BS EN 71-12:2016 pdf download. Safety of toys Part 1 2: N-Nitrosamines and N-nitrosatable substances.
5 Principle
N-nitrosamines and N-nitrosatable substances migrate into a test solution. N-nitrosatable substances are converted to N-nitrosamines by acidification. The final test solutions are analysed for N-nitrosamines by a suitable validated analytical technique. The N-nitrosamines and N-nitrosatable substances are expressed in mg/kg of sample.
The test solution for N-nitrosamines in finger paints is water. The test solution for N-nitrosatable
substances in finger paints and for N-nitrosamines and N-nitrosatable substances in elastomers is saliva test solution.
6 Reagents and apparatus
6.1 Reagents
Unless otherwise specified, all reagents shall be of analytical grade and distilled water, or water of
equivalent purity conforming to at least grade 3 of EN ISO 3696.
6.1.1 Sodium hydrogen carbonate (CAS 144-55-8)
6.1.2 Sodium chloride (CAS 7647-14-5)
6.1.3 Potassium carbonate (CAS 584-08-7)
6.1.4 Sodium nitrite (CAS 7632-00-0)
6.1.5 Hydrochloric acid (CAS 7647-01-0), aqueous solution, c(HCL) = 0,1 mol/l
6.1.6 Sodium hydroxide (CAS 1310-73-2), aqueous solution, c(NaOH) = 0,1 mol/l
6.1.7 Saliva test solution
Dissolve (4,2 ± 0,021) g of the sodium hydrogen carbonate (6.1.1), (0,5 ± 0,002 5) g of the sodium
chloride (6.1.2), (0,2 ± 0,001 0) g of the potassium carbonate (6.1.3) and (0,03 ± 0,000 15) g of the
sodium nitrite (6.1.4) in water and dilute to (950 ± 5) ml with water. Adjust to pH 9,0 ± 0,1 if necessary by adding the hydrochloric acid solution (6.1.5) or sodium hydroxide solution (6.1.6) drop by drop.
Transfer into a 1 l volumetric flask and dilute to the mark with water.
This solution has a limited stability. Saliva test solution kept for more than five days shall not be used.
6.1.8 Hydrochloric acid solution, c(HCL) = 1 mol/l.
6.1.9 Sodium hydroxide solution, c(NaOH) = 1 mol/l.
6.1.10 Methanol, ≥ 99,9 %, HPLC-grade.
6.1.11 Formic acid, ≥ 99,5 %, LC-MS grade.
6.1.12 Eluent A: 0,1 % (volume fraction) formic acid in water.
6.1.13 Eluent B: 0,1 % (volume fraction) formic acid in methanol.
6.2.1 N-nitrosamines or their solutions, with known purities.
6.2.2 Internal standard, d8-N-nitrosodiethanolamine (d8-NDELA), with known purity.
6.2.3 Internal standard, d6-N-nitrosodimethylamine (d6-NDMA), with known purity.
6.3 Apparatus
Laboratory equipment that can come into contact with the sample shall be free from N-nitrosamines. Standard laboratory equipment and equipment appropriate for applying the test method shall be used. The following equipment could be used when applying the test method specified in this standard.
6.3.1 Vortex mixer
6.3.2 Shaking machine
6.3.3 Centrifuge, capable of achieving not less than 20 000 g
6.3.4 Glass balls
6.3.5 Conical flask, made of amber glass
6.3.6 Oven, capable of maintaining a temperature of (40 ± 2) °C
6.3.7 High performance liquid chromatography apparatus coupled with tandem mass
spectrometry equipped with atmospheric pressure ionization (APCI)BS EN 71-12 pdf download.