Abstract
The advances in nebulizer technology of the evaporative light scattering detector (ELSD) for high temperature gel permeation chromatography (GPC) allowing lower operation temperatures, overcome the limitations of the differential refractive index (DRI) and infrared (IR) detectors, thus allowing xylene as solvent for evaluation of the molecular weight distributions (MWD) of polyolefins. Different types of polyolefins, previously characterized by GPC in trichlorobenzene (TCB) with a DRI detector, in an interlaboratory study conducted by International Union of Pure and Applied Chemistry (IUPAC) (Luruli, Phase 1: IUPAC SEC/GPC round robin project report: repeatability and reproducibility of sample preparation and analysis in high-temperature SEC, http://media.iupac.org/projects/2005/2005-011-3-400_rpt-phase1_110510.pdf, 2010), and also in a recent study by GPC in TCB with an ELSD and DRI (Boborodea and O’Donohue, Int J Polym Anal Charact 22:631–638, 2017), were for the first time analyzed by GPC with ELSD in xylene. In this solvent, the power exponent, governing the non-linear correlation between the ELSD signal and concentration, was found to be 1.40. After linearization of the ELSD signal, the measured average molecular weights of polyolefins in xylene were in good agreement with the values given by DRI detector in TCB.
Graphical abstract
The molecular weight distributions obtained in xylene with an evaporative light scattering detector are similar with those evaluated by classical GPC with differential refractive index detector in TCB.
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References
Luruli N (2010) Phase 1: IUPAC SEC/GPC round robin project report: repeatability and reproducibility of sample preparation and analysis in high-temperature SEC. http://media.iupac.org/projects/2005/2005-011-3-400_rpt-phase1_110510.pdf. Accessed 26 Aug 2017
Boborodea A, O’Donohue S (2017) New evaporative light scattering detector for high temperature gel permeation chromatography. Int J Polym Anal Charact 22:631–638
ASTM D 6474-12 (2012) Standard test method for determining molecular weight distribution and molecular weight averages of polyolefins by high temperature gel permeation. ASTM International, Subcommittee: D20.70
Commission Regulation (EC) No. 552/2009 of 22 June 2009 (2009) Amending regulation (EC) No 1907/2006 of the European Parliament and of the Council on the Registration, Evaluation, Authorization and Restriction of Chemicals (REACH) as regards Annex XVII. Off J Eur Union L 164:7–31
Wild L, Ranagath R, Ryle T (1971) Structural evaluation of branched polyethylene by combined use of GPC and gradient-elution fractionation. J. Polym. Sci. A2 9:2137–2150
Holtrup W (1977) Zur Fraktionierung von Polymeren durch Direktextraktion. Makromol Chem 178:2335–2349
Goede E, Mallon P, Pasch H (2010) Fractionation and analysis of an impact poly(propylene) copolymer by TREF and SEC-FTIR. Macromol Mater Eng 295:366–373
Boborodea A, Mirabella FM (2014) Elution temperatures of polyethylene copolymers in temperature rising elution fractionation (TREF): comparison in xylene and trichlorobenzene diluents. Int J Polym Anal Charact 19:468–473
Boborodea A, O’Donohue S (2017) Linearization of evaporative light scattering detector signal. Int J Polym Anal Charact. http://www.tandfonline.com/doi/abs/10.1080/1023666X.2017.1367066. Accessed 26 Aug 2017
Agilent Application Note 5990-8425EN (2011) Polystyrene and polyethylene calibrants in gel permeation chromatography with TCB. http://cn.agilent.com/cs/library/technicaloverviews/public/5990-8425EN.pdf. Accessed 26 Aug 2017
Marcus Y (1999) The properties of solvents. Wiley series in solution chemistry, vol 4. Wiley, Chichester
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Boborodea, A., Mirabella, F.M. & O’Donohue, S. Polyolefin Characterization in Xylene by High-Temperature Gel Permeation Chromatography with a New Evaporative Light Scattering Detector. Chromatographia 81, 419–424 (2018). https://doi.org/10.1007/s10337-018-3481-9
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DOI: https://doi.org/10.1007/s10337-018-3481-9