The Stability Study of Thermodynamic Parameters of Sorption of Light Hydrocarbons on Poly [Trimethylsilyl (Propyn-1)] at Different Temperatures

2019 ◽  
Vol 57 (9) ◽  
pp. 778-783
Author(s):  
V E Shiryaeva ◽  
A A Korolev ◽  
T P Popova ◽  
A Y Kanateva ◽  
A A Kurganov

Abstract Chromatographic determination of the thermodynamic parameters of sorption for light hydrocarbons retention on a stationary phase based on poly [trimethylsilyl (propyn-1)] (PTMSP) was performed and the effect of column preheating at temperatures up to 260°C on the retention of analytes was investigated. It was shown that heating the column to 130°C does not affect the retention of the analytes. At temperatures above 130°C, the gradual decrease of the retention of analytes on PTMSP stationary phase is observed. The process is non-selective and proceeds at the same extent for all the studied hydrocarbons, regardless of the size and geometry of the molecule. Values of enthalpy and entropy of sorption of light hydrocarbons are determined for the original column and after its aging at 200°C. The enthalpy of sorption of the analytes at the PTMSP phase is practically independent on the heating temperature of the PTMSP phase, whereas the loss of entropy increases after heating. The increase of the entropy factor after the heating of the PTMSP stationary phase is associated with its aging and is confirmed by the construction of compensation functions for treated and untreated columns.

2015 ◽  
Vol 2015 ◽  
pp. 1-5 ◽  
Author(s):  
Mohammed Mutasim Elimam ◽  
Shaza Wagiealla Shantier ◽  
Elrasheed Ahmed Gadkariem ◽  
Magdi Awadalla Mohamed

Simple spectrophotometric methods were developed for the quantitative determination of colistin sulphate in bulk and dosage forms. The methods were based on the measurement of first and second derivative spectra of colistin sulphate at 298 nm and 318 nm, respectively. Beer’s law was obeyed in the concentration range 800–4000 IU/mL with good correlation coefficient (not less than 0.998) for both methods. The developed first derivative spectrophotometric method was then selected to study the degradation behavior of colistin sulphate in alkaline media at different temperatures as the second derivative method failed to give reproducible results for the stability study. The pH-rate profile indicates a first-order dependence of the degradation rate on [OH−] at pH ranging between 8 and 11. The obtained results for the photochemical study reflected photostability of colistin sulphate.


2021 ◽  
Vol 18 (39) ◽  
pp. 14-32
Author(s):  
Hind Sadiq Al-WARD ◽  
Mouayed Qassssim AL-ABACHI ◽  
Mohammed Rifaat AHMED

Background: Tetracycline is one of the most important antibiotics. It is used to treat many different bacterial infections. It is often used in treating severe acne, or sexually transmitted diseases such as syphilis, gonorrhea, or chlamydia. In some cases, tetracycline is used when penicillin or another antibiotic cannot be used to treat serious infections such as the ones caused by Bacillus anthracis, Listeria, Clostridium, Actinomyces. Aim: synthesized a new novel reagent used to determine TCH spectrophotometrically by using diazonium and coupling reaction. Methods: Four new substituted procaine derivatives were prepared by simple organic methods using aniline derivatives. A spectrophotometric approach was established for the micro-determination of TCH. The stoichiometry was investigated using mole ratio and continuous variation methods, and the stability constant was also estimated. The ΔG, ΔH, and ΔS were determined as thermodynamic parameters for evaluating the effect of temperature on the reaction. Results: Substituted procaine derivatives were prepared, and o-hydroxy procaine seems to be the best reagent used to determine TCH by diazotization and coupling reaction. The result was a yellow water-soluble dye with a maximum absorbance of 380 nm. The reaction conditions were studied and optimized. Beers law was obeyed over a concentration range (2.5–50) μg.mL-1 for TCH. The molar absorptivity was (14.4669.103) L.mol-1.cm-1, and the detection limit was (0.5052) μg.mL-1. The stoichiometry of the formed product was found 1:1 (o-hydroxyprocaine: TCH). The stability constant indicated that the product formed was stable, and the thermodynamic parameters showed that the diazonium salt reaction was preferred to occur at a low temperature. Conclusions: a simple, accurate, and fast method was developed to determine TCH in pure form and pharmaceuticals by coupling the TCH with a newly synthesized procaine derivative reagent (o-hydroxy procaine) in a basic medium.


