Tightness detection scheme of pharmaceutical packaging - vacuum decay method

At present, the domestic testing standards for packaging integrity/tightness are mainly GB/T 15171-1994 "Test Method for Sealing Performance of Flexible Packaging"
.
Through the vacuum chamber of the testing instrument, the sample immersed in the vacuum chamber water produces an internal and external pressure difference, observe the gas escape in the test sample, if the sample does not produce continuous bubbles during the vacuum and vacuum holding, the sample tightness is qualified
.
By vacuuming the vacuum chamber, the sample produces an internal and external pressure difference, and the sealing performance
of the sample is judged by observing the expansion of the sample and the recovery of the shape of the sample after the vacuum is released.
The above traditional water inspection method can stably detect leaks with a diameter of about 20 microns, so what impact will leaks below 20 microns have on the tightness of the packaging and the quality of the contents? Figures 1 and 2 give the answer
.
In Figure 1, we can find 1E-3mabr.
L/s (0.
001mbar.
L/S) leakage rate corresponds to about the leakage hole diameter
of 6~10um right.
From Figure 2, this leak rate can increase the oxygen content in the package from nearly 0% to 1.
8%
in about 100 days.
In the case of 1E-1mabr.
L/s, that is, 0.
1mabr.
L/S leakage rate (about 70um), the oxygen content rises from 0 to 2.
5%
in about 1 day.
For pharmaceutical packaging with extremely strict sealing requirements, if the water inspection method is used, it is easy to ignore the infiltration of oxygen and water vapor caused by leakage of pores below 20 microns, resulting in deterioration in the quality of drugs during the shelf life
.
Therefore, the water inspection method is far from meeting the sealing performance quality control requirements
of pharmaceutical packaging.
Figure 1: Correlation between leakage pore size and leakage rate Figure 2: Relationship between leakage rate, storage time and oxygen content in the package Secondly, another defect of the water inspection method is that the test results cannot quantitatively produce leakage values, and the sealing effect is determined by manual visual inspection of whether continuous bubbles are generated, and the results are not reproducible and are greatly
affected by humans.
Finally, and fatally, the water test method is a destructive method, and all samples that have been tested for water are not allowed to be sold regardless of whether they are qualified or not, which will cause a very large waste of samples (separators), especially expensive drugs
.
Innovative solution - vacuum attenuation method tightness testing At present, various non-destructive tightness testing methods in developed countries such as Europe and the United States have been widely used in pharmaceutical packaging tightness testing, among which vacuum decay method is a universal solution
for non-destructive tightness testing.
The principle is to create a differential pressure environment
between the package and the measuring chamber by vacuuming the measuring chamber to the target pressure.
In this environment, the gas escapes through the tiny leak in the package and fills the measuring chamber, resulting in an increase in pressure in the measuring chamber, and the leakage rate
can be calculated using the known pressure difference, time interval, and pressure rise.
MK-1000 Vacuum Decay Method Tightness Tester Jinan Saicheng's self-developed vacuum decay method tightness tester adopts the principle of vacuum and differential pressure dual sensor method to conduct non-destructive testing, make it repeatable and automatically generate dossier files
after the test.
Precision pressure test system, test accuracy greatly improved
.
The products use pneumatic components imported from the world, imported pressure sensors, stable and reliable
performance.
The instrument has the characteristics of small size, low noise, no pollution, etc.
; The built-in high-precision flow meter is used to facilitate the verification of instrument linearity, and measurement and verification
can be carried out without disassembly.
Test process 1: Put the sample into the test chamber and vacuum the test chamber according to the set vacuum
degree.
In the evacuation stage, if the actual vacuum level cannot reach the reference vacuum level within the vacuum time, then the packaging has a large leakage
.
2.
In the holding stage, if the actual vacuum degree cannot reach the reference vacuum degree during the holding time, then the packaging has a leakage
.
3.
In the test stage, if the actual vacuum decay rate value is greater than the reference vacuum decay rate value, then the packaging has micro-leakage
.
Test process step schematic test application: vials, ampoules, infusion bottles, KF bottles, pre-filled needles, infusion bags, etc