Chromato-desorption method for obtaining gas streams with a given content of organohalogen compounds
Abstract
The paper shows the possibility of using chromato-desorption systems to obtain calibration mixtures in this case, it is a promising method for obtaining GOS in the range of less than 10 ppm. It is revealed that the buffer capacity is largely determined by the concentration gradient in the initial part of the system, while the concentration gradient can be provided not only by the amount of analyte applied, but also by the geometric features of the system: for a cylindrical sectional system used in dynamic mode, the buffer capacity is formed due to the difference in the mass of the sorbent, which is similar in efficiency to 25% the concentration gradient in the initial part of the system at an equal mass of analyte and sorbent.
Injection-type CDCs operated in discrete mode show greater efficiency (the greater the stability of maintaining quasi–constant concentration and the lower the quasi-constant concentration) - the smaller the difference between the diameter of the system and the outlet pipe, which is due to the formation of a dead volume in the wall space, due to which the redistribution of the analyte occurs more slowly and unevenly, which in turn determines the effectiveness the analyte is replenished on the last theoretical plate, which is responsible for concentration at the exit of the system. In such systems, it is optimal to exceed no more than twice the diameter of the tubular flow system and the outlet pipe.
In a cone-shaped CD with a gradual narrowing, the effect of the wall dead zone is smoothed out. At the same time, in the case of miniature sizes, the system can be operated in the backwash mode: in this case, the effect of the buffer zone manifests itself more slowly, the system resource increases (6-8 discrete inputs at 1 stage of quasi-stability), but stability deteriorates significantly at 2 stages (COE increases to 25-35%).
The testing of the proposed approaches for the quantitative determination of GOS using the "introduced-found" method using the example of carbon tetrachloride (in the concentration range of 8-1 ppm) has shown the effectiveness of chromato-desorption systems in dynamic mode and injection systems in discrete mode with automatic dosing. The deviation from the reference value does not exceed 20-24%. Similar dependences were obtained for the organofluorine compound perfluoro3-dimethylcyclohexane (for the concentration range from 1 to 0.1 ppm).
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