Wolf Heinz, Stauffer Tony, Chen Shu-Chen Y, Lee Yoojin, Forster Ronald, Ludzinski Miron, Kamat Madhav, Godorov Phillip, Guazzo Dana Morton
Packaging Technologies & Inspection, LLC, Tuckahoe, NY 10707, USA.
PDA J Pharm Sci Technol. 2009 Sep-Oct;63(5):472-88.
ASTM F2338-09 Standard Test Method for Nondestructive Detection of Leaks in Packages by Vacuum Decay Method is applicable for leak-testing rigid and semi-rigid non-lidded trays; trays or cups sealed with porous barrier lidding materials; rigid, nonporous packages; and flexible, nonporous packages. Part 1 of this series describes the precision and bias studies performed in 2008 to expand this method's scope to include rigid, nonporous packages completely or partially filled with liquid. Round robin tests using three VeriPac 325/LV vacuum decay leak testers (Packaging Technologies & Inspection, LLC, Tuckahoe, NY) were performed at three test sites. Test packages were 1-mL glass syringes. Positive controls had laser-drilled holes in the barrel ranging from about 5 to 15 microm in nominal diameter. Two different leak tests methods were performed at each site: a "gas leak test" performed at 250 mbar (absolute) and a "liquid leak test" performed at about 1 mbar (absolute). The gas leak test was used to test empty, air-filled syringes. All defects with holes > or = 5.0 microm and all no-defect controls were correctly identified. The only false negative result was attributed to a single syringe with a < 5.0-microm hole. Tests performed using a calibrated air leak supported a 0.10-cm3 x min(-1) (ccm) sensitivity limit (99/99 lower tolerance limit). The liquid leak test was used to test both empty, air-filled syringes and water-filled syringes. Test results were 100% accurate for all empty and water-filled syringes, both without holes and with holes (5, 10, and 15 microm). Tests performed using calibrated air flow leaks of 0, 0.05, and 0.10 ccm were also 100% accurate; data supported a 0.10-ccm sensitivity limit (99/99 lower tolerance limit). Quantitative differential pressure results strongly correlated to hole size using either liquid or gas vacuum decay leak tests. The higher vacuum liquid leak test gave noticeably higher pressure readings when water was present in the defect. Both the ASTM F2338-09 test method and the precision and bias study report are available by contacting ASTM International in West Conshohocken, PA, USA (www.astm.org).
ASTM F2338 - 09《用真空衰减法无损检测包装泄漏的标准试验方法》适用于对刚性和半刚性无盖托盘、用多孔阻隔盖材密封的托盘或杯、刚性无孔包装以及柔性无孔包装进行泄漏测试。本系列的第1部分描述了2008年进行的精密度和偏差研究，以将此方法的范围扩大到包括完全或部分装有液体的刚性无孔包装。使用三台VeriPac 325/LV真空衰减泄漏测试仪（包装技术与检验有限责任公司，纽约州塔克霍伊）在三个测试地点进行了循环试验。测试包装为1毫升玻璃注射器。阳性对照在针筒上有激光钻出的孔，标称直径约为5至15微米。在每个地点进行了两种不同的泄漏测试方法：在250毫巴（绝对压力）下进行的“气体泄漏测试”和在约1毫巴（绝对压力）下进行的“液体泄漏测试”。气体泄漏测试用于测试空的、充有空气的注射器。所有孔大于或等于5.0微米的缺陷以及所有无缺陷对照均被正确识别。唯一的假阴性结果归因于一个孔小于5.0微米的注射器。使用校准空气泄漏进行的测试支持0.10立方厘米/分钟（ccm）的灵敏度极限（99/99较低公差极限）。液体泄漏测试用于测试空的、充有空气的注射器和装有水的注射器。对于所有空的和装有水的注射器，无论有无孔（5、10和15微米），测试结果的准确率均为100%。使用校准空气流量泄漏为0、0.05和0.10 ccm进行的测试准确率也为100%；数据支持0.10 ccm的灵敏度极限（99/99较低公差极限）。使用液体或气体真空衰减泄漏测试时，定量差压结果与孔尺寸密切相关。当缺陷中有水时，较高真空的液体泄漏测试给出的压力读数明显更高。通过联系美国宾夕法尼亚州韦斯特康舍霍肯的ASTM国际组织（www.astm.org）可获取ASTM F2338 - 09测试方法以及精密度和偏差研究报告。
