BS EN 14362-1-2012 禁用偶氮染料释放芳香胺欧盟测试方法(15)

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)

9.4 Separation and concentration of the amines

Add, to the reaction solution, 0,2 ml of the NaOH solution (6.11) and shake vigorously. Transfer the reaction solution to the diatomaceous earth column (7.5) and allow to be absorbed by the column for 15 min.

Meanwhile add 10 ml t-butyl methyl ether in the reaction vessel, shake vigorously and after the 15 min period the t-butylmethyl ether is decanted with the fibres onto the top of the column and the eluate is collected in a 100 ml round-bottom flask with standard ground joint or in a glass vessel for an evaporation apparatus (7.6). The reaction vessel is rinsed with 10 ml t-butylmethyl ether and the solvent is transferred to the column. Subsequently, 60 ml t-butyl methyl ether is poured directly on the column.

For amine detection and quantification, the t-butyl methyl ether extract is concentrated to about 1 ml (not to dryness!) at not more than 50 °C. If necessary, to exchange to another solvent, remove the remainder of the solvent very carefully by means of a weak flow of inert gas.

NOTE 1 Removal of the solvent (concentration in the rotary vacuum evaporator, evaporation to dryness) may lead to substantial amine losses if performed under uncontrolled conditions.

The extract or residue are immediately taken up to 2,0 ml of an appropriate solvent, e.g. acetonitrile or t-butyl methyl ether, and analysed without delay. If the complete analysis cannot be performed within 24 h, keep the extract below -18 °C.

NOTE 2 Owing to the matrix, individual amines, such as 2,4-diaminotoluene and 2,4-diaminoanisole are likely to exhibit a very poor stability. Where delays occur in the work routine, amines may be no longer detectable by the time of instrumental measurement.

9.5 Amine detection and quantification

Amine detection can be performed using the chromatographic techniques listed (7.8). Other validated methods may be used. If any amine is detected by one chromatographic method, then confirmation shall be made using one or more alternative methods. The result is positive only if both methods give a positive result. If any of the amines listed in Table 1 is identified, then at least a three point calibration curve is built up to quantify amine content.

NOTE

If the identified amines have isomers, care should be taken about the correct identification.

9.6 Check procedure

9.6.1 General

To check the procedure, 100 µl of the amine stock solution (6.10.1) (or a volume to give 30 µg of each amine in the reaction vessel) and 2,0 ml methanol are added to a reaction vessel (7.3) containing 15 ml of the preheated citrate/sodium hydroxide buffer solution (6.6). This check procedure shall be carried out with each batch of samples.

Then the procedure set out in 9.4 and 9.5 is carried out. Quantify this check standard based on the daily calibration (6.10.2).

9.6.2 Calibration using internal standard (quantification performed by gas chromatography)

ρS=ρc ×

where

As×AISC Vs

×

A c ×AISSV

ρs

concentration of the amine in the sample solution in µg/ml;

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