BS EN 71-5:1993+A2:2009
$215.11
Safety of toys – Chemical toys (sets) other than experimental sets
Published By | Publication Date | Number of Pages |
BSI | 2009 | 72 |
Specifies requirements for chemical toys other than those covered by EN 71-4 (BS 5665:Part 4).
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1 | BRITISH STANDARD BS EN 71-5:1993 BS 5665-5: 1993 Safety of toys – Part 5: Chemical toys (sets) other than experimental sets The European Standard EN 71-5:1993, with the incorporation of amendment A1:2006, has the status of a British Standard UDC 688.72:54:614.8:620.1 |
3 | EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM EN 71-5 +A1 Descriptors: Toys, games, chemical compounds, safety requirements, accident prevention, dangerous material, approved doses, specifications, packing, marking English version Safety of toys Part 5: Chemical toys (sets) other than experimental sets (includes amendment A1:2006) CEN European Committee for Standardization Comité Européen de Normalisation Europäisches Komitee für Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels © 1993 Copyright reserved to CEN members Ref. No. EN 71-5:1993 + A1:2006 E |
7 | Introduction 1 Scope |
8 | 2 Normative references 3 Definitions 3.1 plaster of Paris (gypsum) moulding set 3.2 ceramic and vitreous enamelling materials supplied in miniature workshop set |
9 | 3.3 oven hardening plasticized PVC-modelling clay set 3.4 plastic moulding set 3.5 embedding set 3.6 photographic developing set 3.7 adhesives, paints, lacquers, varnishes, thinners and cleaning agents supplied or recommended in model sets 3.7.1 adhesive 3.7.2 water-based paint 3.7.3 paint and lacquers containing solvents 3.7.4 varnishes 3.7.5 thinners and cleaning agents (solvents) 4 Plaster of Paris (gypsum) moulding sets 4.1 Marking 4.2 Safety rules 5 Ceramic and vitreous enamelling materials supplied in miniature workshop sets 5.1 Chemical preparations 5.2 Marking 5.3 Safety rules |
10 | Table 1 – Chemical preparations Table 2 – Plasticizers 6 Oven hardening plasticized PVC-modelling clay sets 6.1 Chemical substances 6.2 Marking 6.3 Safety rules |
11 | 7 Plastic moulding sets 7.1 Polystyrene granules 7.1.1 Chemical substances Table 3 – Polystyrene 7.1.2 Marking 7.1.3 Safety rules 7.2 Embedding sets 7.2.1 Packaging 7.2.2 Marking 7.2.3 Safety rules 8 Photographic processing sets 8.1 Chemical substances and preparations 8.2 Packaging |
12 | Table 4 – Maximum amounts of chemical substances 8.3 Marking 8.3.1 Marking of the outer packaging 8.3.2 Marking of the individual packaging 8.4 Safety rules 9 Adhesives, paints, lacquers, varnishes, thinners and cleaning agents (solvents) supplied or recommended in model sets 9.1 General 9.2 Adhesives 9.2.1 Water-based adhesives |
13 | Table 5 – Basic materials for water-based adhesives and water-based paints and lacquers 9.2.1.1 Liquid adhesives for paper and wood Table 6 – Special materials for adhesives for paper and wood and water-based paints and lacquers Table 7 – Special additives for liquid adhesives for paper and wood 9.2.1.1.1 Packaging 9.2.1.1.2 Marking 9.2.1.2 Adhesive sticks for paper |
14 | Table 8 – Special material for adhesive sticks for paper 9.2.1.2.1 Packaging 9.2.1.2.2 Marking 9.2.2 Solvent-based adhesives 9.2.2.1 Multi-purpose adhesives Table 9 – Basic materials for multi-purpose adhesives 9.2.2.2 Contact adhesives Table 10 – Basic materials for contact adhesives 9.2.2.3 Special adhesives Table 11 – Basic materials for special adhesives |
15 | Table 12 – Solvents 9.2.2.4 Packaging 9.2.2.5 Marking 9.2.2.6 Safety rules 9.3 Water-based paints and lacquers Table 13 – Organic solvents and film forming agents |
