EN 71-7-2014 pdf download.Safety of toys – Part 7 : Finger paints – Requirements and test methods.
The sample preparation is the same for all analytes using the solvent and so’id phase extraction stages. However, to achieve the lower limits specified for B[aJP the concentration stage has been separately described to HCB and PCB congeners.
E.6.2 Sample preparation
A screw cap amber bottle (E.3.1) Is filled with approximately 6 g of anhydrous sodium sulphate (E2.8). Weigh accurately (1,0 ± 0,1) g of the test portion onto the surface of the anhydrous sodium sulphate and record the weight (M). Add an additional 6g of anhydrous sodium sulphate to cover the test portion and Lightly close the screw cap.
Shake the bottle vigorously for (60 ± 5) s to mix the test portion and sodium sulphate. Remove the cap and allow the mixture to stand for 24 h ± 1 h under standard laboratory conditions ensuring the mixture will not come into contact with any possible contaminants.
After 24 h. replace the screw cap onto the amber bottle and shake vigorously again for a further (60 ± 5) S. The mixture shou’d consist of particles no larger than 1 mm to 5 mm, where larger particles have formed a glass rod can be used to break up the larger particles.
E.6.3 Solvent extraction
E.6.3.1 Solvent extraction of soluble HCB and PCBs
Transfer the mixture in E.6.2 into a glass microfibre thimble (E.3.3) and add a filter paper disc to the top of the thimble. Insert the thimble into a soxhlet extractor (E.3,4) and connect to a water cooled condenser (E.3.5). Add approximately 175 ml of cyclohexanelacetone (E.2.6) into a 250 ml round bottom flask (E.3.6) and connect to the soxhlet extractor, place on a heating mantle (E.3.7) and reflux gently for > 6 Ii.
Allow sufficient time for the cyclohexane/acetone to cool before disconnecting the soxhlet extractor and gently evaporate the cydohexane/acetone extract to approximately 5-10 ml using a rotary evaporator or equivalent sample concentration system (E3.8).
Transfer the cyclohexane/acetone extract into a graduated gLass tube washing with 2 x 3 ml cyclohexane and evaporate the extract to approximately 3 ml under a gentle stream of nitrogen (E.3.8).
E.6.3.2 Solvent extraction of soluble B(oJP
Transfer the mixture in E.6.2 into a glass microfibre thimble (E.3.3) and add a filter paper disc to the top of the thimble. Insert the thimble into a soxhlet extractor (E.3.4) and connect to a water cooled condenser (E.3.5). Add approximately 200 ml of toluene/acetone (E.2.7) into a 250 ml round bottom flask (E.3.6) and connect to the soxhiet extractor, place on a heating mantle (E,3.7) and reflux gently for> 6 h.
Allow sufficient time for the toluenelacetone to cool before disconnecting the soxhlet extractor and gently evaporate the toluene/acetone extract to approximately 3 ml using a rotary evaporator or equivalent sample concentration system (E.3.8).
Transfer the toluenelacetone extract into a graduated glass tube washing with I ml toluene and evaporate the extract to approximately 3m1 under a gentle stream of nitrogen (E.3.8).
E.6.4 Solid phase extraction
E.6.4.1 Solid phase extraction of HCB and PCBs
Transfer the extract obtained in E.6.3 onto a column containing kieselguhr (E.3.9) and leave to stand for approximately 1 h. Then wash the column with 3 x 5m1 portions of cyclohexane (E.2.2) collecting the eluent into a suitable glass vessel. To the glass vessel and eluent add approximately 6 ml of 2,2,4-tnmethdpentane
(E.2.4).
E.6.4.2 Solid phase extraction of B[ajP
Transfer the extract obtained in E.6.3.2 onto a column containing kieselguhr (E.3.9) and leave to stand for approximately 1 h. Then wash the column with 3 5 ml portions of toluene (E.2.5) collecting the eluent into a suitable glass vessel.
E.6.5 Sample concentration for determining HCB and PCB congeners
Evaporate the eluent obtained In E.6.4 to approximately 3 ml using the sample concentrator (E.3.8) and quantitatively transfer into a graduated test tube and make to the 6 ml mark with 2,2.4-tnmethylpentane. Transfer 1 ml to a sample vial and add 0.025 ml of the HCB internal standard solution (E.2.12.1) and 0,05 ml of each PCB internal standard solutions (E.2.12.2 and E.2.12.3) for quantitative determination by GC-MS.
E.6.6 Sample concentration for determining B(a]P
Evaporate the eluent obtained in E.6.4 to approximately 3 ml using the sample concentrator (E.3.8) and quantitatively transfer into a graduated test tube and make to the 4 ml mark with 2,2.4-trimethylpentane. Transfer 1 ml to a sample vial and add 0,05 ml of the B[a]P internal standard solution (E.2.12.4) for quantitative determination by GC-MS.
E.6.7 Gas chromatography conditions
Set up the gas chromatography-mass spectrometer detection system according to manufacturer’s instructions, to monitor the selected mass fragmentation ions for HCB, PCB congeners, and B(a]P.
The following conditions have been shown to be suitable for HCB and PCB congeners.EN 71-7-2014 pdf download.