Designation: F 1929 – 98 (Reapproved 2004)
Standard Test Method for
Detecting Seal Leaks in Porous Medical Packaging by Dye Penetration1 This standard is issued under the fixed designation F 1929; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript supers cript epsilon (e) indicates an editorial change since the last revision or reapproval.
Standards:3 2.2 ANSI Standards: Z1.4 Z1. 4 Sam Sampli pling ng Pro Proced cedure uress and Tabl ables es for Ins Inspec pectio tion n by Attributes
1. Sco Scope pe 1.1 This test method defines defines materials materials and a procedure procedure that will detect and locate a leak equal or greater than a channel formed by a 50 µm (0.002 in.) wire in package edge seals formed between a transparent film and a porous sheet material. A dye penetrant solution is applied locally to the seal edge to be tested for leaks. After contact with the dye penetrant for a specifi spe cified ed tim time, e, the pac packag kagee is vis visual ually ly ins inspec pected ted for dye penetration. 1.2 This test method method is inte intended nded for use on pack packages ages with edgee sea edg seals ls for formed med between between a tra transp nspare arent nt film and a por porous ous sheet material. This test method is limited to porous materials which can retain the dye penetrant solution and prevent it from disc di scol olor orin ing g th thee en enti tire re se seal al ar area ea fo forr a mi mini nimu mum m of 20 s. Uncoated papers are especially susceptible to leakage and must be evaluated carefully fro use with this test method. 1.3 This test method requires requires that the dye penet penetrant rant have good contrast to the opaque packaging material. 1.4 The values values stated in SI units are to be regarded regarded as the standard. The values given in parentheses are for information only. 1.5 This sta standa ndard rd does not purport purport to add addre ress ss all of the safe sa fety ty co conc ncer erns ns,, if an anyy, as asso soci ciat ated ed wi with th it itss us use. e. It is th thee responsibility of the user of this standard to establish appro priate safety and health practices and determine the applicability of regulatory limitations prior to use.
3. Terminology 3.1 wicking—The migration of a liquid into the body of a fibrous fibr ous material material.. Thi Thiss is dis distin tinct ct fro from m a lea leak k as defi defined ned in Terminology F 1327. 3.2 dye pene — An aq aque ueou ouss so solu luti tion on of a dy dyee an and d a penetrant trant —An surfactant designed to penetrate and indicate a defect location in the time prior to the onset of wicking which could mask its presence. 3.3 channel—A small continuous open passage across the width of a package seal through which microorganisms could pass. It is the objective of this test method to visually observe the presence of these defects by the leakage of dye through them. 4. Signi Significanc ficancee and Use 4.1 Harmful Harmful biol biologica ogicall or parti particulat culatee conta contamina minants nts may enter ent er the dev device ice thr throug ough h lea leaks. ks. The These se lea leaks ks are fr frequ equent ently ly found at seals between package components of the same or dissimilar materials. Leaks may also result from a pinhole in the packaging material. 4.2 This This dye pen penetr etrant ant pro proced cedure ure is app applic licabl ablee onl only y to individual leaks in a package seal. The presence of a number of small sma ll lea leaks, ks, as fou found nd in por porous ous pac packag kaging ing mat materi erial, al, whi which ch could be detected by other techniques, will not be indicated. 4.3 There is no gene general ral agreement agreement concerning concerning the level of leakage that is likely to be deleterious to a particular package. Howeve How everr, sin since ce the these se tes tests ts are des design igned ed to det detect ect lea leakag kage, e, components that exhibit any indication of leakage are normally rejected. 4.4 Since leaks may change in size with differe different nt ambient conditions, comparisons between test stations are not conclusive. Therefore this method is usually employed as a go, no-go test.
2. Referenced Documents 2.1 ASTM Standards: 2 F 1327 Te Terminology rminology Relating to Barrier Barrier Materials for MediMedical Packaging
1 This test method is under the jurisd jurisdiction iction of ASTM Committee Committee F02 on Flexib Flexible le Barrier Mate Barrier Material rialss and is the dir direct ect resp respons onsibil ibility ity of Sub Subcom commit mittee tee F02 F02.40 .40 on Package Integrity. Curren Cur rentt edit edition ion app approv roved ed Jun Junee 1, 200 2004. 4. Pub Publish lished ed Jun Junee 200 2004. 4. Ori Origin ginally ally approved in 1998. Last previous edition approved in 1998 as F 1929 – 98. 2 For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@
[email protected] astm.org. g. For For Annual Annual Book of ASTM volume information, refer to the standard’s Document Summary page on Standards volume Standards the ASTM website website..
