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Journal of Thermal Analysis and Calorimetry

, Volume 112, Issue 1, pp 293–300 | Cite as

Combining zone melting and preparative chromatography to purify Phenanthrene

  • Nicolas Couvrat
  • Antoine Burel
  • Séverine Tisse
  • Yohann Cartigny
  • Gérard Coquerel
Article

Abstract

The impacts of zone melting and preparative chromatography on Phenanthrene purity were established by GC and DSC experiments. On the one hand, phase diagrams investigations between Phenanthrene and its major impurities (Dibenzothiophene, Fluorene, Carbazole, and Anthracene) have revealed inadequate heterogeneous equilibria for an efficient purification by zone melting, especially for Fluorene. Nevertheless, a clear purification effect has been noticed by applying this thermal process. On the other hand, preparative chromatography has shown a propensity to separate Phenanthrene from Fluorene. This uncommon case demonstrates the advantages of combining purification techniques to reach a sufficient purity level. Moreover, this study highlights the limitations of analytical tools to quantify such high level of purity.

Keywords

Zone melting Preparative chromatography Chemical purity Phenanthrene Solid–solid transition DSC analyses 

Abbreviations

HPLC

High performance liquid chromatography

P-HPLC

Preparative HPLC

GC

Gas chromatography

LOQ

Limit of quantification

NQ

Not quantifiable

MS

Mass spectroscopy

DSC

Differential scanning calorimetry

LT

Low temperature

HT

High temperature

R-P

Raw Phenanthrene

ZM-P

Zone melted Phenanthrene

TP-P

Twice purified Phenanthrene

Supplementary material

10973_2012_2746_MOESM1_ESM.doc (292 kb)
Supplementary material 1 (DOC 292 kb)

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Copyright information

© Akadémiai Kiadó, Budapest, Hungary 2012

Authors and Affiliations

  • Nicolas Couvrat
    • 1
  • Antoine Burel
    • 1
  • Séverine Tisse
    • 1
  • Yohann Cartigny
    • 1
  • Gérard Coquerel
    • 1
  1. 1.Laboratoire SMSUniversité de RouenMont Saint AignanFrance

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