16 | 9.3.1 Packaging 9.3.2 Marking 9.3.3 Safety rules 9.4 Solvent-based paints, lacquers, thinners and cleaning solvents Table 14 – Basic materials Table 15 – Solvents 9.4.1 Packaging 9.4.2 Marking 9.4.3 Safety rules |
17 | 10 Marking 10.1 Marking of the outer packaging 10.1.1 Manufacturer’s identification 10.1.2 Warning and caution phrases 10.2 Marking of individual containers and packagings a) The name of the chemical substance or preparation as given in the relevant tables and clauses, if necessary according to the … b) The required danger symbol and the required risk/safety phrases specified in Directive 67/548/EEC17) (with subsequent amendments and adaptations). 11 Instructions for use 11.1 General 11.2 Contents list a) Where relevant, the chemical(s) supplied. b) Where relevant, the risk/safety phrases specified in Directives 67/548/EEC17) (with subsequent amendments and adaptations) and 88/379/EEC17) (with subsequent amendments and adaptations) as appropriate to each particular substance. c) Where relevant and if the substances/preparations are dangerous according to the Directives mentioned in 11.2 b), an empty sp… d) General first aid information as follows: |
18 | e) Specific first aid information when appropriate. 11.3 Advice for adult supervision a) This chemical toy is for use only for children over the age of …. years (as appropriate). b) Read and follow these instructions, the safety rules and the first aid information and keep them for reference. c) Incorrect use of chemicals can cause injury and damage to health. Only carry out those activities which are listed in the instructions. d) Because children’s abilities vary so much, even within age groups, supervising adults should exercise discretion as to which … e) The supervising adult should discuss the warnings, safety information and the possible hazards with the child or children bef… f) The area surrounding the activity should be kept clear of any obstructions and away from the storage of food. It should be well lit and ventilated and close to a water supply. A solid table with a heat resistant top should be provided. g) The working area should be cleaned immediately after carrying out the activity. 11.4 Safety rules 11.5 Instructions for carrying out the activities 11.6 Spills and disposal of chemicals 12 Test methods 12.1 General 12.2 Determination of elements in ceramic and vitreous enamelling materials 12.2.1 Principle |
19 | 12.2.2 Standards and reagents 12.2.2.1 Standards Table 16 – Standards 12.2.2.2 Reagents Table 17 – Reagents 12.2.3 Apparatus 12.2.3.1 Platinum crucible 12.2.3.2 Muffle furnace, 12.2.3.3 Analytical balance, 12.2.3.4 Glassware (beaker, funnel, volumetric flask and pipettes) 12.2.3.5 Atomic emission spectrometer 12.2.4 Preparation of standard solutions 12.2.4.1 Multi-element standard solution I 12.2.4.2 Multi-element standard solution II 12.2.4.3 Multi-element standard solution III 12.2.5 Blank solution 12.2.6 Sampling 12.2.7 Sample preparation 12.2.8 Procedure Table 18 – Wavelengths |
20 | 12.2.9 Evaluation of results 12.2.9.1 General Table 19 – Conversion factors 12.2.9.2 Calculation of the pigment contents in the enamel samples 12.2.9.2.1 Calculation of the concentration of copper oxide (CuO) and tin dioxide (SnO2) 12.2.9.2.2 Calculation of the concentration of aluminium cobalt oxide (CoO.Al2O3) 12.2.9.2.3 Calculation of the concentration of praseodymium zirconium silicate (Pr2O3 + ZrSiO4) 12.2.9.2.4 Calculation of the concentration of vanadium zirconium silicate (V2O4 + ZrSiO4) 12.2.9.2.5 Calculation of the concentration of di-iron oxide (Fe2O3), iron zirconium silicate (Fe2O3 + ZrSiO4) and zirconium ortho silicate (ZrSiO4) |
