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YY/T 0681.4-2021 English PDF (YY/T 0681.4-2010)
YY/T 0681.4-2021 YY PHARMACEUTICAL INDUSTRY STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 11.080.40 C 31 Replacing YY/T 0681.4-2010 Test methods for sterile medical device package - Part 4: Detecting seal leaks in porous packages by dye penetration ISSUED ON: MARCH 09, 2021 IMPLEMENTED ON: APRIL 01, 2022 Issued by: National Medical Products Administration Table of Contents Foreword ... 3 Introduction ... 5 1 Scope ... 6 2 Terms and definitions ... 6 3 Significance and application ... 7 4 Instruments ... 7 5 Security measures ... 8 6 Test sample ... 8 7 Sampling ... 8 8 Conditioning ... 8 9 Procedure ... 9 10 Report ... 10 Appendix A (Informative) Precision and bias of test methods ... 12 Appendix B (Informative) False positive guidelines ... 17 References ... 19 Test methods for sterile medical device package - Part 4: Detecting seal leaks in porous packages by dye penetration 1 Scope This Part of YY/T 0681 specifies the test method for detecting seal leaks in porous packages by dye penetrant. This Part applies to the detection of channel, whose package sealing area is greater than or equal to 50 μm, that is composed of transparent materials and porous materials. This Part does not apply to porous materials that are dyed due to wicking within 5 s; it does not apply to situations where the dye penetrant is not much different from opaque materials. 2 Terms and definitions The following terms and definitions are applicable to this document. 2.1 Wicking The liquid moves into the fibrous material. 2.2 Dye penetrant A mixed aqueous solution of a coloring agent and a surfactant, which is designed to indicate the location of the defect in the period before wicking (which masks the existence of the defect). 2.3 Channel Any undamaged path across the entire width of the intended sealing area. If conditioning is required, it is recommended to be performed in a standard environment where the temperature is (23±2) °C and the relative humidity is (50±2) %; the conditioning shall last for at least 24 h before the test. 9 Procedure 9.1 Method A (injection method) 9.1.1 Inject a sufficient amount of dye penetrant into the package, so that the dye penetrant can form a depth of about 5 mm on the longest side of the package. When piercing the packaging bag and injecting the dye penetrant, special care must be taken not to pierce or damage other surfaces of the package. It is easier to pierce in the position beside the virtual sample in the package. The sample will act as a bulge to separate the two surfaces of the packaging bag, so as to reduce the risk of accidentally piercing the two surfaces. 9.1.2 Visually inspect the sealing area through the transparent surface of the package. Observe the sealing area through which the dye penetrant flows, and the channel can be directly observed. For packages that are sealed on four sides, it’s at most 5 s for each side, and the total time is less than or equal to 20 s. The long stay of the dye penetrant will cause the sealing area to be dyed due to the wicking of the porous material, making observation difficult. If necessary, use a 5 ~ 20 times optical magnifying glass for detailed inspection. 9.1.3 The packaging bag must be rotated, so that each side is in contact with the dye penetrant. If necessary, add more dye penetrant to ensure that each side can be in contact with the dye penetrant. 9.2 Method B (edge immersion method) 9.2.1 Choose a container of sufficient length to at least contain the longest sealed side of the to-be-tested package. 9.2.2 Pour enough dye penetrant into the container, so that the dye penetrant can cover the bottom of the container, with a minimum depth of about 3 mm ~ 6 mm. If there is extra material on the outer edge of the seal of the tested packaging bag, such as the skirt for the opening, some modifications must be made to the packaging. Use a cutting tool to cut off the excess material from the skirt along the outer edge of the sealing area at a distance of 3 mm; be careful not to cut it into the sealing area. Cutting off the excess material will bring the dye penetrant close to the sealing area. 9.2.3 Immerse one of the sealed edges of the package down into the dye penetrant so that the entire sealing edge of the sealing area is in contact with the dye penetrant for a short time. This immersion operation is short, but it is just enough to completely wet the sealing edge. 9.2.4 Remove the package along the immersion direction; confirm that the entire sealing edge is in contact with the dye penetrant. Observe the penetration of the dye penetrant in the sealing width direction of the package from the transparent surface of the package. For packages that are sealed on four sides, it’s at most 5 s for each side, and the total time is less than or equal to 20 s. 9.2.5 If necessary, use a 5 ~ 20 times optical magnifying glass for detailed inspection. 