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BS EN 71-5:1993+A2:2009

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Safety of toys – Chemical toys (sets) other than experimental sets

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BSI 2009 72
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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
BS EN 71-5:1993+A2:2009
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