21 | 12.2.10 Test report a) type and identification of the product and/or material tested; b) a reference to this European Standard; c) the results of the tests expressed as x % (m/m) pigment content rounded to 0,01 % (m/m), but not more than three significant digits; d) any deviation from the test procedure specified; e) date of test. 12.3 Determination of plasticizers in oven hardening polyvinyl chloride (PVC) modelling clay sets 12.3.1 Principle |
22 | 12.3.2 Standards and reagents 12.3.2.1 Standards Table 20 – Phthalic acid esters Table 21 – Adipic acid polyesters a) Polymeric plasticizer derived from adipic acid and polyhydric alcohols. b) Polyester adipate. Table 22 – Citric acid esters Table 23 – Alkylsulfonic acid esters 12.3.2.2 Reagents Table 24 – Solvents |
23 | 12.3.3 Apparatus 12.3.3.1 Analytical balance, precision 0,1 mg 12.3.3.2 Spark-proof heating mantle/water bath 12.3.3.3 Oven, capable of maintaining a temperature of (105 ± 5) ºC 12.3.3.4 Desiccator chamber 12.3.3.5 150-ml or 250-ml glass stoppered flat bottomed flask 12.3.3.6 Soxhlet glass extractor with siphon cup 12.3.3.7 Soxhlet cellulose thimble (Whatman or equivalent) 12.3.3.8 Water-cooled glass condenser 12.3.3.9 Cotton wool 12.3.3.10 Glass volumetric flask 12.3.3.11 General volumetric glassware 12.3.3.12 Stainless steel scalpel blade 12.3.3.13 Attenuated Total Reflectance Fourier Transform Infra Red Spectrometer (ATR-FT-IR) 12.3.3.14 Gas chromatograph with mass spectrometer detector (GC-MS) Figure 1 – Total ion chromatogram of a mixture of phthalates |
24 | Figure 2 – Total ion chromatogram of a mixture of phthalates 12.3.4 Preparation of standard solutions 12.3.4.1 Stock solutions Table 25 – Stock solutions I |
25 | Table 25 – Stock solutions I (concluded) Table 26 – Stock solutions II 12.3.4.2 Calibration solutions Table 27 – Calibration solutions 12.3.4.3 Stability of standard solutions 12.3.5 Sampling 12.3.6 Sample preparation |
26 | 12.3.7 Procedure 12.3.7.1 Extraction of phthalic acid esters, citric acid esters and alkylsulfonic acid esters 12.3.7.2 Extraction of adipic acid polyesters 12.3.7.3 Evaporation of the solvent and weighing 12.3.7.4 Blank determination 12.3.7.5 GC-MSD determination of phthalic acid esters, citric acid esters and alkylsulfonic acid esters 12.3.7.6 ATR-FT-IR identification of adipic acid polyesters |
27 | 12.3.8 Evaluation of Results 12.3.8.1 Calculation of solvent-extractable content containing plasticizers 12.3.8.1.1 Content of hexane extractable material, in % (m/m), identified as phthalic, citric and alkylsulfonic acid esters by GC-MS 12.3.8.1.2 Content of methanol extractable material, in % (m/m), identified as adipic acid polyester by ATR-FT-IR 12.3.8.1.3 Content of combined (hexane + methanol) extractable material % (m/m) 12.3.8.2 Calculation and identification of plasticizer content by GC-MS analysis 12.3.8.2.1 Identification of plasticizers 12.3.8.2.2 Calculation of plasticizers content by GC-MS 12.3.8.2.2.1 Content of phthalic acid ester, in % (m/m), by GC-MS 12.3.8.2.2.2 Content of citric acid ester, in % (m/m), by GC-MS |
28 | 12.3.8.2.2.3 % (m/m) Alkylsulfonic acid ester content by GC-MS 12.3.9 Test report a) type and identification of the product and/or material tested; b) a reference to this European Standard; c) the results of the tests expressed as: d) any deviation from the test procedure specified; e) date of test. 12.4 Determination of the emission of benzene, toluene and xylenes from oven hardening plasticised PVC modelling sets and plastic moulding sets 12.4.1 Principle 12.4.2 Standards and reagents Table 28 – Standards Table 29 – Solvents 12.4.3 Apparatus 12.4.3.1 Gas chromatograph with mass spectrometer detector (GC-MS) |
