GB2380803A - Vial integrity test - Google Patents

Abstract

The sealed chamber means 1 totally encloses the item under test 2. Sealed volume means 4 is in close communication with the contents of the sealed chamber means 1 by way of a connecting valve means. Sealed volume means 4 may also incorporate the evacuation means including other valves for the sealed volume, evacuation and ambient gas admittance means. Micro-sensor array means are incorporated within either or both of the sealed volume means 4 and the chamber means 1.

Description

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Via ! mtegrity test

Background Di : U. r\YI UUIIU The production of drugs and similar preparations to be stored in sealed glass containers, via ! s and suchlike, often invoives freeze drying the product in the u ; adH ; o : , I I ct I Ul,., 1 UU\t : J U lC11 I VU V ; I c : c' : : "c u : Y II I : : ; U It : fJI UU, -", l U I lIl vial, backfilling the vial with a low pressure gas and then sealing by stoppers under reduced pressure conditions prior to removal for testing and packing.

I u u-Ul, l-I L I L) l 1$ al IU IV.

The process is only economic when handling typically 50, 000 vials per batch, with the products on sheives that can be arranged to stopper under vacuum.

VVlt,, ; lilt : fJlU l" UII 11t : : v'='llldll"dll ut :' : Ifeal'Y lU lUf-JfJ""' : U ; IUt : : t Vdl"UU ; IL The purpose of the container is to provide a high integrity barrier against any contamination of, and a ready means of dispensing, the drugs/preparations.

'L Li-Urugs/'prepara'tl :-Ul-l.,-). e, C). C 4 Such vials, of 1 0-20-mill i litre volume, hold sma ! ! quantities of the dry material, I ; 1 1.- :-h----1-H=,-a-, art : all vacuum typicay mi ! ! igrams rather than grams, which are kept under a partia ! vacuum j I -BY I 1I11I (d II Id llld ; ; Y ; dfl ; , \tt,' ; : ; L,. ; dlt : : I'\. --,.., l UIIUt : : : 1 d iJdlUdl VdL. UUHl of typicafiy 10 kPa rather than normal atmospheric pressure of about 100 kPa.

I er'LLIL I i I I L I v R A I I I L Many descriptions exist dealing with the choice of giass and other materials, iviany ex'lsf. dealing w : tL I U-I. such as the material for the (rubber) septum, through which a solvent will be injected when the contents of the vial are finally being prepared for use. The

I I L t-. C L-e via ! conslruc'L L most important characteristics of the via ! construction are that the glass walls I L are considered rigid and the septum very nearly so, despite near atmospheric pressure differential across them after vial seal off during production process.

Testing of small ! ! defects in g'assware under vacuum has been traditionally l f. a ; ; t : lt : : \"'l I . Y "-'"IU : Vd\.,. ; ~ ; "'11111 UI ; lIdUllIUlld I performed manually by means of a spark gun, wherein an electric discharge coil or suchlike is passed close by the glass surfaces to locate defective vials

uue to enhanced spar"cLi I L L due to enhanced spark characteristics through the leak path in the glassware. Again there are many descriptions of this process and spark gun technology.

There are some major disadvantages with the spark gun approach when faced with testing a large number of vials, the principal ones being that it will miss large leaks causing the via ! to revert to atmospheric pressure condition, that it is not measurable, that sparks may damage good vials, that ozone and radio frequency emissions from spark discharges often exceed legal levels, spark guns need dangerous high voltages typically in excess of 20-30 kV and sparking from guns depends on relative humidity and atmospheric conditions.

The present invention does not utilise the small-scale leak location testing I-e small-scale leak location teslli-lycharacteristics of the spark gun approach but encompasses the whole vial, L without the use of electrical discharge and it's concomitant disadvantages, in a manner that is suited to high speed ( > 1 testlsecì production line leak testing. k I'-es"ec'production i : ne lea"tes't : i ;-iy-.

RA Mu ! tip ! e test chambers, each testing a single item, are often used to handle Lithe several per minute production rate for automotive components, but test rates for vials need to be > 10 times faster. Testing multiple items within a I-in a single chamber, which is the other approach, suffers from a loss of sensitivity to individual leaking items and a need for off-iine retesting of suspect batches.

