Gas Chromatographic Parameters. I. Correlation Between Column Efficiency, Resolving Power, and Analysis Time

1986 ◽  
Vol 24 (4) ◽  
pp. 147-152 ◽  
Author(s):  
J. Ceulemans
1969 ◽  
Vol 52 (5) ◽  
pp. 1010-1014
Author(s):  
Akos D St Clair ◽  
J G Lamberton ◽  
R R Claeys ◽  
R L Goulding

Abstract A vacuum trapping apparatus was developed for the collection of volatiles and for the determination of rates of volatilization of DDVP from Vapona-PVC resin formulations. More than 99% of the total volatiles was collected by this apparatus. To determine the total content of DDVP in the resin four extracting solvents were tested. Acetone was the most effective solvent. An improved GLC procedure was developed for the quantitation of DDVP. Several liquid phases were compared and optimum chromatographic parameters were examined. Tailing peaks were obtained with DC-11 and DC-11 + Epon 1001. Carbowax 20M gave symmetrical peaks, but optimum column efficiency was obtained on a 7% neopentyl glycol adipate column. The relative standard deviation for the analysis of DDVP by GLC was ±1.8%.


Separations ◽  
2020 ◽  
Vol 7 (3) ◽  
pp. 46
Author(s):  
Maria Kalaboka ◽  
Christoforos Chrimatopoulos ◽  
Cristina Jiménez-Holgado ◽  
Vasiliki Boti ◽  
Vasilios Sakkas ◽  
...  

Aside from the classical residues of persistent organic pollutants (POPs), the occurrence of emerging contaminants (ECs) in the environment has become a subject of increasing concern due to their harmful impact on the aquatic environment. Wastewater treatment plant (WWTP) effluents are major sources of environmental pollution. Therefore, data concerning their existence is required. In this study, twenty compounds representative of different drug groups considered ECs and belonging to antibiotics, antipsychotics, anti-inflammatory drugs plus acesulfame K were selected to be accurately detected and quantified with UHPLC–LTQ-Orbitrap MS in hospital and urban WWTP effluents. Chromatographic parameters (column efficiency, mobile phase, etc.), as well as mass spectrometry conditions concerning ionization mode and Orbitrap analysis (ESI options, mass resolving power, AGC target, tube lens, injection time), were evaluated. Moreover, a novel fabric phase sorptive extraction (FPSE) method based on fiber glass coated with PEG300 was employed as sample preparation process. Experimental parameters affecting extraction and desorption steps such as sample pH, extraction time, ionic strength, elution time and solvent have been optimized. The optimized methodology was validated providing excellent linearity (R2 > 0.99), and low detection and quantification limits up to 3.1 and 9.3 ng/L, for carbamazepine, respectively. Relative recoveries ranged from 81.1% to 114.0%, while a medium matrix effect for most of the target compounds occurred. Applying the above analytical method in effluents of WWTPs from NW Greece, nine compounds were quantified with concentrations that varied from 55.4 to 728.4 ng/L.


2018 ◽  
Vol 42 (1) ◽  
pp. 38-50 ◽  
Author(s):  
José Luís Dores-Sousa ◽  
Jelle De Vos ◽  
Sebastiaan Eeltink

Author(s):  
F.J. Sjostrand

In the 1940's and 1950's electron microscopy conferences were attended with everybody interested in learning about the latest technical developments for one very obvious reason. There was the electron microscope with its outstanding performance but nobody could make very much use of it because we were lacking proper techniques to prepare biological specimens. The development of the thin sectioning technique with its perfectioning in 1952 changed the situation and systematic analysis of the structure of cells could now be pursued. Since then electron microscopists have in general become satisfied with the level of resolution at which cellular structures can be analyzed when applying this technique. There has been little interest in trying to push the limit of resolution closer to that determined by the resolving power of the electron microscope.


Author(s):  
A. V. Crewe

The high resolution STEM is now a fact of life. I think that we have, in the last few years, demonstrated that this instrument is capable of the same resolving power as a CEM but is sufficiently different in its imaging characteristics to offer some real advantages.It seems possible to prove in a quite general way that only a field emission source can give adequate intensity for the highest resolution^ and at the moment this means operating at ultra high vacuum levels. Our experience, however, is that neither the source nor the vacuum are difficult to manage and indeed are simpler than many other systems and substantially trouble-free.


Author(s):  
Henry S. Slayter

Electron microscopic methods have been applied increasingly during the past fifteen years, to problems in structural molecular biology. Used in conjunction with physical chemical methods and/or Fourier methods of analysis, they constitute powerful tools for determining sizes, shapes and modes of aggregation of biopolymers with molecular weights greater than 50, 000. However, the application of the e.m. to the determination of very fine structure approaching the limit of instrumental resolving power in biological systems has not been productive, due to various difficulties such as the destructive effects of dehydration, damage to the specimen by the electron beam, and lack of adequate and specific contrast. One of the most satisfactory methods for contrasting individual macromolecules involves the deposition of heavy metal vapor upon the specimen. We have investigated this process, and present here what we believe to be the more important considerations for optimizing it. Results of the application of these methods to several biological systems including muscle proteins, fibrinogen, ribosomes and chromatin will be discussed.


Author(s):  
C. T. Nightingale ◽  
S. E. Summers ◽  
T. P. Turnbull

The ease of operation of the scanning electron microscope has insured its wide application in medicine and industry. The micrographs are pictorial representations of surface topography obtained directly from the specimen. The need to replicate is eliminated. The great depth of field and the high resolving power provide far more information than light microscopy.


Author(s):  
A. V. Crewe

We have become accustomed to differentiating between the scanning microscope and the conventional transmission microscope according to the resolving power which the two instruments offer. The conventional microscope is capable of a point resolution of a few angstroms and line resolutions of periodic objects of about 1Å. On the other hand, the scanning microscope, in its normal form, is not ordinarily capable of a point resolution better than 100Å. Upon examining reasons for the 100Å limitation, it becomes clear that this is based more on tradition than reason, and in particular, it is a condition imposed upon the microscope by adherence to thermal sources of electrons.


Author(s):  
Teruo Someya ◽  
Jinzo Kobayashi

Recent progress in the electron-mirror microscopy (EMM), e.g., an improvement of its resolving power together with an increase of the magnification makes it useful for investigating the ferroelectric domain physics. English has recently observed the domain texture in the surface layer of BaTiO3. The present authors ) have developed a theory by which one can evaluate small one-dimensional electric fields and/or topographic step heights in the crystal surfaces from their EMM pictures. This theory was applied to a quantitative study of the surface pattern of BaTiO3).


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