29 | 12.4.3.2 Headspace analysis conditions 12.4.3.3 Other laboratory equipment 12.4.3.3.1 Analytical balance, precision 0,1 mg 12.4.3.3.2 Refrigerator, capable of maintaining a temperature of (4 ± 2) ºC 12.4.3.3.3 Brown glass vials for headspace sampling 12.4.3.3.4 Volumetric glass pipettes, 0,5 ml, 1 ml, 2 ml, 10 ml and 20 ml capacity 12.4.3.3.5 Brown glass volumetric flasks, 10 ml, 20 ml, 50 ml and 100 ml capacity 12.4.3.3.6 Syringe, 1 000 µl capacity 12.4.4 Preparation of standard solutions 12.4.5 Sampling 12.4.6 Sample preparation 12.4.7 Procedure 12.4.8 Evaluation of results |
30 | 12.4.9 Test report f) type and identification of the product and/or material tested: g) a reference to this European Standard; h) the results of the tests expressed as: benzene emitted from PVC or polystyrene, in mg/kg; toluene emitted from PVC or polystyrene, in mg/kg; xylene emitted from PVC or polystyrene, in mg/kg; i) any deviation from the test procedure specified; j) date of test. 12.4.10 Critical control points 12.5 Determination of styrene content in polystyrene granules 12.5.1 Principle 12.5.2 Standards and reagents 12.5.2.1 Standards Table 30 – Standard 12.5.2.2 Reagents Table 31 – Reagents 12.5.3 Apparatus 12.5.3.1 12.5.3.2 General equipment and glassware used in laboratory 12.5.3.3 Analytical balance, precision 0,1 mg 12.5.3.4 Centrifuge, able to maintain at least 2 300 g 12.5.3.5 Refrigerator, capable of maintaining a temperature of (4 ± 2) ºC |
31 | 12.5.3.6 Glass containers equipped with a glass stopper 12.5.3.7 Volumetric flask and volumetric pipettes 12.5.4 Preparation of the standard solutions 12.5.5 Sampling 12.5.6 Sample preparation 12.5.7 Procedure 12.5.8 Evaluation of results 12.5.9 Test report k) type and identification of the product and/or material tested; l) a reference to this European Standard; m) results of the tests reported as: – content of styrene, in mg/kg polystyrene; n) any deviation from the test procedure specified; o) date of test. 12.6 Identification and determination of substances in photographic processing sets 12.6.1 General 12.6.2 Identification of cations and anions of inorganic substances in photographic sets Table 32 – Inorganic substances in photographic sets |
32 | 12.6.2.1 Method for ammonium cation in ammonium thiosulfate 12.6.2.1.1 Principle 12.6.2.1.2 Standards and reagents 12.6.2.1.2.1 Standard Table 33 – Standard 12.6.2.1.2.2 Reagents Table 34 – Reagents 12.6.2.1.3 Apparatus 12.6.2.1.4 Procedure 12.6.2.2 Method for sodium cation in sodium carbonate or sulfite or thiosulfate or disulfite 12.6.2.2.1 Principle 12.6.2.2.2 Standards and reagents 12.6.2.2.2.1 Standard Table 35 – Standards 12.6.2.2.2.2 Reagent Table 36 – Reagent 12.6.2.2.3 Apparatus 12.6.2.2.3.1 Bunsen burner 12.6.2.2.3.2 Magnesia bacilli (stick) or platinum wire 12.6.2.2.4 Procedure 12.6.2.3 Method for potassium cation in potassium bromide 12.6.2.3.1 Principle 12.6.2.3.2 Standards and reagents 12.6.2.3.2.1 Standard Table 37 – Standards 12.6.2.3.2.2 Reagent Table 38 – Reagents 12.6.2.3.3 Apparatus 12.6.2.3.3.1 Bunsen burner 12.6.2.3.3.2 Magnesia bacilli (stick) or platinum wire 12.6.2.3.3.3 Cobalt glass 12.6.2.3.4 Procedure |