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The pnndp ! e of the testing arrangements underlying the present invention is aiready common ! y used in other industries for use with he ! ium ! eak testing of ILI-helium leak'L-es'L"11-ly--u-ir t : auy 10-er ; ri'us'r : es'-r use w :-L I alr---J--niy used in o'LILI I U L I lu somewhat larger items, such as automotive airbag gas generator cans, as somewli L It it L Li I Li j : L-u. r, 4 1'19 AI-"-er novelties described in my earlier patent [Hoath 1394]. However some further nove ! ties and improvements sre possibte for the particu ! ar case of via ! integrity testing.

The present invention uses a sealed chamber around the via !, or around that part of the via ! enclosing the seaiing arrangement around the septum. To that fJdl UI U It : V ClI 1 ; : ; 111... 1 ; : ; ; 1118 I ; : ; ; t : ; dlll ! : : : i dll dl ! : : : i11 ;.., lll dl VUIIU U t : ; t : ; fJLUI,. I U U leH seaied chamber, another sealed volume is connected, having an evacuation seale J cLi Lil I I-Lt : U, lldv,, means or vacuum supply such that the known sealed volume can be prepared to a measured pressure be ! ow a reference absoiute pressure which is close to t-a measured p.. L) I L LL-L : that of ambient atmospheric pressure in the area for the vial validation test.

11 L t-ou'hal-c oz art-ib ; enl pressure, to The prepared pressure is often greater than about half of ambient pressure, to T Li-a'-when"'-e gas from'-L u I-e sealie-J volume into"-e volume ensure"L I L Li I Li I I t Lil li A." ensure that when the gas f ! ows from the seaied vo) ume into the voiume

around the vial, after a connecting means is opened, effects arising from the pressure ratio for choked flow do not slow the gas mixing. Another test rate restriction for the method is dictated by size of the gas temperature changes caused by the expansion of the gas from the seaied voiume into the chamber.

L, i-ti lu-e L CILUI U Li ICII lyt : b ii-e gas irru, ii le-'volume : n-o"he cIL-amL-e.uy Li ie expansion of L, itv-tva u I L I I tj Altematively, when running with prepared pressures appreciably less than pi tvbb I c--1-6 ! y less'-L I AI ti prepa, t :.'U-, apprecia-,. !-a.-, aboul ha !-'-'amlul L I I I U about ha ! f of ambient pressure, the ratio of the pressure changes experienced Ul en-pressure, Li I L ; I may be optimised by choosing approximately equal sizes for the sealed volume and the net chamber voiume, when the chamber contains a good vial.

Practical testing systems utilising these conditions for other applications, such rr-'rac'LLI : cai'Lc-sL : ng systems uLL ; li' : Is ; ngLLI I iu Li I I Li I Li-ese conditions-e-r o-L I I Ll-er appl : ca- : ons, such as for airbag gas generator leak testing, may utilise a series of calibration runs with items of a known ! evel of"good/bad"integrity to establish the practical test time settings for reprodudbie fina ! pressures and corresponding pass/fail lC ; ; :' ; l III t : : : II I I 1 VUUI... IUII ; : ; II dl fJl u dllU I... I C ; ; :' ; f-IUI I 8 f-Id ;, ;, t I I L-e"-eor-y 'LhresL ; i 10 L U Ll thresholds for the subsequent production runs. These ! ie close to the theory I I-anges expec. e--j-c--, LL-for the final equilibrium pressure changes expected for the voiumes involved, which therefore correspond to timescales needed to regain thermal stability.

