SummaryThe selection of stationary phases in capillary gas chromatography is discussed. Methyl silicone, phenyl methyl silicone, trifluoropropyl methyl silicone, biscyanopropyl silicone, and high molecular weight (HMW) polyethylene glycol are considered to be the basic phases. Selectivities and polarities between these phases are obtained by selectivity tuning. Selectivity tuning can be performed in three different ways, namely by synthesizing a tuned stationary phase, by mixing the basic phases, or by coupling capillary columns of different selectivities. In coupling capillary columns the variables are column length, @-value, temperature, and/or pressure.
The conversion of substantial amounts of ammonia nitrogen into organic nitrogen as a direct result of nitrification at neutral pH-values, was monitored in soil suspensions amended with ammonium nitrogen. The influence of the chemolithotrophic nitrifying bacteria was verified by applying nitrapyrin as a selective inhibitor in control experiments. In addition, the role of phenolic compounds was examined by adding a naphthol. The factors influencing the nitrification process i.e. pH, NH+-N, NO~-N, NO~-N were measured during a 60 days incubation period. Nitrification started to be active after 5 and 10 days in the normal and the naphthol spiked soil suspensions respectively; it was inhibited in the nitrapyrin controls. Parallel with nitrification, formation of organic nitrogen was observed. The humic matter fractions were extracted and analyzed by I.R. spectroscopy which revealed the valence vibration ranges of nitro and nitroso groups fixed in different positions on aromatic compounds, both for normal and naphthol spiked samples. High resolution gas chromatography combined with mass spectroscopic analysis indicated the formation of nitrosonaphtholes. In addition a novel organic nitro compound was identified i.e. an azido nitro benzene. No nitrogen was fixed in the samples treated with nitrification inhibitor. A mechanism for the fixation of nitrite nitrogen during nitrification is proposed.
SummaryThe chromatographic performance of 10 m X 100 pm i.d. capillary columns, coated with different stationary phases, was studied. TZ-6 plots were measured at different temperature program rates. The polarity and selectivity are strongly influenced by the temperature program rate. The analysis time depends on the capacity ratio and the selectivity factor; stationary phase selection thus is an important aspect in high speed capillary GC. A number of applications is presented and the applicability of split injection is discussed.
SummaryThe resolution of the diastereoisomers of norpristane, pristane, and phytane was studied as a function of the column internal diameter and/or the residence time of the compounds in the column. Increasing the residence time in the column by operating the column at a lower temperature program rate enhances the resolution more than reducing the internal diameter of the column. Practical experience with ultra narrow bore columns is also presented.
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