Supercritical fluid chromatography and two-dimensional supercritical fluid chromatography of polar car lubricant additives with neat CO2 as mobile phase

Lavison, Gwenaelle; Bertoncini, Fabrice; Thiébaut, Didier; Beziau, Jean-François; Carrazé, Bernadette; Valette, Pascale; Duteurtre, X.

doi:10.1016/j.chroma.2007.05.068

Cited by 19 publications

(12 citation statements)

References 29 publications

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“…The composition study of formulated lubricant is currently a long and complex process involving several characterization techniques such as mass spectrometry, nuclear magnetic resonance, infrared spectroscopy as well as separation technique such as liquid or gas chromatography . Indeed, formulated lubricants are complex mixtures composed of base oil(s) and numerous molecular or polymeric additives with different function (detergents, corrosion inhibiter, antioxidant, viscosity modifiers, etc.)…”

Section: Introductionmentioning

confidence: 80%

Rapid analysis of lubricants by atmospheric solid analysis probe–ion mobility mass spectrometry

et al. 2014

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Formulated lubricants are complex mixtures composed of base oil(s) and additives with various functions (detergents, corrosion inhibiter, antioxidant, viscosity modifiers, etc.). Because of the aliphatic nature of base oil and the chemical diversity of additives, the characterization of lubricant is currently a long and complex process. The comprehensive analysis of lubricant samples involves several techniques such as nuclear magnetic resonance, mass spectrometry, chromatography and infrared spectroscopy. The coupling of atmospheric solid analysis probe (ASAP) with ion mobility-mass spectrometry (IM-MS) has been shown to be an efficient tool for the characterization of complex mixture containing vaporizable polar to non-polar compounds. This approach affords the coupling of a direct ionization technique that does not require sample preparation, with a bi-dimensional separation method with high peak capacity. In this work, we show that ASAP-IM-MS is a suitable method for rapid and direct characterization of lubricant samples. Indeed, base oil and additives yielded, by ASAP, ions series which could be separated by IM-MS. Molecular additives such as Zn-dithiocarbamate, phosphite, thiophosphate and Alkyl diphenylamine were ionized as molecular ions [M](+•) or protonated molecules [M + H](+), depending of their polarity. In some cases, fragment ions were observed, confirming the additive identification. In addition, high molecular weight polymeric additives such as poly(alkyl methacrylate) (PAM) were pyrolized in the ASAP source leading to characteristic fragment ions. ASAP-IM-MS is shown to be a powerful tool for studying complex mixtures, allowing the first comprehensive analysis of lubricants in just a few minutes.

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Section: Introductionmentioning

confidence: 80%

Rapid analysis of lubricants by atmospheric solid analysis probe–ion mobility mass spectrometry

et al. 2014

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“…The column was placed in the HP5890 oven. Detection was carried out with both a FID and a multi‐wavelength photodiode array detector (DAD) HP 1050 (acquisition frequency 20 Hz, 1.7 μL cell volume); for dual FID/UV detection, the column effluent was split via a T‐piece placed in the oven between the column outlet and the UV detector 10. The T‐piece was connected both to a laboratory made integral restrictor (50 μm id deactivated fused silica capillary tubing from S.G.E., Villeneuve St. Georges, France) for transferring ca.…”

Section: Methodsmentioning

confidence: 99%

“…For the same reasons as in HTLC, SFC enables better kinetics and shorter analysis times (3–10 times shorter) than LC, whereas the pressure drop is several times lower than in LC. Since its commercial development in the 1990s, SFC has demonstrated that separations could be performed as fast as in UHPLC using neat carbon dioxide for the separation of hydrocarbons or medium polarity species 9, 10 or modified carbon dioxide for a wide range of applications, including fast chiral separations in analytical or preparative scale 11. Indeed, very high speed separations using sub‐2 μm particles were demonstrated recently by Berger in SFC with CO 2 – polar modifier mobile phase 12.…”

Section: Introductionmentioning

confidence: 99%

“…ASTM method has been issued for group‐type analysis of hydrocarbons 13, and SFC is a complementary technique to gas chromatography (GC) for simulated distillation 9. The main drawback of SFC using neat carbon dioxide as the mobile phase lies in its lack of solubility for polar compounds despite the fact that well‐protected stationary phases showing very low silanol activity can allow elution of medium polarity compounds without polar modifiers 10.…”

Section: Introductionmentioning

confidence: 99%

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Feasibility of ultra high performance supercritical neat carbon dioxide chromatography at conventional pressures

Sarazin

Thiébaut

Sassiat

et al. 2011

J of Separation Science

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The implementation of columns packed with sub-2 μm particles in supercritical fluid chromatography (SFC) is described using neat carbon dioxide as the mobile phase. A conventional supercritical fluid chromatograph was slightly modified to reduce extra column band broadening. Performances of a column packed with 1.8 μm C18-bonded silica particles in SFC using neat carbon dioxide as the mobile phase were compared with results obtained in ultra high performance liquid chromatography (UHPLC) using a dedicated chromatograph. As expected and usual in SFC, higher linear velocities than in UHPLC must be applied in order to reach optimal efficiency owing to higher diffusion coefficient of solutes in the mobile phase; similar numbers of theoretical plates were obtained with both techniques. Very fast separations of hydrocarbons are presented using two different alkyl-bonded silica columns.

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“…Instead, when reliable quantitative results are required chromatographic methods after extraction of stabilizers from a polymeric sample play a dominant role. Besides the application of gas chromatography (GC), pyrolysis GC and supercritical fluid chromatography (SFC), high‐performance liquid chromatography (HPLC) is commonly applied for the separation and quantification of additives. These chromatographic methods suffer from several disadvantages: the use of GC is confined to a limited number of additives, as normally stabilizers with low volatility are employed to avoid physical loss from the polymer.…”

mentioning

confidence: 99%

High‐throughput quantification of stabilizers in polymeric materials by flow injection tandem mass spectrometry

Beißmann

Reisinger

Reimann

et al. 2014

Rapid Comm Mass Spectrometry

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Supercritical fluid chromatography and two-dimensional supercritical fluid chromatography of polar car lubricant additives with neat CO2 as mobile phase

Cited by 19 publications

References 29 publications

Rapid analysis of lubricants by atmospheric solid analysis probe–ion mobility mass spectrometry

Rapid analysis of lubricants by atmospheric solid analysis probe–ion mobility mass spectrometry

Feasibility of ultra high performance supercritical neat carbon dioxide chromatography at conventional pressures

High‐throughput quantification of stabilizers in polymeric materials by flow injection tandem mass spectrometry

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