Different carrier gases may be used: nitrogen, hydrogen or helium. The type of carrier gas does not significantly modify the signal of toluene in water. We used helium at 2 ml/min as carrier gas. The flow rate also has a significant effect on the signal form: at too low rates, the peak becomes smaller and wider and is more difficult to interpret.
3.2. Equilibration and extraction time
With optimized apparative conditions, it was possible to test the other parameter affecting the measurement of a headspace. The headspace measurement takes place in two steps: in the first step, the solution to be analyzed has to be brought to equilibrium with the headspace of the vial; in the second step, the headspace is adsorbed on the SPME-fiber. Let define the equilibration time as the time necessary for the volatile compound to reach the partition equilibrium between the liquid phase and the headspace, and the extraction time, as the time necessary for the fiber to reach the equilibrium with the headspace. Both need to be optimized, even if it is not always necessary to reach the full equilibrium. The curves describing the area of the signal as a function either of the extraction time or the equilibrium time are of the same type. The first part of the curve is characterized by a strong slope, as long as the equilibrium is not reached and a plateau afterward. In order to obtain reproducible results, it is necessary to make the measurements in a region of the curve where the sampling error is minimized.
The extraction time depends on the coating of the SPME-fiber and on the analyte to be extracted. Using toluene (600 μg/l) as a model substance and the PDMS fiber with an equilibration time of 30 min, it could be shown (Fig. 3) that an extraction time of 51 s was necessary to reach 95% of the plateau. With other fibers, the time necessary to reach this plateau will be different depending on the process at the surface of the fiber [1]. The dependence of the extraction time on the analyte has to be tested in each individual case.
Different carrier gases may be used: nitrogen, hydrogen or helium. The type of carrier gas does not significantly modify the signal of toluene in water. We used helium at 2 ml/min as carrier gas. The flow rate also has a significant effect on the signal form: at too low rates, the peak becomes smaller and wider and is more difficult to interpret.
3.2. Equilibration and extraction time
With optimized apparative conditions, it was possible to test the other parameter affecting the measurement of a headspace. The headspace measurement takes place in two steps: in the first step, the solution to be analyzed has to be brought to equilibrium with the headspace of the vial; in the second step, the headspace is adsorbed on the SPME-fiber. Let define the equilibration time as the time necessary for the volatile compound to reach the partition equilibrium between the liquid phase and the headspace, and the extraction time, as the time necessary for the fiber to reach the equilibrium with the headspace. Both need to be optimized, even if it is not always necessary to reach the full equilibrium. The curves describing the area of the signal as a function either of the extraction time or the equilibrium time are of the same type. The first part of the curve is characterized by a strong slope, as long as the equilibrium is not reached and a plateau afterward. In order to obtain reproducible results, it is necessary to make the measurements in a region of the curve where the sampling error is minimized.
The extraction time depends on the coating of the SPME-fiber and on the analyte to be extracted. Using toluene (600 μg/l) as a model substance and the PDMS fiber with an equilibration time of 30 min, it could be shown (Fig. 3) that an extraction time of 51 s was necessary to reach 95% of the plateau. With other fibers, the time necessary to reach this plateau will be different depending on the process at the surface of the fiber [1]. The dependence of the extraction time on the analyte has to be tested in each individual case.
การแปล กรุณารอสักครู่..