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Selection of Internal Standard for Quantitative Analysis of Extraction of Benzene from Cyclohexane with N,N-Dimethylformamide/Potassium Thiocyanate Complex Solvent

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Abstract

The use of novel complex solvents in liquid–liquid extraction of aromatic hydrocarbons has become an important aim in the petrochemical industry. Phase equilibrium data are necessary for the design, evaluation, and optimization of extraction processes that are based on phase equilibria. To detect the separation effect of benzene/cyclohexane mixtures accurately and obtain the phase equilibrium data, a fast and efficient liquid–liquid extraction method combined with internal-standard gas chromatography was established for the quantitative analysis of the extraction of benzene from cyclohexane with the N,N-dimethylformamide/potassium thiocyanate (DMF/KSCN) novel complex solvent. The phase separation phenomenon occurred in a quaternary (benzene/cyclohexane/DMF/KSCN) system. KSCN as a cosolvent to improve the selectivity of DMF was innovatively applied and there was no prior report of any quantitative analysis of this system. After repeated experiments, n-butyl alcohol was found to be a suitable internal standard. The proposed method exhibits good linearity with a coefficient of correlation ranging from 0.9982 to 0.9994. The limits of detection varied from 0.16 to 0.58 mg L−1. The recovery was from 90.91 to 109.44 %. The method achieved excellent reproducibility with interassay relative standard deviations of 1.9–7.1 %. Furthermore the accuracy and precision of the proposed method with DMF/KSCN as the extractant were compared with the same method with only DMF as the extractant. The results indicated that adding KSCN had no significant impact on this quantitative method, although the KSCN could not be detected by gas chromatography (the mass fraction of KSCN was calculated via mass balance). Liquid–liquid equilibrium data obtained from this proposed method also revealed that the DMF/KSCN complex solvent had a higher selectivity for benzene than that of only DMF. This method is suitable for routine quantification of benzene, cyclohexane, DMF, and KSCN with high precision and accuracy.

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Acknowledgments

This work was supported by the National Natural Science Foundation of China (20976032, 21076049), Fundamental Research Funds for the Central Universities (HEUCFZ1018), and Natural Science Foundation of Heilongjiang Province (E-200808).

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Authors and Affiliations

  1. The College of Materials Science and Chemical Engineering, Harbin Engineering University, Harbin, 150001, People’s Republic of China

    Sha Song

  2. Jinzhou Design Institute, Petro China Northeast Refining and Chemicals Engineering Co. Ltd., Jinzhou, 121000, People’s Republic of China

    Chunguang Lin & Na You

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  1. Sha Song
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  2. Chunguang Lin
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  3. Na You
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Correspondence to Sha Song.

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Song, S., Lin, C. & You, N. Selection of Internal Standard for Quantitative Analysis of Extraction of Benzene from Cyclohexane with N,N-Dimethylformamide/Potassium Thiocyanate Complex Solvent. Chromatographia 77, 159–164 (2014). https://doi.org/10.1007/s10337-013-2593-5

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  • DOI: https://doi.org/10.1007/s10337-013-2593-5

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