33 | 12.6.2.4 Method for thiosulfate anion in sodium/ammonium thiosulfate 12.6.2.4.1 Principle 12.6.2.4.2 Standards and reagents 12.6.2.4.2.1 Standard Table 39 – Standards 12.6.2.4.2.2 Reagents Table 40 – Standards 12.6.2.4.3 Apparatus 12.6.2.4.4 Procedure 12.6.2.5 Method for sulfite anion in sodium sulfite 12.6.2.5.1 Principle 12.6.2.5.2 Standards and reagents 12.6.2.5.2.1 Standard Table 41 – Standards 12.6.2.5.2.2 Reagent Table 42 – Reagents 12.6.2.5.3 Apparatus 12.6.2.5.3.1 Test tube 12.6.2.5.3.2 Spot plate 12.6.2.5.4 Procedure 12.6.2.6 Method for disulfite in disodium disulfite 12.6.2.6.1 Principle 12.6.2.6.2 Standards and reagents 12.6.2.6.2.1 Standard Table 43 – Standard 12.6.2.6.2.2 Reagent Table 44 – Reagent 12.6.2.6.3 Apparatus 12.6.2.6.3.1 Infrared spectrometer (IR), range 4 000 cm-1 to 400 cm-1 12.6.2.6.3.2 Oven, capable of maintaining a temperature of (105 ± 2) ˚C |
34 | 12.6.2.6.4 Procedure Figure 3 – IR-spectrum of sodium disulfite Na2SO5 |
35 | Figure 4 – IR-spectrum of sodium sulfite Na2SO3 12.6.2.7 Method for carbonate anion in sodium carbonate 12.6.2.7.1 Principle 12.6.2.7.2 Standards and reagents 12.6.2.7.2.1 Standards Table 45 – Standards 12.6.2.7.2.2 Reagents Table 46 – Reagents 12.6.2.7.3 Apparatus 12.6.2.7.3.1 Test tube 12.6.2.7.3.2 Water bath 12.6.2.7.3.3 Tube with a fermentation lock 12.6.2.7.4 Procedure 12.6.2.8 Method for bromide anion in potassium bromide 12.6.2.8.1 Principle |
36 | 12.6.2.8.2 Standards and reagents 12.6.2.8.2.1 Standards Table 47 – Standards 12.6.2.8.2.2 Reagents Table 48 – Reagents 12.6.2.8.3 Apparatus 12.6.2.8.4 Procedure 12.6.2.9 Evaluation of results 12.6.3 Gravimetric determination of inorganic substances 12.6.3.1 Principle 12.6.3.2 Standards and reagents 12.6.3.3 Apparatus 12.6.3.3.1 Analytical balance, precision 0,1 mg 12.6.3.3.2 Crucible 12.6.3.3.3 Desiccator 12.6.3.3.4 Muffle furnace 12.6.3.3.5 Oven, capable of maintaining a temperature of (105 ± 2) ˚C 12.6.3.4 Procedure 12.6.3.5 Evaluation of results |
37 | 12.6.4 Identification of organic substances and determination of acetic acid 12.6.4.1 Principle Table 49 – Organic substances in photographic sets 12.6.4.2 Identification of acetic acid, ascorbic acid and citric acid 12.6.4.2.1 Standards and reagents 12.6.4.2.1.1 Standards Table 50 – Standards 12.6.4.2.1.2 Reagents Table 51 – Reagents 12.6.4.2.2 Apparatus 12.6.4.2.2.1 Graduated flasks, 100 ml and 1 000 ml 12.6.4.2.2.2 Pipettes 12.6.4.2.2.3 2-ml vials with crimp caps 12.6.4.2.2.4 Pasteur pipettes 12.6.4.2.2.5 Analytical balance, precision 0,1 mg 12.6.4.2.2.6 High performance liquid chromatography (HPLC) with UV-DAD-detector 12.6.4.2.3 Preparation of standards solutions 12.6.4.2.3.1 Stock standard solutions 12.6.4.2.3.2 Diluted standard solutions |
38 | 12.6.4.2.4 Sampling 12.6.4.2.5 Sample preparation 12.6.4.2.6 Procedure 12.6.4.2.7 Evaluation of results Table 52 – Sequence of elution Figure 5 – Chromatogram of organic acids |
39 | 12.6.4.3 Identification of N-(4-Hydroxyphenyl)glycine, N-Methyl-p-aminophenol and its salts and 1-Phenyl-pyrazolidin-3-one 12.6.4.3.1 Standards and reagents 12.6.4.3.1.1 Standards Table 53 – Standards 12.6.4.3.1.2 Reagents Table 54 – Reagents 12.6.4.3.2 Apparatus 12.6.4.3.2.1 Graduated flasks, 100 ml and 1 000 ml 12.6.4.3.2.2 Pipettes 12.6.4.3.2.3 2-ml vials with crimp caps 12.6.4.3.2.4 Pasteur pipettes 12.6.4.3.2.5 Analytical balance, precision 0,1 mg 12.6.4.3.2.6 Ultrasonic bath 12.6.4.3.2.7 High performance liquid chromatography (HPLC) with UV-DAD 12.6.4.3.3 Preparation of standard solutions 12.6.4.3.4 Sampling 12.6.4.3.5 Sample preparation 12.6.4.3.6 Procedure 12.6.4.3.7 Evaluation of results Table 55 – Sequence of elution |
