Identification of the Compounds Evaporating from Waste Waters of Petrochemical Plants
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Since our olfactory test proved that the waste waters from each plant were most important source of the odor at a petrochemical industrial area, we sampled the waste waters in 2-20 1 of polyethylene bottles at the oil separator of each plant and the waste water treatment plant, and brought to our laboratory. For infrared spectrometry and mass spectroscopy, the nitrogen gas was bubbled through the 500ml-waste water in a flask and components evaporated with nitrogen gas were trapped in a 30cm U-sharped glass trap which was packed with glass beads (30-60 mesh) and was attached to the six-port gas sampling valve on a gas chromatograph and was chilled in liquid nitrogen. The exit end of the trap was led to water in a flask and the gas flaw rates measured by bubbles were maintained at 100-200ml/ min (see Fig. I). Sampling times were 40 to 60 minutes. At the completion of a run, the trap was brought to 80-100°C by hot water and its content was simultaneously swept into the column by turning the sampling valve through 60°. But for determination of sulfur compounds, We directly injected about 3ml of gas samples taken over the surface of waste waters into a gas chromatograph.<BR>The combination of gas chromatography with infrared spectrometry has been studied by many workers, and we reported simple and efficient technique for it. This technique is composed of three processes, viz, collection of effluent gas fractions from gas chromatograph into a smoothly movable 100ml glass syringes, introduction of these fractions into a gas cell (volume: 100ml, light path length; 10cm, window: NaCl), and measurement on an infrared spectrometer. To introduce separately the fractions of close peaks to syringes, an inlet port of a six-port cock (see Fig. 5) is connected to the exit of effluent gas and syringes to every other exit of the cock. The empty ports are utilized to vent unnecessary effluent gas. When the fractions are above three, syringes are detached from the cock and are sealed with vinyl cup at the spout. After attaching an injection neeile to the syring, the fraction in the syringe is introduced through silicone rubber septum into the evacuated gas cell (see Fig. 6). The maximum permissible pressure of the gas cell is a few atmospheres and therefore the fractions of the same component taken in different syringes can be added to make up several hundred milliliters in the cell if the infrared absorption by the component is too weak to identify. The infrared spectrum is illustrated in Fig. 7, in which benzene and chloroform make one peak on the chromatogram and are identified on the same spectrum.<BR>To combine a gas chromatographic unit with a mass spectrometer, the separation jet method was used. The gas chromatograms were taken by monitoring the total ion current of a mass spectrometer. The mass apectrum of the fraction which correspounds to the infrared spectrum of Fig. 7 is shown in Fig. 8 and the same two compounds as identified by the infrared spectrum were also recognized. But the sensitivity of the mass spectrometer was hundreds times of that of the infrared spectrometer.<BR>The compounds identified are listed in Table 1 together with the comoounds reported in a previous paper We notice that common compounds were found in most of plants and at other place, so we can expect that these compounds in Table 1 will be found at many other petrochemical plants.
- 社団法人 大気環境学会の論文
社団法人 大気環境学会 | 論文
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