Development of a membraneless extraction module for the extraction of volatile compounds: application in the chromatographic analysis of vicinal diketones in beer.
A membraneless extraction module (MLEM) for the sample preparation of volatile compounds and its use for the chromatographic analysis of vicinal diketones in beer are reported. The extraction process is based on the same principles of gas diffusion (GD) and pervaporation (PV); however it does not use a membrane. This module has a lower chamber where the sample continuously flows, while volatile compounds evaporate to the headspace. Inside the module there is a suspended small reactor, where a small volume of a suitable acceptor solution is placed. This extraction module was tested in the determination of vicinal diketones (VDKs) in beer (CV=5%; LOD=4 microg L(-1)), showing applicability with real samples. Several parameters of the extraction process, such as temperature, sample flow and extraction time, were studied and optimized. This module proved to be a good tool for the sampling of volatile compounds, since the extraction is made without using a membrane avoiding all the robustness problems related with its use.
Membraneless vaporization unit for direct analysis of solid sample.
A new apparatus, called 'membraneless vaporization' (MBL-VP) unit was designed and developed for direct analysis of solid samples. Solid analyte was converted into a gaseous form which then reacts with an indicator reagent. Change in absorbance was used to quantitate the analyte. Stirring with a magnetic bar was employed to facilitate the evaporation of the gas. Unlike the pervaporation technique, hydrophobic membrane was not required for this MBL-VP technique. Application of the membraneless technique for direct determination of calcium carbonate in calcium supplements, has shown to be very precise (R.S.D.=2.5% for 0.16 mmol CO3(2-)), with detection limit of 0.5 mg CaCO3. Results by this method agreed well with flame atomic absorption spectrometric method. Sample throughput was 20 samples h(-1).
Temperature effects on lily development rate and morphology from the visible bud stage until anthesis.
Day (DT) and night temperatures (NT) influenced Lilium longiflorum Thunb. 'Nellie White' stem elongation and development rate from the visible bud stage (VB) until anthesis. Plant height increase after VB was a function of the difference (DIF) between DT and NT (DT-NT). Plant height increased 90% as DIF increased from - 16 to 16C. A cubic model described bud development rate as a function of temperature from 14 to 30C. A linear model adequately described bud development rate as a function of average daily temperature from 14 to 21C. Based on the linear model, bud development rate increased 0.05 per day for each 1C increase in average daily temperature. The base temperature for bud development, i.e., the temperature at which bud development rate was 0, was calculated as 3.5C. Greenhouse forcing of vernalized Easter lilies is commonly divided into three phases: I) placement of vernalized bulbs in the greenhouse to flower initiation, II) flower initiation to VB, and III) VB to anthesis (De Hertogh and Wilkins, 1971). Plant morphological development differs during each of the forcing phases (De Hertogh and Wilkins, 1971). Growth during phase I is vegetative and consists of stem elongation and leaf expan- sion. Flower initiation, leaf expansion, and stem elongation oc- cur during phase II. Inflorescence expansion and stem elongation occur during phase III. Lily responses to temperature during phase III differed from those during phases I and II (Wang and Roberts, 1983). Lily development rate, quantified as days to unfold a leaf, is a de- creasing linear function of average daily temperature between 14 and 30C during phases I and II (Karlsson et al., 1988). Lily development rate during phase III is a nonlinear function of temperature (Healy and Wilkins, 1984). The effect of temper- ature on the rate of lily development decreases as DT and/or NT increase during phase III (Rob and Wilkins, 1973; Healy and Wilkins, 1984). Easter lily morphological development is thermomorpho- genie. For instance, internode length increases as the DIF be- tween DT and NT increases (Erwin et al., 1989). In addition, leaf orientation, leaf length, and flower length are also influ- enced by diurnal changes in temperature.