Quantitation method of N ,N ′-disalicylidene-1,2-propanediamine by comprehensive two-dimensional gas chromatography coupled to a nitrogen chemiluminescence detector

Abstract

Metal deactivator additives (MDAs) have been used for over 60 years to prevent metal catalyzed reactions in petroleum products; a commonly used metal deactivator is N,N'-disalicylidene-1,2-propanediamine. The quantitation of low MDA concentrations in fuels is challenging due to the complexity of the sample matrix. In this work, this difficulty was overcome using GC × GC hyphenated with a nitrogen chemiluminescence detector. The high resolution power of GC × GC avoided co-elution between the MDA and other sample matrix compounds; while the enhanced sensitivity of GC × GC and the use of a nitrogen chemiluminescence detector supplied a high sensitivity and specificity for nitrogen compounds. For the analysis, the MDA additive was derivatized with the silylation agent N,O-bis (trimethylsilyl)trifluoroacetamide at room temperature and its quantitation was based on an external calibration curve; good linear response was obtained in the 1.4-8.6 ppm range.

Characterization of Organic Nitrogen Compounds and Their Impact on the Stability of Marginally Stable Diesel Fuels

“…Current multidimensional chromatography (GCxGC) methods provide compositional maps based on polarity, using columns with orthogonal column chemistries that offer a more comprehensive means to isolate fuel constituents on the basis of polarity, without the losses inherent in liquid–liquid extraction procedures. Although it is possible to analyze nitrogen-containing compounds with GCxGC-MS, the low concentrations of those compounds in fuels, as well as the complex sample matrix, make identifications difficult. , A nitrogen detector such as an NPD or an NCD can be utilized with gas chromatography to characterize the organonitrogen compounds in fuels . In this work, an optimized liquid extraction procedure, similar to that used in the 1982 study, was used to separate BNC and NBNC fractions from marginally unstable fuels.…”

“…16,17 A nitrogen detector such as an NPD or an NCD can be utilized with gas chromatography to characterize the organonitrogen compounds in fuels. 18 In this work, an optimized liquid extraction procedure, similar to that used in the 1982 study, was used to separate BNC and NBNC fractions from marginally unstable fuels. These fractions were then analyzed by GC−MS and GC-nitrogen− phosphorous detection (NPD).…”

Inlet backflushing device for the improvement of comprehensive two dimensional gas chromatographic separations

“…GC × GC is considered an established separation technique and for the last decade focus has shifted away from the development of modulation technology to applying the technique to an ever increasing number of analytical challenges. Fields in which GC × GC applications are popular include petroleum and petrochemicals [6][7][8][9][10][11][12][13][14][15][16]; food, flavours and fragrances [17][18][19][20][21][22][23][24][25][26][27][28][29][30]; metabolomics [31][32][33][34][35][36][37][38][39][40][41][42] and environmental analysis [43][44][45][46][47][48][49]. Although GC × GC has never been more widespread, there are some applications that remain challenging for a chromatographer to perfect.…”

Quantification of nitrogen compounds in diesel fuel samples by comprehensive two-dimensional gas chromatography coupled with quadrupole mass spectrometry

“…For this reason, an orthogonal 2D system (GC × GC) can be utilized to quantify N‐compounds without using fractionation steps due to the broadly disseminated advantages of the technique .…”