Improvements in the vial testing rates are therefore restricted by the need to Improvements in ILI I L Li Li I t U LJ L lu wait for equilibrium pressures that are based on good/bad volumes alone, .. III-e greater"-an 4 per secc) n-' whi ! e the vial production test rates do need to be greater than 1 per second. spe, ---U' via,'integrity'esl : ng as a special One reason for the need to treat high speed vial integrity testing as a special case of the general ! eak testing is by virtue of the nature of the via ! itself, L- : L I'Ll-a we', !--je-c : ne-j being primarily a poory thermally conducting glass surface with a we ! !-defined small size which is reproducible from one good vial to the next vial tested, and small s : ze-wL I I I u u I t Lil another is the relatively stable and contro ! ! ed conditions for via ! production, in L, 0. Ou I I particular that they are produced within a freeze-drying process environment Lila"L I that has known temperature and humidity ! eve ! s within a close band of values.

Vial production is, however, sti ! ! subject to ambient pressure changes, and vial integrity testing does need a demonstrate and repeatabie caiibration method, in common with all the applications where such testing vaiidates final quality.

-rt~ ti L-ration lec ; hniques.

The present invention therefore includes the necessary caiibration techniques.

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Essentia ! features

The present invention improves the achievable rates for vial integrity testing.

A A reduction of the time for the test can be achieved by opening the connection valve rapidly and making a series of measurements of the subsequent sealed , e L L L chamber pressure during (short) times later, but well before attainment of the aLe-I equilibrium conditions associated with the standard equations of the prior art.

The relative sizes of volumes of the chamber, the sealed and via ! voiumes, I to and also the valve design, are critical to the technique because the fastest flow rates that may be encountered in the testing must not become so limited II I c : lll : : llldl. II UI : : 1 : : 1 1\"'1,) 1 l 1 1 1 III l l I I IUl I Ul Ul : : l.. 1111 : : u I I ll : : U by choked flow that they prevent the early detection of additional test volume.

The sealed volume might be chosen to approximately match the chamber volume, as appropriate to the choked flow limitations mentioned, although may bye largeur than this if the chosen evacuation level is also raised.

The voiume and shape of the sealed chamber should be chosen to allow gas The volume an'shape of'LILI I I u u JLL-E-L-ambe,--. r-ssure can be flow around the via ! contained within it so that the chamber pressure can be IL--e neL relative size o'this monitored by a measuring means and so that the net relative size of this chamber containing a vial is less than the internal volume of the vial, so that Li I w when the sealed volume is connected to it the gas should be able to flow w : tli 11 u without appreciate hindrance. n Pressure changes arising from temperature changes can be equalised rapidly by using sealed chamber walls of a good thermal conductivity - as glass vials have poor thermal conductivity-and by attention to the operating speed of the valve connection means between the sealed volume and the sealed chamber around the vial. At high speed the evacuation means for the sealed volume also needs a similar consideration to avoid extra temperature effects, so the sealed volume walls should likewise be of a good thermal conductivity.

The method uses gas pressure readings in the chamber volume before and after a connection means is opened between the sealed volume and the sealed chamber that contains, or partially contains, a vial. The sealed volume starts with a pressure well below ambient to ensure a measurable pressure difference between good and failed vials, and to check the test is also valid.

The final pressure value will ! be higher if the via ! or the seated chamber seat has poor integrity than if the vial has good integrity and the sealed chamber vacuum seal is also good, because of the additional air within the via ! or through a poor chamber seal whereby ambient enters the sealed volume.

The validation testing algorithm therefore decides between good and failed vials by computing the predicted final pressure for the given initial conditions on the basis of known volumes of chamber, sealed volume and vial and comparing these predictions with the observed readings for every vial test.

The evacuation means can be monitored with a suitable pressure sensor on the sealed volume. The starting pressure level for the sealed volume need not be close to absolute vacuum, which is an advantage for real vacuum pumping arrangements, provided that this pressure is known to be beiow a preset limit.

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The validation testing itseif needs to ensure failsafe resui s. The pressure sensors need to be checked for consistency and calibration for zero and span, which may be achieved by monitoring and checking the atmospheric and vacuum conditions within the equipment, before and after every via ! test.

