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- Long, A J, et al.
(författare)
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Detection of banned amines in leather
- 2005
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Ingår i: Leather International. - 1473-6314. ; 207:4, s. 79-82
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Tidskriftsartikel (refereegranskat)abstract
- There currently exists legislation within Europe banning the use of dyestuffs based on certain carcinogenic amine compounds. Currently a test method exists that is used by the industry (CEN ISO TS 17234 based on DIN 53316). This is able to detect twenty of the compounds listed by the legislation but is not validated for the recently added 2-methoxyaniline and is unsuitable for analysis of -Aminoazobenzene. The method is also known to have problems related to the reproducibility of the analysis both within and between laboratories. Work has been carried out as part of a European Commission funded project to look into the issues surrounding the test method. Within the project there are three key objectives. These are: * To carry out a feasibility study for the development of a certified reference material for banned azo dyes in leather * To develop a method suitable for certifying any proposed reference material * To develop a method suitable for routine testing in industry. Research to develop a method for certifying the reference material has resulted in a procedure based on supercritical fluid extraction for degreasing the leather, followed by sodium dithionite microwave assisted extraction in order to reduce the dyestuffs present. The samples obtained are then cleaned up using solid phase extraction before analysis using High Performance Liquid Chromatography with Diode Array Detection (HPLC-DAD). The technique of standard addition is also used to improve recovery rates. In order to certify a reference material it is necessary to have a method which is very accurate and precise. The method is not planned for general use and, therefore, has incorporated techniques that may not be suitable for all laboratories. A routine test method has also been developed. This method was designed considering that it should be suitable for use in laboratories within the leather industry on a routine basis. It should be relatively straight forward to carry out, providing results with good reproducibility. It is not critical, however, to obtain 100% recovery rates, provided the results are consistent. Also of importance is the cost effectiveness of the method along with the speed in which results can be obtained. A method has been developed incorporating ultrasound based degreasing that can be carried out on the day of analysis. This is followed by an optimised sodium dithionite reduction and solid phase extraction for clean-up. Both HPLC-DAD and Gas Chromatography with Mass Spectroscopy (GCMS) have been evaluated for analysis. During development the methods have been assessed in inter-laboratory trials.
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