40 | Figure 6 – Chromatogram of N-(4-hydroxyphenyl)glycine, N-methyl-p-amino-phenol and 1-phenyl-pyrazolidin-3-one 12.6.4.4 Determination of acetic acid 12.6.4.4.1 Standards and reagents 12.6.4.4.1.1 Standards Table 56 – Standards 12.6.4.4.1.2 Reagents Table 57 – Reagents 12.6.4.4.2 Apparatus 12.6.4.4.2.1 Graduated flasks, 100 ml and 1 000 ml 12.6.4.4.2.2 Pipettes 12.6.4.4.2.3 2-ml vials with crimp caps 12.6.4.4.2.4 Pasteur pipettes 12.6.4.4.2.5 Analytical balance, precision 0,1 mg 12.6.4.4.2.6 High performance liquid chromatography (HPLC) with UV-DAD detector 12.6.4.4.3 Preparation of standard solutions 12.6.4.4.3.1 Stock standard solution 12.6.4.4.3.2 Diluted standard solutions: |
41 | 12.6.4.4.4 Sampling 12.6.4.4.5 Sample preparation 12.6.4.4.6 Procedure 12.6.4.4.7 Evaluation of results 12.6.5 Gravimetric determination of the amount of certain organic substances (see Table 49) 12.6.5.1 Principle 12.6.5.2 Standards and reagents 12.6.5.3 Apparatus 12.6.5.3.1 Analytical balance, precision 0,1 mg 12.6.5.3.2 Crucible 12.6.5.3.3 Graduated cylinders, 100 ml and 200 ml 12.6.5.3.4 Desiccator 12.6.5.3.5 Oven, capable of maintaining a temperature of (105 ± 2) ˚C 12.6.5.4 Sampling 12.6.5.5 Sample preparation 12.6.5.6 Procedure 12.6.5.7 Evaluation of results 12.6.6 Test report a) type and identification of the product and/or material tested; b) a reference to this European Standard; c) the results of the qualitative tests: d) any deviation from the test procedure specified; e) date of test. |
42 | 12.7 Determination of organic solvents 12.7.1 General Table 58 – Solvents / identification |
43 | Table 59 – Solvents / determination a) Limits are based on the maximum allowable use of petroleum fractions. 12.7.2 Principle |
44 | 12.7.3 Standards and reagents 12.7.3.1 Standards Table 60 – Solvents a) The density values are those of the pure substance. b) The relevant petrol fractions are not commercially available; the closest match has been referenced. 12.7.3.2 Reagents Table 61 – Reagents 12.7.4 Apparatus 12.7.4.1 Analytical balance, precision 0,1 mg 12.7.4.2 Headspace vial, glass, 22 ml with crimp cap 12.7.4.3 Glass volumetric flask, 20 ml 12.7.4.4 Volumetric flask, 50 ml 12.7.4.5 Volumetric flask, 100 ml 12.7.4.6 General volumetric glassware 12.7.4.7 Variable positive displacement pipettes (range 0,02 ml to 10,00 ml) 12.7.4.8 Filter paper, general purpose laboratory, medium retention, medium/fast flow rate, pore size 11 µm 12.7.4.9 Syringe filter, nylon membrane, 0,45 µm 12.7.4.10 Syringe filter, surfactant-free cellulose acetate (SFCA) membrane, 0,45 µm 12.7.4.11 Headspace gas chromatograph with flame ionisation detector (HS-GC-FID) |
45 | 12.7.4.12 Gas chromatograph with mass spectrometer detector (GC-MS) 12.7.4.13 Gas chromatograph with flame ionisation detector (GC-FID) 12.7.5 Preparation of the standard solutions 12.7.5.1 Stock solutions for the identification and determination of solvents using HS-GC-FID |
46 | Table 62 – Organic solvents for analysis by HS-GC-FID 12.7.5.2 Stock solutions for the identification and determination of solvents using GC-MS Table 63 – Organic solvents for analysis by GC-MS 12.7.5.3 Stock solution for the identification and determination of propane-1,2-diol 12.7.5.4 Calibration solutions 12.7.5.4.1 Calibration solutions for the identification of solvents using HS-GC-FID Table 64 – Working solution 1 Table 65 – Working solution 2 Table 66 – Working solution 3 Table 67 – Working solution 4 |
47 | Table 68 – Working solution 5 12.7.5.4.2 Calibration solutions for the identification of solvents in aqueous-based materials 12.7.5.4.3 Calibration solutions for the identification of solvents in solvent-based materials 12.7.5.4.4 Calibration solutions for the identification of solvents in solvent-based materials Table 69 – Calibration solutions in saline for aqueous-based materials Table 70 – Calibration solutions in DMF for solvent-based materials Table 71 – Calibration solutions for the determination of solvents using HS-GC-FID |
