Metrics of separation in chromatography

Blumberg, Leonid M.; Klee, Matthew S.

doi:10.1016/s0021-9673(01)01256-0

Cited by 47 publications

(40 citation statements)

References 20 publications

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“…We, therefore, expected SN and n to decrease with decreasing column length and with increasing heating rate, although the decrease in efficiency was not directly proportional to the reduction in column length ( Table 3). The average peak widths of the Grob test components ranged from 4.76 s for PEG 20 M stationary phase in C-GC to 0.100 s for OV 1701 in UFM-GC in agreement with the values reported by Blumberg and Klee [17] and Magni et al [5]. In general, column length and inner diameter and temperature rate characterising each GC approach condition column performance while, separation parameters were comparable within each approach independently of the stationary phase.…”

Section: Column Evaluationsupporting

confidence: 87%

“…They will be evaluated on the basis of the separation measure, S, the universal parameter recently introduced by Blumberg and Klee [17] to evaluate the metric of separation in chromatography.…”

Section: Discussionmentioning

confidence: 99%

“…The Lan and Jorgenson algorithm was here adopted to calculate n because it overcomes some of the limits of the equation previously reported for instance by Giddings and Gruskha [13][14][15]. These parameters have been considered because they are the most widely used in spite of their limits, in particular their incompatibility and lack of additivity, which were recently discussed in depth by Blumberg and Klee [17]. Grob test and separation parameters were used to evaluate how column performance differed at different GC speeds and whether the loss of column efficiency under UFM-GC conditions is compatible with reliable analyses of essential oils of differing complexities while maintaining the dramatic gain in analysis time with UFM-GC.…”

Section: Column Evaluationmentioning

confidence: 99%

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Direct resistively heated column gas chromatography (Ultrafast module-GC) for high-speed analysis of essential oils of differing complexities

Bicchi

Brunelli

Cordero

et al. 2004

Journal of Chromatography A

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This study applies Ultrafast module-GC (UFM-GC) with direct resistively heated columns to routine analysis of a group of essential oils of differing complexities (chamomile, peppermint, rosemary and sage). Essential oils were analysed by conventional GC with conventional inner diameter (i.d.) columns (0.25 mm) of different lengths (5 and 25 m long) and by Fast GC and Ultrafast module-GC with narrow bore columns (0.1 mm i.d., 5 m long). Column performance were evaluated and compared through their Grob test, separation number and peak capacity. Ultrafast module-GC was successful in the qualitative and quantitative analysis of essential oils of different compositions with analysis times between 40 s and 2 min versus 20-60 min required by conventional GC. Critical pairs or groups of components were separated by carefully tuning selectivity of the stationary phase to compensate for loss of efficiency due to the use of short columns and high temperature rates. The Ultrafast module-GC results of peppermint e.o. analyses were also validated and compared to those obtained by conventional GC; by measuring precision over time (i.e. repeatability and intermediate precision) and accuracy. Ultrafast module-GC showed a good separation reproducibility affording reliable component identification through the relative retention times and quantitative determination through normalised peak areas. Accuracy data also showed that Ultrafast module-GC and conventional GC normalised areas and areas percentage were perfectly comparable.

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Section: Column Evaluationsupporting

confidence: 87%

Section: Discussionmentioning

confidence: 99%

Section: Column Evaluationmentioning

confidence: 99%

See 1 more Smart Citation

Direct resistively heated column gas chromatography (Ultrafast module-GC) for high-speed analysis of essential oils of differing complexities

Bicchi

Brunelli

Cordero

et al. 2004

Journal of Chromatography A

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“…The separation measure (S) is an universal parameter independent of the peak shape introduced by Blumberg and Klee [16] and defined as the number of consecutive non-overlapping r-intervals within an arbitrary time interval (t b -t a ); it can be calculated with Eq. (5)…”

Section: Influence Of F-gc Combined With a Qmsmentioning

confidence: 99%

Fast‐GC–conventional quadrupole mass spectrometry in essential oil analysis

Rubiolo

Liberto

Sgorbini

et al. 2008

J of Separation Science

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This study reports on the compatibility of a conventional quadrupole MS (qMS) as detector for Fast-GC in terms of separation, identification, and quantitation when applied to the analysis of peppermint essential oil (e.o.), adopted as representative of this field. The influence of Fast-GC carried out on a 10 mx0.1 mm id narrow bore column with temperature programmes from 20 to 60 degrees C/min on the results of a qMS in total ion chromatograms (TIC) at different speeds (from 999 and 11 111 amu/s) and SIM modes was evaluated on ten differently abundant components characterizing peppermint e.o. Separation measure (S), peak capacity (n), and half height peak width were taken as separation parameters; match quality, number of scans per peak (NP), spectral skewing, and TIC area repeatability were used for identification. Quantitation was in SIM mode and NP, dwell time, SIM area repeatability and calibration curves, LOD, and LOQ of the selected components were measured. The results show that the peppermint e.o. markers can successfully be analysed qualitatively and quantitatively by F-GC-qMS up to temperature programmes of 60 degrees /min provided that a suitable scan speed is applied. Fast-GC-qMS reduces analysis time by a factor greater than ten and gives results that are qualitatively reliable and quantitatively comparable to those obtained by conventional GC-qMS.

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“…Nevertheless, n c is useful for the comparison of the separation performance of different analytical systems. Additional discussion of the concept of peak capacity including comparison of its alternative (not always equivalent) definitions can be found elsewhere [2].…”

Section: Introductionmentioning

confidence: 99%

Linear peak capacity of a comprehensive multi‐dimensional separation

Blumberg¹

2008

J of Separation Science

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In order to resolve (quantifiably and identifiably separate) the same number of peaks in the analysis of the same mixture yielding statistically uniform peak distribution, a comprehensive 2-D separation needs a two times larger peak capacity than a 1-D separation does. Each additional dimension further reduces the utilization of the peak capacity of comprehensive multi-dimensional (MD) separation by a factor of two per dimension. As a result, the same peak capacity means different things for separations with different dimensionalities. This complicates the use of the peak capacity for comparison of the potential separation performance of the separations with different dimensionalities. To facilitate the comparison, a concept of a linear peak capacity has been proposed. The linear peak capacity of an MD separation is the peak capacity of a 1-D separation that, in the analysis of the same mixture, is statistically expected to resolve the same number of peaks as the MD separation is. There are other factors that differently affect the performance of the separations that have different dimensionalities. Peak capacity of a 2-D separation with a rectangular separation space is 27% larger than the product of the peak capacities of its first and second dimension. This advantage of a 2-D separation is essentially nullified by the fact that the peak capacity of the first dimension of an optimized 2-D separation cannot be higher than 80% of the peak capacity of its first dimension standing alone. All in all, the incremental peak capacity gained from addition of a second dimension will not exceed 50% of the peak capacity of the added second dimension. All results are valid for arbitrarily shaped (not necessarily Gaussian) peaks.

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Metrics of separation in chromatography

Cited by 47 publications

References 20 publications

Direct resistively heated column gas chromatography (Ultrafast module-GC) for high-speed analysis of essential oils of differing complexities

Direct resistively heated column gas chromatography (Ultrafast module-GC) for high-speed analysis of essential oils of differing complexities

Fast‐GC–conventional quadrupole mass spectrometry in essential oil analysis

Linear peak capacity of a comprehensive multi‐dimensional separation

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