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F 1929 – 98 (2004) 8. Calibration and and Standardization
4.5 The dye solution solution will wick through any porous material material over time, but usually not within the maximum time suggested. If wic wickin king g doe doess occ occur ur,, it may be ver verifie ified d by obs observ erving ing the poro po rous us si side de of th thee su subj bjec ectt se seal al ar area ea.. Th Thee dy dyee wi will ll ha have ve discolored the surface of the material. 4.6 When puncturing the packaging packaging to allow injection injection of the dye penetrant solution, care should be taken not to puncture other package surfaces. Puncturing of the package is facilitated if it is done adjacent to a dummy device inside the package. The device will provide a tenting effect that will separate the two sides of the package, reducing the chance of accidental puncture of both sides.
8.1 These procedures procedures are suitable suitable for use on selected selected parts during receiving inspection or to verify and locate leakage sites for production control. They are not quantitative. No indication of leak size can be inferred from the test. 9. Cond Conditio itioning ning 9.1 Pac Packag kaging ing must be fre freee of con conden densat sation ion or any other source of liquid water. Water already in the seal defects may render them undetectable with a dye penetrant. If there is any indication that the package has been exposed to any liquid, it must be thoro thoroughl ughly y drie dried d at its typical storage temperature temperature before testing. 9.2 Test specimens specimens shall be condi conditione tioned d prio priorr to testi testing. ng. When no speci specific fic condi conditioni tioning ng requ requirem irements ents are give given, n, and packaging materials are moisture sensitive, a standard conditioning atmosphere of 23 6 2°C (73.4 6 3.6°F 3.6°F)) and 50 6 2 % relative humidity is recommended, for a minimum of 24 h prior to testing.
5. Appar Apparatus atus 5.1 Means of breaching breaching one of the packaging materials such as a small knife. 5.2 Dye Dispe Dispenser nser , such as an eyedropper or syringe for injection of the dye penetrant solution. 5.3 Microscope or optical loop with magnification of 5 3 to 203. 5.4 Fresh aqueous aqueous dye penet penetrant rant solution solution consisting consisting of, by weight: Wetting agent: Indicator dye:
TRITON X-100 4 Toluidine blue
10. Procedure 10.1 Clean Cleaning ing of packa packaging ging prior to dye penetrant penetrant application is unnecessary. 10.2 Inject suffi sufficient cient dye penetrant into the package to cover cover the longest edge to a depth of approximately 5 mm (0.25 in.). Allow the dye penetrant solution to remain in contact with the seal se al ed edge ge fo forr a mi mini nimu mum m of 5 s an and d a ma maxi ximu mum m of 20 20.. Channels will be detected within this time period but beyond 20 s, wicking of dye through the porous packaging will color the entire seal. 10.3 Rotat Rotatee the package package as necessary necessary to expos exposee each seal edge to the dye penet penetrant rant solution. solution. Inject additional additional dye as needed to insure complete edge exposure. 10.4 Visua Visually lly examine the seal area through the transparent side si de of th thee pa pack ckag age. e. Ch Chan anne nels ls in th thee se seal al wi will ll be re read adil ily y apparent without magnification, as the dye will rapidly wick into the area adjacent to the channel, making a much larger stain than the actual channel size. size. An optical device with 7 3 to 203 magnification may be used for detailed examination.
0.5 % 0.05 %
5.5 Other colored or fluorescent fluorescent dyes may be substituted substituted for toluidine blue but their precision and bias must be experimentally determined. 5.6 Because Because of the viscosit viscosity y of the TRITON TRITON X-1 X-100 00 the preparation of the solution is most easily accomplished by first taring a container with about 10 % of the required amount of water on a scale. The appropriate amount of TRITON X-100 is added to the water by weight and the mixture stirred or shaken. Once the TRITON X-100 is dispersed, the remaining water can then be added, followed by the toluidine blue dye. 6. Safet Safety y Precautions Precautions 6.1 Inje Injecting cting dye penetrant penetrant into a package with a hypod hypoderermic needle and syringe is a common method for performing this test. This practice can result in puncture of the skin with a contaminated needle and is therefore not recommended. Because of this hazard, it is recommended that the dye penetrant be dispensed using a flexible tube attached to a syringe through an opening formed with an appropriate cutting instrument.
