BS EN 71-7:2002 pdf download

BS EN 71-7:2002 pdf download.Safety of Toys Part 7: Finger paints — Requirements and test methods.
0.2.4 Citrat&sodium hydroxide buffer, c(tnsod.um citrate) = 0,06 moê’l. pH 6, p’elieated to 70 eC or 37 C:
Dissolve 12,6 g citric acid monohydrate and 6.4 g sodium hydroxide in 900 ml water. Acust the volume to 1 1
NOTE Ready•for-use’ solution, Merck 1*. 1.09437. has been found 5uitable,
D.2.5 Sodium dittlionile solution, freshly dissolved in water. p — 200 mg/mI
0.2.6 Porous, granular kieselguhr” SPE column
NOTE Chrownabondj XTR has been found suitable,
0.2.7 Amine standards, primanly those listed in Tables 3 and 4, (highest available purity)
NOTE The amines in Tables 3 and 4 are human carcinogens or cancer suspect agents (MAI(.lisl III Al/Ill A2: EU C1IC2, respectively). The handing of these chemicals reopires the ulmost care and commensurate safely measures
D.2.8 Internal standards for gas chromatography
D.2.8.1 IS 1; Naphthalene-ci. CAS No. 1146-65-2
D.2.8.2 lS2: 2,4,5-Tnchloroaniline, CAS No. 636-30-6
D.2.8.3 IS 3: 4-Am ino-2-melhylquinoline. GAS No. 6628-04-2
D.2.8.4 IS4: Anthracene-d10. CAS No. 1719-06-8
D.2.9 Standard solutions
D.2.9.1 CalIbration solution of amines of Tables 3 and 4.p 10.0 igimI of each amine of a suitable solvent
D.2.9.2 Internal standard solution of IS 1 to IS 4, (D.2.8.1 — D.2.8.4) p — 10,0 pg/nil of each required IS of a suitable solvent
D2.9.3 Solutions of ammes of Tables 3 and 4 for procedure check, p = 30,0 pglrnl of each amine of a suitable solvent
NOTE The solvent used a depend on the clwomatogrhic method chosen for analysis.
The stability of the amine solutions shall be demonstrated.
D.3 Apparatus
Ordinary laboratory equipment, and
D.3.1 Reaction vessel (20 ml to 50 ml) of ternperature-res*stant glass with tight-fitting screw cap
D.3.2 Water bath, drying oven or heating block: all devices thorrnostatod. capable of maintaining a tornporaw of (37±2) C and ( 70±2) °C
D.3.3 Column made from glass or polypropylene, 25 mm to 30 mm internal diameter, 140 mm to 150 mm length, filled with about 20 g porous, granular kieselguhr SPE material, fitted on the outlet with a glass fibre filter (or commercial SPE column).
NOTE Chromabondic XTR iMacherey-Nagel Catalogue No. 730 507) has been Iound suitable.
D.3.4 Vacuum rotary evaporator or equivalent low temperature sample concentration system
D.3.5 Plpettes 10 ml. 5 ml, 2 ml. 1 ml
D.6,2 Reductive cleavage of azo colourants
17 ml butler (D.2.4). preheated to (70 ± 2) “C, is added to the sample. The reaction vessel is tightly closed and after bnef vigorous shaking to homogenize the contents Is kept at (70 ±2) “C for 30 mm.
To achieve reductive cleavage of the azo colourants 3,0 ml of sodium dithionite solution (D.2.5) is added to the reaction vessel, The vessel is immediately tightly sealed, thoroughly shaken and kept again at (70 ± 2) “C for another (30±2) mm, and then cooled to ambient temperature within 2 mm.
D.6.3 extraction of soluble amines
For the determination of tree aromatic ammnes (see 4.5.2), the reductive cleavage (0.6.2) is not carried out. Irstead, 20 ml of the butler solution (D.2.4) preheated only to (37 ± 2) “C Is added to the sample. The reaction vessel is tightly closed and alter brief vigorous shaking to homogenize the contents Is kept at (37±2) “C for 30 mirm.
D.6.4 Solid phase extraction and concentration Of amines
The solution from D.6.2 or D.6.3. as appropriate, is poured onto the SPE column without rinsing the vessel with water or butler. The aqueous phase is left for 15 mm to absorb onto the column. The amines are then extracted twice with 40 ml tort’butyl methyl ether as described below.
Before extracting the SPE column, the first 40 ml of tert-butyl methyl ether is divided into portions of 2 x 10 ml and 1 x 20 ml for rinsing the reaction vessel. 10 ml of ether is added to the vessel, it is closed and shaken vigorously. After allowing 15 mm for the water phase to absorb onto the column, the tert-butyl methyl ether is decanted from the reaction vessel onto the column. The eluant is collected in a 100-mi round-bottom flask. This operation is repeated with the remaining 10-mi and 20-mi portions of tert-butyf methyl ether. Finally, the second 40 ml is poured directly onto the column. The eluate is usually clear and needs no drying.
The rert-butyl methyl ether extract is carefully concentrated at a maxm,um temperature of 25 “C using a rotary evaporator with vacuum, or equivalent sample concentrator, to about I ml (not to dryness!). If ferl-butyl methyl ether is not the required chromatographe solvent, the remainder of the ether is carefully removed under a light flow of Inert gas. It tert•butyl methyl ether is the required chromatographic solvent, the residue Is quantitatively transferred to a small graduated tube and the volume made up to 2.0 ml with washings from the round-bottom flask.