9.2.6 Repeat the above edge immersion operation for other sealing sides. 9.3 Method C (drip method) 9.3.1 Pour the dye penetrant into an open container. 9.3.2 Use fingers or a paper clip to carefully separate the skirt of the transparent material from the porous material. 9.3.3 Insert the eye dropper or pipette into the dye penetrant. 9.3.4 Face the transparent surface of the package to the operator; drip the dye penetrant along the sealing side between the transparent material and the porous material. Make sure that the entire side is immersed in the dye penetrant. 9.3.5 For small packaging bags, slowly rotate the packaging, while continuously dripping the dye penetrant, until the sealing side of the whole package is in contact with the dye penetrant. If it is inconvenient to operate, drip on only one side at a time. 9.3.6 Observe the penetration of dye penetrant along the entire width in the sealing area of the package. For packages that are sealed on four sides, it’s at most 5 s for each side, and the total time is less than or equal to 20 s. 10 Report The report shall contain the following information: a) Sample information: Completely confirmed test material information, including but not limited to the batch number, source, date, time, location and operator of the test; b) Conditioning information; c) Test method: Method A, Method B or Method C; d) The dye penetrant to be identified, if the used dye penetrant is different from that specified in 4.7; The test results show that, when using the coloring agent that is specified in this method to test the package, one side of which is a porous material, the measurement confidence of the channel that is constructed of a wire whose diameter is 50 μm is more than 95%. It was observed in this test series that when using indicator dye liquid other than toluidine blue to test the bag that is composed of plastic film, the test performance is significantly reduced (the probability of detection of a defect is < 60%). Early-developed tests show that when other wicking reagents are used, the inspection capacity is obviously poor; based on these test results, the formulations of the coloring agents and wicking agents in this test method are specified. A.2 Edge immersion method and drip method A.2.1 Test example Laboratory studies on the edge immersion method and drip method in the standard were carried out in 2012. 12 laboratories participated, 7 of which tested the edge immersion method, and 5 tested the drip method. The defect is made by the wire of 50 μm that is artificially placed in a sealing area; after the wire is drawn out, a channel of the same diameter as the wire is formed. For 5 materials, each laboratory tested 50 samples (25 with channels and 25 without channels). Each laboratory reported the presence or absence of the channel. Put all the results into the table, and there are results of correct recognition, false positive and false negative. A.2.2 Edge immersion method test results A.2.2.1 When the edge immersion data of all laboratories are combined, the results show that these two methods also have a 95% accuracy rate for 50 μm channels. The 95% confidence interval ranges from 93.8% to 96%. Table A.2 ~ Table A.4 show the results of correct recognition, false positive and false negative. A.2.2.2 When using the analysis of variance to compare the edge immersion laboratories, the test results of the laboratories 6520 and 6521 are significantly different from those of the other 5 laboratories. This may contain other reasons causing a larger error rate. If the results of these two laboratories are not recorded, the accuracy can be increased to 98%. A.2.2.3 The remarks of laboratory 6521 describe the observation that some samples have a unique path highlighted by the dye penetrant, but only part of them pass through the sealing area of the package. These samples cannot be recorded as having channel defects. Because the definition of the channel is a complete channel through which the dye penetrant can pass through the entire sealing area. All partial channels in this laboratory are considered channels Appendix B (Informative) False positive guidelines B.1 Wicking The dye penetrant used in this Standard has strong activity and will quickly pass-through TYVEK or other porous materials to produce wicking. It will partially penetrate the sealing area and cause a false judgment as a test failure. The difference is that the channel defect in the sealing area provides a path through the entire sealing area, which will be found immediately when exposed to the dye penetrant. The test time is very important because it can distinguish between wicking and channel leakage. The test time is 5 s, because the penetration in the