In gas chromatography, for the analysis, the most important thing is the well-chosen column. After having decided about which stationary phase is the best for our measurement and we know the length, the inner diameter and film thickness, we can buy the column from a lot of manufacturers. The products of these manufacturers’ look similar to each other, but they are different, because of the different manufacturing technologies. These differences could have significant influence on the separation. It is so important to compare the „same” columns, despite the manufacturers’ efforts to produce the best quality columns.5 % diphenyl – 95 % dimethyl polysiloxane stationary phase is widely used. Its slight polarity makes it able to determine very different compounds from the alkanes, through volatiles, drugs, fatty acid methyl esters, amines or phenols.In our work, we tested 5 % diphenyl – 95 % dimethyl polysiloxane stationary phase columns with an 8-component mixture. These columns were from different manufacturers. During isothermal conditions, we determined the height equivalent of theoretical plates on 8 linear velocity level. We represented these parameters as the function of linear velocity. With a constant linear velocity, we measured the excess sorption enthalpy and entropy. From the chromatograms we spotted differences in the retention and in resolution, which is important if we use the column for volatiles or for complex samples. With these parameters we can show many differences between the columns. These parameters have significant influence when we want to use our column for a given task.
Detector response of 12 chlorobenzenes was investigated (mono-, di-, tri-, tetra-, penta-, and hexachlorobenzene, CBs) using flame ionization detector in a capillary gas chromatographic system. We determined the signal-reducing effect of the chlorine atom on the aromatic ring relative to the number of the chlorine substituents and expressed with the effective carbon number (ECN). Benzene was applied as a reference substance. Using the signal-modifying pattern of the chlorine atoms on the benzene's response, we developed an alternative calibration measurement method (CBs-ECN method) for the 12 CBs and compared it with classic calibration. The differences in the concentrations calculated by the two quantitative methods were under 4.5% for 11 CBs and 7% for one compound.Taking advantage of the opportunities provided by the CBs-ECN pattern it is not necessary to apply all of the 12 CBs but only one single component, the hexachlorobenzene for the calibration. With this simplification, the preparation of the calibration standards is faster, does not require purchasing all 12 CBs for each subsequent calibration, and the exposure to harm and expenses are reduced.
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.
In our research, seven 624-type capillary columns were investigated. All the columns were the same in length, internal diameter, and film thickness (30 m × 0.32 mm × 1.0 µm). However, they were produced by different manufacturers or the same manufacturer but in different batches. Even though the manufacturers recommend them as "equivalent columns" this equivalence did not prevail even in the case of columns produced by the same manufacturer. Our examination criteria centered on the quantitative determination ability of the columns. A homemade column test mixture was compiled to represent all the second-order interactions that can occur between the analyte and stationary phase. Although theoretically these columns have the same stationary phase quality, they did not result in the same chromatograms. In addition to the origin and batch of the column, the "history of the column" contributes likewise to the different peak symmetry, retention order, and even peak areas that affect the quantitative determination. We quantified this quantitative determination ability with the effective carbon number (ECN) and the Limit of Quantitation (LoQ) values. Based on our results the attainable LoQ and ECN values depend at least as much on the origin and actual state of the stationary phase as on the measurement conditions to be optimized. In our paper, we demonstrate the extent to which the same stationary phases offered by different companies and/or different backgrounds can influence our detection limit and detector response even if the relevant columns have theoretically the same chemical structure.
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