Via ! integrity validation requires that the test system hardware provides a ful ! safeguard against power interruptions that might cause the via ! to be passed, so the reference voitage is uninterruptible or so linked to the testing control cyc ! e that it must be present throughout for a va ! id test signa ! to be generated. t t k L U t 11, 0 11 L I L LJ The technique reiies on pressure measurements made at high speed, which 1 1 le'ecil I ieS idi-i PF6Sc-LjF- :-- i-f-teasure u Lill I FJ f I !-.. are made with pressure sensors have very low intrinsic size, rather than with conventional capacitance diaphragrn gauge or manometer pressure sensors that are typically housed in cases severa ! times larger than the size of a via !.

Sma ! ! size sensors wouid normal be associated with low thermal capacity, and hence temperature fluctuations might masquerade as pressure changes. There will always be large gas temperature changes in the present technique, so it is quite surprising that this invention could work better than the slower, conventional, approach that actually waits for and uses final state readings.

However the avaiiabnity of arrays of combined sensors on siiicon-based

"microchips"'i ! ows use of muiiipie sampling techniques to average out variations in pressure, with temperature compensation essentiatiy inbuilt.

A . Ai-ioAheF a-vantage of'L-r---LLAnother advantage of these arrays is that they have a size commensurate with the via !, so that the hardware can be readily integrated for production. important features The pressure in the sealed chamber around the part, or around that part of

the via ! enciosing the seating arrangement around the septum, starts at a , ; I L., I L IL L value ciose to the reference absolute pressure, although it may be slight ! y higher than ambient atmospheric pressure in the area for the vial validation test by virtue of the effect of the sealing forces applied to the sealed chamber.

Typicaiiy, the chamber pressure increases by iess than 1% of this reference. Checks on the vacuurn pressure levei within the sealed volurne, by a pressure sensor means, can a ! so identify when the isolation vaive for the evacuation I e C at means or vacuum supply might ieak, thereby potentiaiiy nvahddting the test uec, ause'Llle pressure e" EF CL-ai--because the pressure e < ther changes faster or f) na ! ! y ts ! ower than expected.

"ru-----..---c--t-:--i---t-.-: t--.-- :j:.----L-II It : : tJl t : : UI t : : UI 1I t dll UJIt : : lll dU : : Uf-I ( JI t : If I U tt : VdllUdLlUl1 tt : : : l df t : : : d c : L't ; readiiy checked a ainst an absoiute reference pressure by measurement us < g standard sensor-mea s, such as a capacitance diaphragm manometer, U : :'IIIY : :'ldllUdl U : :. t : ; II : :. UI If It : ; df I :', :'Ul-II d : :' d U : lfJdl. : lldll\,.. t : ; UldfJl 1/dyrr I fIldf IUIIIlr, or by means of a mtcro-sensor array such as appiied io the two test voiumes.

Standard feedback methods to the evacuauon means can then be used to enSure that pie-test preparatton of the sea ! ed vo ! ume pressure ! cve ! conforms within the required range for the chosen voiumes for the via ! testing hardware.

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; tfOdut*ttU)) to the ufetw < n &

The fuiiuwing bnef ttf0ductiun & ofc) cfe ! CnCtid tu the nUtf'ibcnng System shown) n the drawings, which dep) Ct arrangements for ease of understanding.

More com 'tOr ! features, such as power supphes and controis, are not shown. yp : cal PF : OF ser-iscifs.

Figure 1 shows one typica ! configuration of prior art using pressure sensors.

I f I dl. JL. UIIIUldUUII L. f IdIIIU : : : 1 r r It : dllb \ I) lUldll Y : : : 11L. IVt : : : ; lIl Ilt : : : f II Ullut : : : r It : : : : : > t i. L J.

) SeC'e-1 U, eS' ) tally el-IC ; IC Li I I ef FFlea. L I) L Li IIL u The accumulation chamber means (1) tota ! ! y encloses the item under test (2).

The OnCntatiOn of the combined Ci'tBi'riber cti'td pan BS SnOwi'i is f'iOt Specific, aithough it may be considered favourable to !' both loading arid unloading. e Seal Cjl-l'L-e C ; ai-i-,', 7-C i-,-.-. s a [-isures'Le-s'L is i-lc), L-U, : Isflul wou oy til 11. L)-.. eai. ki) The Sea : or) the chamber r !' lear : s (1) ensures that the test is not disturbed, by preventing addltiona ! gas er ters the chan ber rneans (1) durli g an subsequ8rlt periods of pressure and terr perature stabiiisauO !') before the measurements.