2014 ◽  
Vol 5 (2) ◽  
Author(s):  
Irena Kasagić Vujanović ◽  
Dijana Jelić ◽  
Vesna Antunović ◽  
Biljana Jančić Stojanović ◽  
Darko Ivanović

Valuable information concerning stability of compounds can be obtained by using different media (water, hydrochloric acid or sodium hydroxide) for dissolution of active pharmaceutical substances. Furthermore, additional knowledge is gained by performing experiments at different temperatures. This research paper deals with the stability of amlodipine besylate and bisoprolol fumarate in different media at different temperatures, whereby certain conclusions are drawn. For stability assessment, chemical kinetics approach was used, and constant rate (k), half-time (t1/2) and activation energy (Ea) were used for prediction of compound stability degree. The stability of amlodipine besylate and bisoprolol fumarate were tested, both separately and in mixture, in water and in 0.01M HCl. All the investigated solutions were treated at two temperatures 25° and 70°C at the following time intervals: 0, 1 h, 24 h, 48 h and 72 h. Hydrophilic Interaction Liquid Chromatography – HILIC method, previously developed and validated, was used. On the basis of obtained results it was concluded that amlodipine-besylate was more stable in water than in acid medium, more stable in mixture rather than individually and more stable at lower temperatures. This was confirmed by the obtained values of monitored parameters: amlodipine besylate Ea = 30.68 kJ mol-1, k (25 °C) = 0.000333 mM h-1, k (70 °C) = 0.00169 mM h-1; amlodipine besylate in mixture Ea = 42,414 kJ mol-1, k (25 °C) = 1.27∙10-4 mM h-1, k (70 °C) = 0.0012 mM h-1. Based on the obtained approximate Ea value for bisoprolol fumarate in acid (59 kJ mol-1) and in water (56 kJ mol-1), bisoprolol fumarate showed excellent stability against the media in which it was studied. On the other hand, the temperature had a significant effect on the stability of bisoprolol fumarate. These results provide the relevant information about the stability of the tested active substances, and may be of importance during the development of an appropriate pharmaceutical product. A bigger influence on the stability of bisoprolol fumarate had a temperature effect.


2010 ◽  
Vol 40 (1) ◽  
pp. 30-40 ◽  
Author(s):  
Mariusz Kluska ◽  
Krzysztof Pypowski ◽  
Ireneusz Chrzaścik ◽  
Renata Gadzała-Kopciuch ◽  
Ewa Witkowska-Krajewska

2018 ◽  
Vol 28 ◽  
pp. 01019
Author(s):  
Beata Kultys ◽  
Karolina Waląg

Headspace technique and gas chromatography method with mas detector has been used for the determination of volatile organic compounds (VOC) emitted from various building and finishing materials, such as sealing foams, mounting strips, paints, varnishes, floor coverings. The tests were carried out for different temperatures (in the temperature range of 60 to 180 °C) and the time of heated vials with tested materials inside. These tests were conducted to verify the possibility of use this method of determination the VOC emission. Interpretation of chromatograms and mass spectra allowed to identify the type of compounds emitted from the tested materials and the optimum time and temperature for each type of material was determined. The increase in heating temperature of the samples resulted in increase the type and number of identified compounds: for four materials the increase was in the whole temperature range, for others it was from 90 °C. On the other hand, emission from mineral wool was low in whole temperature range. 30-minutes heating of the samples was sufficient to identify emitted compounds for most of tested materials. Applying a longer time, i.e. 24 hours, significantly increased the sensitivity of the method.


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