48 | Table 72 – Calibration solutions in DMF or saline for hexane Table 73 – Calibration solutions in DMF for 1-methoxypropan-2-ol Table 74 – Calibration solutions in saline for 1-methoxypropan-2-ol, ethanol and propan-2-ol 12.7.5.4.5 Calibration solutions for the identification of solvents using GC-MS 12.7.5.4.6 Calibration solution for the determination of solvents using GC-MS |
49 | Table 75 – Calibration solutions for identification of solvents by GC-MS Table 76 – Calibration solutions for 2-(2-butoxyethoxy)ethyl acetate a) Assuming 1,000 g of sample is taken for analysis and the dilution in subclause 12.7.5.4.1, is applied. Table 77 – Calibration solutions for butyl glycolate a) Assuming 1,000 g of sample is taken for analysis and the dilution in subclause 12.7.5.4.1, is applied. Table 78 – Calibration solutions for (-caprolactam a) Assuming 1,000 g of sample is taken for analysis and the dilution in subclause 12.7.5.4.1, is applied. Table 79 – Calibration solutions for 2-methylpentane-2,4-diol a) Assuming 1,000 g of sample is taken for analysis and the dilution in subclause 12.7.5.4.1, is applied. |
50 | 12.7.5.4.7 Calibration solutions for the determination of propane-1,2-diol using GC-FID Table 80 – Calibration solutions for the determination of propane-1,2-diol by GC-FID a) Assuming 1,000 g of sample is taken for analysis and the dilution in subclause 12.7.5.4.1, is applied. 12.7.6 Sampling 12.7.7 Sample preparation 12.7.7.1 General 12.7.7.2 Sample preparation for identification and determination of solvents by HS-GC-FID 12.7.7.3 Sample preparation for identification of solvents by GC-MS 12.7.7.3.1 Solvent-based glue, thinner and paint samples 12.7.7.3.2 Aqueous-based glue samples 12.7.7.3.3 Aqueous-based paint samples 12.7.7.4 Sample preparation for determination of certain solvents by GC-MS |
51 | Table 81 – Dilution factors for the quantification of solvents by GC-MS and GC-FID 12.7.7.5 Sample preparation for determination of propane-1,2-diol using GC-FID 12.7.7.6 Sample preparation for determination of petrol fractions in aqueous-based paints and lacquers 12.7.7.7 Determination of petroleum fractions 12.7.8 Procedure 12.7.8.1 Identification of solvents using HS-GC-FID Table 82 – Typical retention times for solvents using the polar column (ZB-WAX) |
52 | Figure 7 – Chromatogram of a mixture of organic solvents by HS-GC-FID using a 60 m ° 0,32 mm ° 0,50 µm polar column (ZB-WAX) |
53 | Figure 8 – Chromatogram of a mixture of organic solvents by HS-GC-FID using a 60 m ° 0,32 mm ° 1,00 µm non-polar column ZB-1 Table 83 – Typical retention times for solvents using the non-polar column (ZB-1) |
54 | 12.7.8.2 Identification of solvents using GC-MS 12.7.8.3 Determination of solvent content by HS-GC-FID Table 84 – Typical retention times for certain solvents analysed by GC-MS Figure 9 – Chromatogram: Total ion chromatogram of a mixture of organic solvents by GC-MSD |
55 | 12.7.8.4 Determination of solvent content using GC-MS 12.7.8.5 Determination of propane-1,2-diol by GC-FID 12.7.8.6 Blank determination 12.7.8.6.1 HS-GS-FID blank determination 12.7.8.6.2 GS-MS and GC-FID blank determination 12.7.9 Evaluation of results 12.7.9.1 Calculation of solvent content by HS-GC-FID 12.7.9.2 Calculation of solvent content by GC-MS or GC-FID 12.7.9.3 Calculation of the petroleum fraction content 12.7.10 Test report a) type and identification of the product and/or material tested; b) a reference to this European Standard; |
