thickness of 0,1 pm is recommended.
7 Sampling and sample pre-treatment
Take samples as speci6ed in ISO 5667-13 In a bottle (6.1). Store and transport in the dark at approximately 4 C. Pre-treat the samples immediately in the Laboratory by homogenizing and freeze-drying. Grind the samples using apparatus (6.4) and sieve them using a sieve staker (6.6) according to the analytical task.
Other extraction techniques, e.g. accelerated solvent extraction, and shorter extraction times may be used after performing comparability exercise with a 16 h Soxhlet extraction.