14 Analytical Instrumentation ASTM D5186 Results
The chromatograms of gasoline and jet fuel under the ASTM D5186 method conditions are shown in Figure 10 and Figure 11. The gasoline was determined to have 59.3% non-aromatics and 40.7% aromatics, while the jet fuel had 81.5% non-aromatics and 18.5% aromatics.
The chromatogram (fi gure 12) of the non-aromatic hydrocarbon standard mixture is shown below. Besides C5-
C9 C9 .
which co-eluted, all of the hydrocarbons were successfully separated and identifi ed. As
the BP Calibration standard was diluted in hexane in order to have the FID signal on scale, the strong hexane signal likely contributed to the co-elution of C5-
Figure 12: Chromatogram of the BP Calibration standard mixture of hydrocarbons (diluted in hexane before injection). The mixture contained C5-
C10 Figure 10: ASTM D5186 Analysis of Commercially Available Gasoline. Non-aromatic 59.3% and aromatic 40.7%. Conclusion
The pore size is a signifi cant factor in the separation effi ciency of the column for the separation of alkanes and aromatics. The JASCO 30A packing material provided the best resolution of hexadecane, cyclohexane and toluene with the Princeton 30A a very close 2nd providing equal resolution of hexadecane and cyclohexane, but less resolution of 5.4 compared to 7.7 on the JASCO silica.
The temperature and pressure studies have not only illustrated how the unique parameter of back pressure plays a signifi cant role in retention time, but also how it can be utilised to optimise a separation when resolution is minimal. Both alkanes and aromatics were more retained at higher pressures, but higher temperatures had the opposite effect on retention and also led to peak broadening. These signifi cant effects from back pressure and temperature provide a user the ability to tune a separation depending on to which class of compounds they are looking to maximise the resolution.
As the results show in the repeatability and reproducibility tables, the SFC-FID exceeds the requirements of the ASTM D6550. Having exceeded the acceptable values, the SFC-FID system can successfully be used for the automated analysis of olefi ns in gasoline. The ASTM D5186 method was used to successfully analyse commercially available gasoline and jet fuel.
Figure 11: ASTM D5186 Analysis of Jet Fuel. Non-aromatic 81.5% and aromatic 18.5%.
The SFC-FID system offers versatility for high resolution separations of hydrocarbons in a signifi cantly shorter analysis time than provided by GC.
Author Contact Details DJ Tognarelli, JASCO Inc • 28600 Mary’s Court, Easton, MD, 21601, USA. • Tel: 1-410-822-1220 • Email:
dtognarelli@jascoinc.com • Web:
www.jascoinc.com
, C12 , C14- C18 , C20 , C24 , C28 , C32 , C36 , and C40
, all of which were identifi ed.
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i-Fischer®
DIST D-2892 CC Fully Computer Controlled Distil lation System acc. to ASTM D2892 (TBP)
Pyrolysis-GC×GC- QTOF for the Improved Characterisation of Crude Oil
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Pyrolysis coupled to comprehensive two-dimensional gas chromatography-mass spectrometry (py-GC×GC-MS) is a very powerful technique for the characterisation of complex, heavy matrices such as crude oils. In the application note the py- GC×GC-MS method was applied to 3 samples from different origins and with differing density and sulphur content.
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The results substantiated that two-dimensional resolution provides enhanced separation of the pyrolysis products, leading to improved classifi cation for groups and individual analytes. Additionally, the 2D pyrograms make sample comparison easier and more informative. In spite of the enhanced separation power offered by GC×GC, complexity is such that complete resolution is often not possible. The use of High Resolution Mass Spectrometry (HRMS) can deliver extra selectivity and identifi cation power, especially for compounds with heteroatoms (e.g. N, S, O).
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