56 | c) results of the tests recorded as: d) any deviation from the test procedure specified; e) date of test. 12.8 Combined approach for the determination of plasticizers in solvent-based adhesives and in solvent-based paints and lacquers, film forming agents in paints and lacquers and modifiers in solvent-based paints and lacquers 12.8.1 Principle 12.8.2 Determination of total extract 12.8.2.1 Standards and reagents 12.8.2.1.1 Standards 12.8.2.1.2 Reagents Table 85 – Reagents 12.8.2.2 Apparatus 12.8.2.2.1 Centrifuge, at least 1 900 g 12.8.2.2.2 Ultrasonic bath or shaker 12.8.2.2.3 Rotary evaporator 12.8.2.2.4 Oven, capable of maintaining a temperature of (110 ± 2) ˚C 12.8.2.2.5 Analytical balance, precision 0,1 mg 12.8.2.2.6 50-ml glass stoppered flat bottom flasks 12.8.2.2.7 General volumetric glassware 12.8.2.2.8 Desiccator chamber 12.8.2.2.9 Centrifuge tubes, min. 30 ml with caps 12.8.2.3 Sampling 12.8.2.4 Sample preparation 12.8.2.5 Procedure 12.8.2.6 Evaluation of results |
57 | 12.8.3 Identification of nitrocellulose 12.8.3.1 Principle 12.8.3.2 Reagents Table 86 – Reagents 12.8.3.3 Apparatus 12.8.3.3.1 Oven, capable of maintaining a temperature of (105 ± 2) ˚C 12.8.3.3.2 Press for making potassium bromide pellets 12.8.3.3.3 Fourier transform infrared spectrometer (FTIR-Spectrometer) with attenuated total reflectance (ATR) cell 12.8.3.4 Sampling 12.8.3.5 Sample preparation 12.8.3.6 Procedure 12.8.3.7 Evaluation of results Figure 10 – FTIR-spectrum of nitrocellulose in reflection mode |
58 | 12.8.4 Determination of plasticizers 12.8.4.1 Principle 12.8.4.2 Standards and reagents 12.8.4.3 Apparatus 12.8.4.4 Preparation of the standard solution 12.8.4.5 Procedure 12.8.4.6 Evaluation of results 12.8.5 Determination of film-forming agents 12.8.5.1 Principle 12.8.5.2 Standards and reagents 12.8.5.2.1 Standards Table 87 – Substances used for the identification and determination of film forming agents a) Luwax E is a trade name. 12.8.5.2.2 Reagents Table 88 – Reagents 12.8.5.3 Apparatus 12.8.5.3.1 General volumetric glassware 12.8.5.3.2 Analytical balance 12.8.5.3.3 Oven, capable of maintaining a temperature of (65 ± 2) ˚C 12.8.5.3.4 Gas chromatography with mass spectrometer detector (GC-MS) |
59 | 12.8.5.3.4.1 GC-conditions for substances 1 to 9 of Table 87 Figure 11 – Chromatogram of film-forming agent substances 1 to 9 12.8.5.3.4.2 GC-conditions for Luwax E |
60 | Table 89 – Mass numbers of the different substances for the SIM-modus Figure 12 – Chromatogram of film-forming agent Luwax E 12.8.5.4 Preparation of standard solutions 12.8.5.4.1 Stock solutions 12.8.5.4.2 Calibration solutions 12.8.5.4.2.1 Calibration solutions for substances 1 to 9 of Table 87 |
61 | Table 90 – Calibration solutions substances 1 to 9 of Table 87 12.8.5.4.2.2 Calibration solutions for substance 10 of Table 87 Table 91 – Calibration solutions Luwax E 12.8.5.4.3 Stability of the standard solutions 12.8.5.5 Sampling 12.8.5.6 Procedure 12.8.5.7 Evaluation of results |
62 | 12.8.6 Determination of the modifiers 12.8.7 Test report a) type and identification of the product and/or material tested; b) a reference to this European Standard; c) results of the tests recorded as: d) any deviation from the test procedure specified; e) date of test. |
64 | Table B.1 – Solvent content in different matrices and permitted maximum concentration |
65 | Table C.1 – Content of elements a) Calculated on the assumption that the composition of the mixtures or the double oxide is in a stoichiometric relation. b) For elements that are contained in more than 1 compound (as Fe and Zr) the highest amount is considered. |
67 | Table ZA.1 – Correspondence between this European Standard and EU Directives |
68 | Bibliography |