BS EN 16167:2012 pdf download
BS EN 16167:2012 pdf download.Sludge, treated biowaste and soil- Determination of polychlorinated biphenyls(PCB) by gas chromatography with mass selective detection (GC-MS) and gaschromatography withelectron-capture detection(GC-ECD).
5 Interferences
5.1 Interference with sampling and extraction
Use sampling containers of materials (preferably of steel, aluminium or glass) that do not change the sample dunrig the contact time. Avoid plastics and other organic materials during sampling. sample storage or extraction. Keep the samples from direct sunlight and prolonged exposure to light.
During storage of the samples, losses of PCBs may occur due to adsorption on the walls of the containers. The extent of the losses depends on the storage time.
5.2 Interference with GC
Substances that co-elute with the target PCB may interfere with the determination. These interferences may lead to incompletely resolved signals and may. depending on their magnitude, affect accuracy and precision of the analytical results, Peak overlap does not allow an interpretation of the result Asymmetric peaks arid peaks being broader than the corresponding peaks of the reference substance suggest interferences.
Chromatographic separation between the following pairs can be critical. The critical pair PCB28 and PCB31 is used for selection of the capilLary column (see 8.2.2). If molecular mass differences are present, quantification can be made by mass selective detection If not or using LCD. the specific PCB Is reported as the sum of all PCBs present in the peak. Typically, the concentrations of the co-eluting congeners compared to those of the target congeners are low. When incomplete resolution is encountered, peak Integration shall be checked and. when necessary, corrected.
– PCB28—PCB31
– PCB52 – PCB73
– PCB1O1 – PCB89I PCB9O PCB1I8—PCBIO6
PCB138— PCB164 I PC8163
Presence of considerable amounts of mineral oil in the sample may interfere with the quantification of PCB in GC-MS. In presence of mineral oil, GC-ECD may be preferred or mineral oil can be removed using clean-up procedure G (see 10.4.8) using DMF!n4iexane,
Presence of tetractilorobenzyttoluene (TCBT)-mixtures may disturb the determination of the PCB with GCLCD
6 Safety remarks
PCBs are highly toxic end shall be handled with extreme care. Avoid contact with solid materials, solvent extracts and solutions of standard PCB with the body shall not be allowed to occur. It is strongly advised that standard solutions are prepared centrally in suitably equipped laboratories or are purchased from supplier5 specialised in their preparation.
Solvent solutions containing PCB shall be disposed of In a manner approved for disposal of toxic wastes.
For the handling of hexane precautions shall be taken because of its neurotoxic properties.
National regulations shall be followed with respect to all hazards associated with this method.
7 Reagents
7.1 General
MI reagents shall be of recognised analytical grade The purity of the reagents used shall be checked by running a blank test as described in 10.1 The blank shall be less than 50 % of the lowest reporting limit.
7.2 Reagents for extraction
7.2.1 Acetone (2.propanon.), (CH3)2 Co.
7.2.2 n-heptane, C7H18.
7.2.3 Petroleum ether, boiling range 40 C to 60 C.
Hexane-like solvents with a bolng range between 30 C and 69 C are allowed.
7.2.4 Anhydrous sodium sulfate, Na2SO4. The anhydrous sodium sulfate shall be kept carelully sealed.
7.2.5 Distilled water or water of equivalent quality. H20.
7.2.6 Sodium chloride, NaCl, anhydrous.
7.2.7 K..p.r substance High boiling compound, i.e. octane, nonane.
7.3 Reagents for clean-up
7.3.1 Clean-up A using aluminium oxide
7.3.1.1 Aluminium oxid., A1203,
Basic or neutral, speofic surface 200 m2Ig. activity Super I according to Brockmann
7.3.1.2 Deactivated aluminium oxide
Deactivated with approximately 10 % water
Add approximately 109 of water (7.2.5) to 90 g of aluminium oxide (7.3.1.1). Shake until all lumps have disappeared. Allow the aluminium oxide to condition before use for some 16 h, sealed from the air, use it for maximum two weeks
NOTE The activity depends on the water content. can be necessary ID adjust the water content.
7.3.2 Clean-up B using silica gel 64) for column chromatography
7.3.2.1 SilIca g.l 60. particle size 63 pm to 200 pm.
7.3.2.2 Silica gel 60. waler content: mass fraction w(H20) 10 %.
Silica gel 60 (7.3.2.1). heated for at least 3 h at 4500, cooled down in a desiccator and stored containing magnesium perchiorate or a suitable drying agent. Before use heat at least for 5 h at 130 C in a drying oven, Then allow cooling in a desiccator arid add 10 % water (mass fraction) wi a flask Shake for 5 mm intensively by hand until all lumps have disappeared and then for 2 h in a shaking device. Store the deactivated silica gel in the absence of air, use ii for maximum of two weeks.