IAA Fioure 2 shows-a other confiQurauon of the prior al t u inc pressure sensor-.

The accumulatin chamber rneans (11) partiaily encises tile Item unde test (2) by having a sufficient sea ! means (33) around part of the circumference of the item under test (2). The orientation of thE : combined chamber and part 85 shown is not specific, a ! though it may be considered favourabie for ioading.

The seal on the chamber rCleans (1) ensures that the test is not disturbed, by IAI preventing additional gas enters the chamber means (1) during aU subsequent periods of pressure and temperature stab ! ! isation before the measurements.

Figure 3 shows an integrated combination concept of the present invention.

The sea ! ed chamber means (1) totatiy encioses the item under test (2).

Sealed volume means (4) is in c ! ose communication with the contents of the I A 1 I-y Way i-, seaied chamber means (1) by way of a connecting va ! ve means. Seaied voiume means (4) may a ! so incorporate the evacuation means tnciuding other valves for the sea ! ed voiume, evacuation and ambient gas admittance means.

-in either OF L-OLL-o-C the Micro-sensor array means (4) are incorporated within either or both of the IAI- ! So-. c Cl. sealed voiume means (4) and the chamber means (1), also for ambient.

The orientation of combined detection and evacuation, chamber and part as shown is not specific, although it may be considered favourable for hand ! ing and for ioading and unloading if the housing (4) is even ! y distributed around the chamber axis (111) as an annuius as shown, or as one or more end disks.

~F aX ; Z ltiu-I-k I 1 1) as aii art r-or Fi Figure 4 shows an integrated combination concept of the present invention.

The isolation chamber means (11) partial encioses the item under test (2) by having a sufficient sea ! means (333) around part of the circumference of the A\ may alls item under test (2). Sealed voiume means (44) may a ! so incorporate the evacuation means inciuding other vaives for the sealed volume, evacuation I I A are and ambient gas admittance means. Micro-sensor array means (44) are I A A\ arl 11-e incorporated within either or both of the sealed volume means (44) and the . 5 IA alsor chamber means (11), a ! so for ambient. The orientation of combined detection and evacuation, chamber and part as shown is not specific, although it may iod (-I--igarl-u'u.-i !, oc-l-uing j !' tf-le be considered favourable for handling and for ioading and unloading if the housing (44) is evenly distributed around the chamber axis (1111) as an annuius as shown, or as one or more end disks.

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9-% rurllGUlut eAdlg e

t--I--------.-Iwie refere 'fce to the Fure 3 co ftOur tton, but th : s is not an exclusive I LU, ; i% 5-IYUI= LUl I I IgUldLIUl I, L) UL 1, 5 ! lUL d,' ! I Vt : tinpiemertation uflthi pre Ct' ! t tUventfOr,-co'td Others, wi'ttCh-do tnvOke-the lilt : : : : : > t : : : dlt : : : U I. A IdIlIUt : : : 1 1 l : : > t : : : 1 I I Ut : : : : : > I ! : : j1 It : : : U dllU I. VII : : > lI Ul. lt : : : U uy I. UIIVt : : : 1 IUVlldl V'J : U : Ulel U : vt QU U e r yul t XY VUI II IYU dL {V lX DUL u l a : N UL Cf t e xU u~ve ; t It : dllJ'fw'IU I dJ : IIllt : ; ; IcH VU ; UIII lA iUt : : : 11 lU L, UI ; IfJitat : : IY UlllcHI ; u ; VHjl UIIUI tt X lules g lel ItdLÙX Ut Ll l UI e : > UX 1k li~lVes lklul 1 d1 IU uLl Iel a Ws IlUt I utv sf lVuKe Ll le noveiucs of the pre er n't entton, Ut ! ! doubtiess becuf'fte avaxabie ! ater.