11. Repor Reportt 11.1 Report the following information: information: 11.1.1 11 .1.1 A reference reference to this test method, method, 11.1.2 11 .1.2 Ident Identifica ification tion of the dye penet penetrant rant,, 11.1.3 11 .1.3 Metho Method d of inspection, inspection, and 11.1.4 Results: 11.1.4.1 Evidence of dye penetration penetration to the opposite side side of the seal or to the interior of the seal via a defined channel shall be taken as the indication of the presence of a leakage site. 11.1.4.2 11 .1.4.2 Evidence of dye penetration penetration thro through ugh the porous material through general wetting of the surface (wicking) shall not be taken as the indication of the presence of a leakage site. 11.1.4.3 11 .1.4.3 A qualitative qualitative description description or sket sketch ch of the leakage sites.
7. Test Specimen 7.1 The test specimen specimen shall consist consist of a complete complete packaged device dev ice if the test will be use used d as a qua qualit lity y con contro troll me metho thod. d. Blemished or rejected products may be used if the defect will not affect test results and is recorded prior to the test. 7.2 Dumm Dummy y te test st it item ems, s, em empt pty y pa pack ckag ages es,, or ed edge ge se seal al samples may be used for process control, product acceptance, or material development testing. 4
TRITON, a registered trademark of Union Carbide, has been found satisfactory for this purpose.
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F 1929 – 98 (2004) TABLE TAB LE 1 Results on Testing Testing Seals with Channels Generated Using 50 µm (0.002 in.) Wires Test Site
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2
three indep three independen endentt labor laborator atories. ies. Defec Defects ts were inte intention ntionally ally created in the package seals by placing wires of 50 µm (0.002 in.) diameter in the seal area. When the wires were removed a channel approximately the size of the wire was created in the seal. For each specimen set, 50 packages were produced, 25 with wit h wir wiree cre create ated d def defect ectss and 25 con contro trols ls wit with h no art artific ificial ial defects. The results are shown in Table 1 as (the number of correctly identified defects)/(the number of test packages).
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Sample 1: Breathable pouch; coated 44# paper With defect No defect
25/25 24/24
24/25 24/24
22/24 25/25
Sample 2: Tray with breathable lid; dot coated TYVEK A With defect No defect
25/25 25/25
25/25 25/25
24/25 25/25
12.2 The results results show that when using the dye penetrant penetrant as specified in this test methodology on packages with one side consisting of a porous breathable membrane there is better than 95 % confidence that channels in package seals, equivalent in size si ze in th thos osee ma made de wi with th a 50 µm (0 (0.0 .002 02 in.) wire wire wi will ll be detect det ected. ed. In thi thiss tes testt ser series ies,, sig signifi nifican cantt red reduct uction ionss in tes testt performa perf ormance nce (pro (probabil bability ity of dete detecting cting a defe defect ct <60 %) were observed with pouches fabricated with film on both surfaces and with indic indicator ator dyes other than toluidine toluidine blue blue.. Previ Previous ous testing test ing had shown significantly significantly poorer detection detection with other wetting agents. These test results are therefore specific for this dye and wetting agent formulation.
Sample 3: Breathable pouch; coated TYVEK With defect No defect
25/25 23/25
25/25 25/25
24/24 25/25
Sample 4: Breathable pouch; dot coated TYVEK With defect No defect
24/25 25/25
25/25 25/25
25/25 25/25
25/25 B 25/25
Defect Defe ctiv ive e 318 323 98 %
No De Defe fect ct 321 323 99 %
Summary Number correctly identified Total tested Percent correctly identified A
TYVEK, a registered trademark of DuPont, has been found satisfactory for this purpose. B Tested at manufacturing site.
13. Keyw Keywords ords 13.1 Dye pene penetrant trant;; flexi flexible ble packa packaging ging;; porou porouss packa packaging ging;; seal leaks
12. Pre Precisi cision on and Bias 12.1 12. 1 Bet Betwee ween n Jun Junee 199 1997, 7, and March 199 1998 8 tes testt pac packag kages es from four manufacturers were examined using this method by
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