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 gas chromatography with electron-capture detection (GC-ECD).
Keeper substance (7.2.7) is added to the eluate, and then the eluate is reduced to the desired volume (see 10.3)
NOTE Dunng use of the gel perrneabon column a small shift in volume to be collected may occur. This is visible in a decrease of recovenes of the internal standards. If this occurs, readjustment of the sampled volume may be necessary.
10.4.5 Clean-up D — Florisil
Add into a chromatographic tube (8.1 .11) 5 mm sodium sulfate (7.2.4). 1.5 g Florisil (7.3.4.1), and again 5 mm sodium sulfate. To fix the mixture, place glass wool (8.1.9) on the top. Rinse the column with approximately 50 ml isooctane (7.3.4.2). Apply the extract to the column. Rinse the extraction tubelvessel for two times with
1 ml isooctaneltoluene (95/5) (7.3.4.3) and give it onto the column. Afterwards elute with 7 ml isooctane !toluene. One drop of keeper substance (7.2.7) is added to the eluate, and then the eluate is reduced to the desired volume (see 10.3).
10.4.6 Clean-up E—silica H2SO4Isllica NaOH
The combined silica H2S04/silica NaOH phase Is effective in the removal of polar compounds, polycyclic aromatic compounds and triglycerides,
Prepare an adsorption column by pouring consecutively 1 g silica NaOH (7.3.5.4). 5 9 silica H2S04 (7.3.5.2) and 29 sodium sulfate (7.2.4) in a clean chromatography column (8.1.11). Add a sufficient amount of ri-hexane (7.3.5.5) and elute until the top of the n-hexane phase reaches the top of the sodium sulfate layer. Apply the extract to the top of the sodium sulfate layer and make it penetrate into the sodium sulfate layer. Elute with about 60 ml of n-hexane and collect the entire n-hexane fraction. One drop of keeper substance (7.2.7) is added to the eluate. and then the eluate is reduced to the desired volume (see 10.3).
10.4.7 Clean-up F — Benzenesulfonlc acidisulfurlc acid
Benzenesulfonic acidlsulfuric acid pretreatment is effective If the sample contains large amounts of oil.
Condition the silica cartridges by eluting three times with 2 ml portions of n-hexane. Discard the eluate and vacuum dry the columns. Apply 500 p1 of the extract to the column and let slowly seep into the column. After 30 s, add 2 x 1 ml n-hexane like solvent (7.3.5.5) to the column and wait once again for 30 s. Elute the PCB from the column with 3 x 0.5 ml of n-hexane like solvent (7.3.5.5). Collect the entire eluate. Keeper substance (7.2.7) is added to the eluate, and then the eluate is reduced to the desired volume (see 10.3).
10.4.8 Clean-up G — DMF/n-hexane partitioning for aliphatic hydrocarbons removal
Extracts of samples containing a high amount of aliphatic compounds (e.g. oil) need additional clean-up by dimethylformamide/hexane partitioning
This additional clean-up step shall only be applied in case of GC-MS and not for GC-ECD. Indeed in the later case, the extracts are more diluted and interference by aliphatic hydrocarbons are not expected in the ECD signal.
Transfer the extract to a separating funnel of 100 ml and extract the PCBs with 25 ml of DMF (7,3.7.1).
Repeat twice. Transfer the combined DMF extracts to a separatory funnel of 500 ml, add 100 ml of water
(7.2.5) and extract the PCBs with 50 ml of n-hexane (7.3.5.5). Repeat once. One drop of keeper substance
(7.2.7) is added to the eluate. and then the eluate is reduced to the desired volume (see 10.3).
10.4.9 Clean-up H — concentrated sulfuric acid
This treatment is recommended if sulfoniable compounds are present. Face shields, gloves and protective clothing shall be worn.
Transfer the extract to a convenient stoppered glass vial. Dilute the extract to 20 ml with petroleum ether (7.2.3). Pour in 5 ml of concentrated sulfuric acid (7.3.81) and shake vigorously at intervals for 5 mm. Allow to
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BS EN 16167:2012
EN 161 67:2012 (E)
separate completely (about 15 mm). Take the upper layer, rinse the remaining sulfuric acid with petroleum ether. Keeper substance (7.2.7) is added to the eluate. and then the eluate is reduced to the desired volume (see 10.3).
10.4.10 Clean-up I — TBA sulfite reagent
Add 2 ml of TBA sulfite reagent (7.3.9.1) to 1 ml of concentrated extract and shake for 1 mm. Add 10 ml of water (7.2.5) and shake again for 1 mm. Separate the organic phase from the water with a Pasteur pipette and add a few crystals of anhydrous sodium sulfate (7.2.4) to remove the remaining traces of water.
10.4.11 Clean-up J — Clean-up using pyrogenic copper to remove elemental sulfur and some other organic sulfur compounds
Add 1 ml ol the extract (in petroleum ether) to a centrifuge tube. Add 100 mg pyrogenic copper powder
(prepared according to procedure given In 7.3.10). Centrifuge the tube more than 5 mm at approximately
3 500 rpm (ensure that there is no visible turbidity).BS EN 16167-2012 pdf download.