Innovations at INTERPHEX Guide 2022 - 19

Figure 1. Installation schematic showing the Quantum mass spectrometer connected to a bottom integral freeze dryer.
typical installation configuration of the Quantum mass
spectrometer on a freeze dryer.
Results and Discussion
Testing using gas permeators show a linear correlation
between the Quantum mass spectrometer's measured
ion current and the injected 5cSt silicone oil PPM. In
this testing, the PPM of silicone oil was determined by
measuring the mass difference from the calibration tubes
in the gas permeators. The results are shown in Figure 2.
This test proves the sub-1PPM detection capabilities of
the mass spectrometer under consideration. However,
the temperatures used in this test to generate silicone oil
vapors are much higher than normally achievable inside a
lyophilizer. Hence, actual testing under vacuum conditions
in a lyophilizer was necessary to determine the capability of
the Quantum mass spectrometer for leak detection.
Figure 3 shows the results of the 5cSt silicone oil testing
using the Quantum mass spectrometer in the Lyofast3
freeze dryer. The mass spectra for three different oil volume
samples in the same 2.3m2
chamber were compared at the
Figure 2. Quantum Sensitivity curves for 2 types of silicone oils.
same relative time (t=21 mins after start of sampling) from
the start of the test. Figure 3 (left) shows the three scans.
It is evident from the plot that an increasing quantity of
silicone oil in the chamber corresponds to an increasing
max oil ion current. The 150 mg sample in this case shows
a peak value of close to 0.6pA for silicone oil. In similar
tests which were repeated with the same quantities of
silicone oil, plot 3 (right) show the PPM value derived from
the ion current. In this test, the sampling was started at
higher pressures of the chamber to allow for capturing the
evaporation of silicone oil. This can be seen in plot 3 (right)
where the PPM value initially increase with time, peaking
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Innovations at INTERPHEX Guide 2022

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