BS EN 14362-1-2012 禁用偶氮染料释放芳香胺欧盟测试方法(3)

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禁用偶氮染料释放芳香胺欧盟测试方法,替代原-1&-2方法。

BS EN 14362-1:2012

EN 14362-1:2012 (E)

Table 1 — Aromatic amines proscribed under Regulation REACH 1907/2006/Annex XVII

No.

CAS number

Index number

EC number

Substances

1 92-67-1 612-072-00-6 202-177-1 biphenyl-4-ylamine

4-aminobiphenyl xenylamine 2 92-87-5 612-042-00-2 202-199-1 benzidine

3 95-69-2 612-196-00-0 202-441-6 4-chloro-o-toluidine 4 91-59-8 612-022-00-3 202-080-4 2-naphthylamine 5a

97-56-3 611-006-00-3 202-591-2 o-aminoazotoluene

4-amino-2',3-dimethylazobenzene 4-o-tolylazo-o-toluidine 6a

99-55-8 612-210-00-5 202-765-8 5-nitro-o-toluidine

2-amino-4-nitrotoluene

7 106-47-8 612-137-00-9 203-401-0 4-chloroaniline

8 615-05-4 612-200-00-0 210-406-1 4-methoxy-m-phenylenediamine

2,4-diaminoanisole 9 101-77-9 612-051-00-1 202-974-4 4,4'-methylenedianiline

4,4'-diaminodiphenylmethane 10 91-94-1 612-068-00-4 202-109-0 3,3'-dichlorobenzidine

3,3'-dichlorobiphenyl-4,4'-ylenediamine 11 119-90-4 612-036-00-X 204-355-4 3,3'-dimethoxybenzidine

o-dianisidine 12 119-93-7 612-041-00-7 204-358-0 3,3'-dimethylbenzidine

4,4'-bi-o-toluidine 13 838-88-0 612-085-00-7 212-658-8 4,4'-methylenedi-o-toluidine

14 120-71-8 612-209-00-X 204-419-1 6-methoxy-m-toluidine

p-cresidine

15 101-14-4 612-078-00-9 202-918-9 4,4'-methylene-bis-(2-chloro-aniline)

2,2'-dichloro-4.4’-methylene-dianiline 16 101-80-4 612-199-00-7 202-977-0 4,4'-oxydianiline 17 139-65-1 612-198-00-1 205-370-9 4,4'-thiodianiline 18 95-53-4 612-091-00-X 202-429-0 o-toluidine

2-aminotoluene

19 95-80-7 612-099-00-3 202-453-1 4-methyl-m-phenylenediamine

2,4-toluylendiamine 2,4-diaminotoluene 20 137-17-7 612-197-00-6 205-282-0 2,4,5-trimethylaniline 21 90-04-0 612-035-00-4 201-963-1 o-anisidine

2-methoxyaniline 22b

60-09-3 611-008-00-4 200-453-6 4-aminoazobenzene

a The CAS-numbers 97-56-3 (No. 5) and 99-55-8 (No. 6) are further reduced to CAS-numbers 95-53-4 (No. 18) and

95-80-7 (No. 19).

b

Azo colorants that are able to form 4-aminoazobenzene, generate under the condition of this method aniline (CAS-number 62-53-3) and 1,4-phenylenediamine (CAS – number 106-50-3). Due to detection limits, only aniline may be detected. The presence of these colorants should be tested by EN 14362-3.

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禁用偶氮染料释放芳香胺欧盟测试方法,替代原-1&-2方法。

BS EN 14362-1:2012

EN 14362-1:2012 (E)

4 Principle

After selection of a coloured test specimen from the textile article, the test specimen is tested according to the method of colorant extraction for disperse dyes and/or the method of direct reduction for the other classes of dyes.

The application of the combined methods or one of the two methods is based on the nature of the fibre(s) of the test specimen (composed of pure fibre or of fibre blends) and the colour treatment (dyeing or printing process). When relevant, if the test specimen is not discoloured during the application of one of the two methods, the other one is carried out.

When the method of the colorant extraction for disperse dyes is carried out, the colorant is first extracted from the fibre in the headspace (see Figure 1) using chlorobenzene under reflux. The extract is concentrated and transferred to the reaction vessel with methanol for subsequent reduction with sodium dithionite in a citrate-buffered aqueous solution (pH = 6) at 70 °C. If the textile specimen is not completely discoloured after chlorobenzene extraction, the specimen is added to the reaction vessel with the methanolic solution of the dispersed dye for combined reduction.

When the method for the other classes of the dyes is carried out, the test specimen is treated with sodium dithionite in a citrate-buffered aqueous solution (pH = 6) at 70 °C in a closed vessel.

After the reduction, any amine released in the process is transferred to a t-butyl methyl ether phase by means of liquid-liquid extraction using diatomaceous earth columns. The t-butyl methyl ether extract is then concentrated, and the residue is taken up in a solvent appropriate for detection and determination of the amines using chromatography (see Annex A).

A screening method, using liquid/liquid extraction without diatomaceous earth columns, is described in Annex E.

If any amine is detected by one chromatographic method, then confirmation shall be made using one or more alternative methods.

5 Safety precautions

5.1 WARNING — The substances [amines] listed in Clause 3 are classified as substances known to be or suspected of being human carcinogens.

Any handling and disposal of these substances shall be in strict accordance with the appropriate national health and safety regulations.

5.2 It is the user’s responsibility to use safe and proper techniques in handling materials in this test method. Consult manufacturers for specific details such as material safety data sheets and other recommendations. 5.3 Good laboratory practice should be followed. Wear safety glasses in all laboratory areas and a single-use dust respirator while handling powder colorants. 5.4

Users should comply with any national and local safety regulations.

6 Reagents

Unless otherwise specified, analytical grade chemicals shall be used. 6.1 Chlorobenzene. 6.2 Acetonitrile. 6.3 Methanol.

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禁用偶氮染料释放芳香胺欧盟测试方法,替代原-1&-2方法。

BS EN 14362-1:2012

EN 14362-1:2012 (E)

6.4 t-butyl methyl ether. 6.5 n-pentane.

6.6 Citrate/sodium hydroxide buffer solution, pH = 6, c = 0,06 mol/l1).

6.7

Aqueous sodium dithionite solution, ρ = 200 mg/ml2) freshly (daily) prepared.

6.8 Diatomaceous earth.

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