Analysis of commercial Acid Black 194 and related dyes by micellar electrokinetic chromatography

• Published in: Dyes and pigments 2012-08, Vol.94 (2), p.258-265
• Main Authors: Sebastiano, Roberto, Contiello, Nunzia, Senatore, Stanislao, Righetti, Pier Giorgio, Citterio, Attilio
• Format: Article
• Language: English
• Subjects: Acid Black analysis; Acid Brown analysis; Capillarity; Chromatography; Dyes; Electrokinetics; Electrophoresis; Impurities; Mathematical analysis; Metal complexes; Micellar capillary electrophoresis; REACH legislation; Standard deviation; Textile dyes
• ISSN: 0143-7208; 1873-3743
• DOI: 10.1016/j.dyepig.2011.12.014

The commercial dye C.I. Acid Black 194 was analyzed by reversed-phase HPLC, Capillary Zone Electrophoresis and Micellar ElectroKinetic Chromatography under different operative conditions, with the scope to detect the impurity distribution typical of any production processes and synthetic batch. The three chrome(III) complexes deriving from the industrial synthesis of C.I. Acid Black 194, and one of the main impurities were isolated by silica flash chromatography and identified by mass spectrometry and NMR. More than twelve compounds present in the commercial mixture, but undetectable by the analytical protocols known in literature, were fully separated by the MECK mode capillary electrophoresis with low % Relative Standard Deviation of the main electrophoretic parameters. Two of them were identified by isolation from the commercial mixture. As additional examples two other commercial metal-based dyes, C.I. Acid Brown 432 and C.I. Acid Brown 434, were analyzed by the same protocol with very good results. ► Analysis of metal dyes impurities are indispensable because of REACH legislation. ► HPLC and CE-MS protocols known are often not oriented on dyes impurities analysis. ► MECK mode shows to be powerful and stable method for metal dyes analysis. ► MECK mode allows detect impurity distribution typical of any dyes synthetic batch.