channel will be clearly noticed in the first few seconds. If the penetration time of the dye penetrant is 20 s, the wicking will be m...... YY/T 0681.4-2010 Test methods for sterile medical device package.Part 4. Detecting seal leaks in porous packages by dye penetration ICS 11.080.40 C31 People's Republic of China pharmaceutical industry standards Test methods for packaging sterile medical devices Part 4. Determination of breathable packaging staining solution penetration method Seal leakage Part 4. Detectingsealleaksinporouspackagesbydyepenetration Issued on. 2010-12-27 2012-06-01 implementation State Food and Drug Administration issued Foreword YY/T 0681 standard under the general title "sterile medical devices packaging materials, test methods", consists of the following components. --- Part 1. accelerated aging test guidelines; --- Part 2. sealing strength flexible barrier material; --- Part 3. Unconstrained pressure within the package of anti-sabotage; --- Part 4. Determination of staining solution penetrate breathable packaging seal leakage; --- Part 5. coarse leak was detected internal pressure (bubble method); --- Part 6. flexible packaging material printing ink and coating chemical impedance evaluation; --- Part 7. Evaluation of flexible packaging material with adhesive tape or adhesive ink layer; --- Part 8. coating layer weight determination; --- Part 9. constraint plate internal gas pressure method flexible seal bursting; --- Part 10. breathable packaging material and microbial penetration level test. Other parts will continue to develop 1). 1) conversion of the rest of the Test Method ASTMF standards for medical packaging. This section YY/T Section 40681 of. This section drafted in accordance with GB/T 1.1-2009 given rules. YY/T 0681 Part revised adoption ASTMF1929-1998 "seal leakage test dye solution penetration assay breathable packaging method". This part of the National Infusion equipment for medical Standardization Technical Committee. This part mainly drafted by. Shandong Province Medical Devices Product Quality Inspection Center. The main drafters of this section. Zhang Limei, Dong Dandan, Qian Cheng Yu. Test methods for packaging sterile medical devices Part 4. Determination of breathable packaging staining solution penetration method Seal leakage 1 Scope This section YY/T 0681 provisions of the seal can be detected between the transparent film and the formation of a breathable material with silk edge greater than or equal 50μm channel, and the channel position to identify the materials and procedures used. The one kind of dye liquor local effect on the sealing edge for leakage test, and Staining solution for a prescribed time after the contact, eyesight test staining on the packaging penetration. This test method is intended for inspection seal is formed between the transparent film and the breathable material edges. This test method can be maintained only for transfection Color liquid and can not make the entire sealing areas are discolored breathable material within a minimum time of 20s. Non-adhesive paper are particularly vulnerable to infiltration staining solution Through the impact, when using this test method must be carefully evaluated. This test method requires opaque packaging material for a good stain solution off. 2 Terms and definitions The following terms and definitions apply to this document. 2.1 Capillary action wicking Liquid moving into the fibrous material. 2.2 Staining solution dyepenetrant One kind of stain and a mixture of an aqueous surfactant solution, and is designed to take place before the capillary action (which would blur defective) of Period of time to indicate the defective parts. 2.3 Channel channel Small package seal across the width of the continuous open path, through which microorganisms can enter the package. The purpose of this test method is through Eyesight dye through observation, and was found to be defective. 3 meaning and application 3.1 or particulate contamination of harmful microorganisms can enter the device through the leak. These leaks often occur between the packaging material of the same or different shape Into the seal. Pinhole leak can also be caused by material. 3.2 Staining Solution program is only available in a standalone package seal leakage, and not to a plurality of small vent gas permeability of packaging materials found Drain, which requires other techniques to detect. 3.3 For the purposes of a particular package, what degree of leakage was only considered harmful, there is no consensus. However, since this test is To detect seal leakage, and any evidence of leakage usually deemed to have failed. 3.4 degree due to leakage due to different environmental conditions vary, the comparability of data between different test sites is unclear. because ...... 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