Syncrude manifest a great complexity in their chemical nature. Although containing a limited number of chemical classes, these matrices consist of a plethora of individual compounds within these classes. The vast development and improvement of multi-dimensional gas chromatograph methods (GC×GC) over the past years, has allowed for a more than suffice characterization for end products such as middle distillates obtained from classical refinery processes. Even though this method has proven to be very robust the transfer of this methodology for higher distillation cuts, process residues and process intermediates like syncrudes has proven to be quite challenging. Over the last two years two new technologies emerged and have been proven to be a reasonable and complementary progression for the exploration of very complex matrices in conjunction with GC×GC. Firstly, the nowadays standard detection for GC×GC, namely time-of-flight mass spectrometry, has developed further combining now very fast acquisition frequencies (200hz) with accurate ( < 2ppm) and high resolution (25.000) mass information. With this hyphenation it is now possible to obtain isomeric information's from GC×GC and high resolution mass information with one instrumentation. The information space of both techniques could be combined. Hereby, e.g. Kendrick mass defect plots or rings and double binding equivalents plots could be either extended by quantitative information (number of isomers) or directly combined with chromatographic informations to build up a three dimensional information spaces. Beside mass spectrometry also UV absorption spectroscopy has further developed. UV absorption has been reported only sporadically in combination with GC or GC×GC for the investigation of petrochemical matrices. Especially the pure sensitivity and non-specific spectral information are main obstacles. New V(acuum)UV-technology in combination with GC or even GCxGC overcomes both limitations and makes VUV spectrometry accessible for lab and routine applications. The extension to wavelength down to 125 nm allows now very sensitive detections with up to three magnitude higher cross sections compared to the usually accessible wavelength of 250nm. In addition most small organic compounds exhibit very characteristic VUV absorption spectra while their conventional UV spectra is very uniform and not very distinct. We will introduce both techniques in combination with GC×GC for the analysis of syncrude obtained from a laboratory scale iron catalysed FT reactor working on low and high temperature conditions.