Leak Detection Results for Glass and Plastic Vials Subjected to the Effusive Procedure after 7 Days and 30 Days of Storage. Leak Detection Was Based on a Change Greater than 5 Torr between the t0 and 7- or 30-Day Time Points. Values Show the Number of Leaking Vials over the Number of Total Vials Tested for Each Sample Set
| Storage Temperature (°C) | Sample Set | Effective Defect Diameter a (µm) | Fill | Number of Leaking Vials Detected | |||
|---|---|---|---|---|---|---|---|
| Days of Storage | |||||||
| Glass Vials | Plastic Vials | ||||||
| 7 | 30 | 7 | 30 | ||||
| −80 | Negative Control (unmodified) | None | Empty | 0/10 | 0/10 | 0/10 | 0/10 |
| PBS | 0/10 | 0/10 | 1/10 | 0/10 | |||
| Microwire | 20 | Empty | 3/3 | 3/3 | 3/3 | 3/3 | |
| 41 | Empty | 3/3 | 3/3 | 3/3 | 3/3 | ||
| PBS | 1/3 | 1/3 | 0/3 | 0/3 | |||
| 64 | Empty | 3/3 | 3/3 | 3/3 | 3/3 | ||
| PBS | 0/3 | 0/3 | 3/3 | 3/3 | |||
| 80 | Empty | 3/3 | 3/3 | 3/3 | 3/3 | ||
| PBS | 2/3 | 0/3 | 3/4 | 0/2 | |||
| Laser-Drilled Defectb | 2 | Empty | 3/3 | 3/3 | — | — | |
| PBS | 3/3 | 2/2 | — | — | |||
| 5 | Empty | 3/3 | 3/3 | — | — | ||
| PBS | 3/3 | 3/3 | — | — | |||
| 10 | Empty | 3/3 | 3/3 | — | — | ||
| PBS | 3/3 | 3/3 | — | — | |||
| Gross Control (30 G needle) | 159 | Empty | 3/3 | 3/3 | — | — | |
| −20 | Negative Control (unmodified) | None | Empty | 0/3 | 0/3 | 0/3 | 3/3 |
| PBS | 0/3 | 0/3 | 0/3 | 3/3 | |||
| Gross Control (30 G needle) | 159 | Empty | 3/3 | 3/3 | — | — | |
PBS, phosphate-buffered saline.
↵a Values shown for the microwire sample set refer to the outer diameter of the wire; see Table III for accompanying effective defect diameters.
↵b For the PBS-filled vials, leaking vials were detected visually and not by headspace measurements due to glass fractures forming across the laser-drilled defect site as the vials warmed up to room temperature.