Ni(II) complex of octasubstituted tetraphenylporphine as a stationary phase for gas chromatography

2017 ◽  
Vol 21 (02) ◽  
pp. 103-109 ◽  
Author(s):  
Vladimir A. Burmistrov ◽  
Alexander S. Semeikin ◽  
Gregory V. Kuvshinov ◽  
Victor V. Aleksandriiskii ◽  
Tatiana V. Lubimova ◽  
...  

The Ni(II) complex of 5,10,15,20-tetrakis[3[Formula: see text],5[Formula: see text]-di(2[Formula: see text]-methylbutyloxy)phenyl]porphine was synthesized and characterized by 1H NMR, UV-vis spectroscopy and MALDI-TOF mass-spectrometry. The stationary phase on the base of synthesized Ni(II) complex was used for chromatographic separation of isomeric methyl- and dimethylpyridines. The high structural selectivity of this sorbent was explained by giving the results of DFT calculation of pyridine derivatives axial complexes with porphyrin Ni(II) complexes.

2007 ◽  
Vol 2 ◽  
pp. 117739010700200
Author(s):  
Ashraf Ghanem

Chirasil-β-Dex containing an undecamethylene spacer (C11-Chirasil-Dex) was synthesized and used as chiral stationary phase (CSP) in enantioselective gas chromatography (GC). The versatility of the new stationary phase in the simultaneous enantiomeric separation of a set of N-alkylated barbiturates is demonstrated.


2010 ◽  
Vol 75 (11) ◽  
pp. 1097-1114 ◽  
Author(s):  
Romana Sokolová ◽  
Ilaria Degano ◽  
Magdaléna Hromadová ◽  
Jana Bulíčková ◽  
Miroslav Gál ◽  
...  

The oxidation mechanism of hematoxylin was studied in phosphate buffers and 0.1 M KCl by cyclic voltammetry and UV-Vis spectroscopy under deaerated conditions. The redox potential of hematoxylin in buffered solution strongly depends on pH. A two electron oxidation is preceded by deprotonation. The homogeneous rate of deprotonation process of hematoxylin in 0.1 M phosphate buffer is kd = (2.5 ± 0.1) × 104 s–1. The cyclic voltammetry under unbuffered conditions shows the distribution of various dissociation forms of hematoxylin. The dissociation constants pK1 = 4.7 ± 0.2 and pK2 = 9.6 ± 0.1 were determined using UV-Vis spectroscopy. The final oxidation product was identified by gas chromatography with mass spectrometry detection as hemathein. The distribution of oxidation products differs under buffered and unbuffered conditions. The dye degradation in natural unbuffered environment yields hemathein and hydroxyhematoxylin, which is absent in buffered solution.


Author(s):  
Gyula Nyerges ◽  
Dénes Szieberth ◽  
Judit Mátyási ◽  
József Balla

Gas chromatography (GC) is a frequently used analytical method for the determination of permanent and organic air components. The analysis usually needs two different columns in practice. The molecular sieve stationary phase can separate oxygen, nitrogen and carbon monoxide, but irreversibly adsorbs carbon dioxide and water. Porapak type columns are applicable for the measurement of carbon dioxide, however oxygen, argon, nitrogen and carbon monoxide are co-eluted. Usually these two types of columns are used in parallel for the determination. Carboxen stationary phase can separate carbon monoxide and carbon dioxide, but argon, oxygen and nitrogen are co-eluted. Thermal conductivity detector (TCD) and flame ionization detector (FID) are used commonly together for the determination of the separated components. TCD is applied for permanent gas analysis whereas FID – combined with a methanizer – is used for the detection of carbon monoxide, carbon dioxide and light hydrocarbons. Mass spectrometer (MS) is also a potential detector, because the properly chosen fragment ions can increase the selectivity.We developed a method for the determination of air components, using only one column and one detector. This method is suitable for the measurements by combining the advantages of the carboxen column with mass spectrometry. The validation parameters of the method were in the acceptable interval, so this method is able to determine the air components. The application of this technique to the analysis of cave air provided valuable information to the exploration of the Molnár János cave system.


1985 ◽  
Vol 50 (8) ◽  
pp. 1808-1818 ◽  
Author(s):  
Ján Krupčík ◽  
Dušan Repka

A mixture of alcohols obtained by hydroformylation of C10-C13 n-alkenes was analyzed by capillary gas chromatography using Carbowax 20M stationary phase, and acetates prepared from the alcohols were analyzed on capillary columns using Carbowax 20M and Apiezon L stationary phases. The capillary gas chromatography and gas chromatography-mass spectrometry treatment gave evidence that all of the 24 alcohols that could form by the hydroformylation reaction mechanism were present.


2020 ◽  
Vol 25 (1) ◽  
pp. 30-36
Author(s):  
Netra Lal Bhandari ◽  
Kabita Bist ◽  
Jyoti Ghimire ◽  
Santosh Chaudhary ◽  
Durga Prasad Pandey ◽  
...  

In the present study, an attempt has been made to utilize the natural plant dye extracted from petals of Euphorbia pulcherrima (locally called as Lalupate) via green techniques using water as solvent at boiling condition, for fabrics dyeing in combinations with natural mordants such as Aloe vera, Marcha (traditional yeast used in fermentation), and Chuk (traditional concentrated lemon juice), and artificial mordants like K2Cr2O7, CuSO4, and FeSO4. The dye extract has been characterized by thin-layer chromatography (TLC), ultraviolet-visible (UV-Vis) spectroscopy, Fourier transform infrared (FTIR) spectroscopy, gas chromatography-mass spectrometry (GC-MS) and optical microscopy (OM). The results have shown that the dyeing of the fabrics with the E. pulcherrima dye in combination with K2Cr2O7 as well as Chuk is effective concerning wash fastness, dry fastness, and colorfastness.


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