The sealed charnber itse ! f is designed and constructed by conventona ! - ~ ~ ~ ~l. ~~~L ~. ~'t r-~ u ~ ~ ~. ~ ~ Z ~. ~ u ~ ~. ~ ~s~.. ~s ~ ~l .. ~ ~. ~.. ~ ~-~. ~ ~ X 'I le avdleu Ul ldliluel lLaell la UealwUs seu CX u uUI saU uuLeu uy UUI Tvel LIUI IC test, arIU-, WI, Lr-l a-sea ; u-'esigi-I pi I. upul iy I I lea ! l ! Ldil lb Li It--PI I= !,-),-, Ul t : Ull ltV [t : : : ; ; Lld ; Z :, cHCOtjntcrcd, s ! S kriOwr ! to those prdCtiSd < r ! the rt of Qs tcc < t\ uctcctun.

L i--,'L i, ! e 1, e U, c ; I'l a i 1-1 L'i e r v C) 1 Lj i 1-1 e 1, r IAkpressljce Sei-ISC) F afray : !. s-U'I 1. u I-ef-i-lef-it ci I, *L ['-Ie ie-S'L U :-e, ;-je I, U- e- [- ! U-, d--Ul-I'LUut : : IUdUU dlJU UfIl dUt : : IdjJIUty IIllU dflU UUl VI lilt : : cUdU lldIIU') 1 IIUIII d UJ eabul e bel laul d11 c7y la uTube y uQuuleu LdJ L e ae~luu ul lal I lu < : : l VUIUI l le u C (IUSell LC) litaLC ; fl Lft (d fiel VUlUlilt', Ul Ui (c Sealua C ; flalllUtLI aOntdir nQ d QOOd-vtd !. Both 3r6 't-nttT'iScd to ctOw for fSt t St-Cyc ! t !' ! 0 !'c : tcS. i-i alF valve ri-iean ;-z an-uj c ; orrieclt : lort valve ali'ci-V-V-via ! Li-I VVllllt : If I l, f If ; t : l, U :'Y VdJV fJI t : : t : : : 11l d : : ll. dll dUUllIUI leU VUIUIIIJ L, ut IVt : : 1 ItlUlld ; be-Sodcd etnd uniodea ra idiy ! :' ! t0 dHd Out Of tho Scdd chamber from d aFe Cipef-16u', : li-i C ; F'-- ! 6 Lt--'1-111 : 1-1 : 11-111 : t-V Ll it", Ll ! IV ! 11 14=1 the 1.----------.------It- ! ,---I --I----------,-i--- :-.--I n0w v f th6 -ai es d 'c SO- Oi'fSti'L. Ctcd, d- to -ult ! ! I' !' ! : t ii' ! 6 05 f L 0w i' ite th t Ii I lIlI : : > I t : fJt : : : l. l I uUldH leu UIIIY f. J1 t : : : UI t : : : t : : : II ; : ; V 111t : : : dll : :' dl lilt : : : Uldlll\IIIY f. lUf l, occur wisF ! ths Vcvs ro o &commat; ed, ir ! order to rrunirni56 the thcrrria ! cscts.

Whiiti th6 CO !'i !' ! 6Ct ! !' v3 ! v6 prcSi'ttS c ! srnd ! ! ddditiOrid ! v0 ! u)' !'t6, OOrivOi'itiOi'id : I I UlIlel WVI u ; :' lY ;' : ll. dllY ; JU, vvu r d, uy IIIt : : dl I VI Il : : ; VWI I I. Ullllel. UVII lV dllUlIlt : : : 1 vdCuum vcti es wi h ! biaf'tked ff ! n ! et puf t mo b used with- adva taoe as the cornp ! et6 seaSed.'u ! u < Tte and cunneciing vaive n' : ea < 'tS. Fu < 't !') o' advat'itaQe ! < ' ! this respe t tS oblained using pressure sensor means at the biankinQ port, or b "teeino"it into th va !-ve of the evacuation mea s f r the-sealed vo ! urne.

Ti'tC-seaied vo ! ume is evac ated to a pres & ure euuai to !') -! f ar tbent-pr ssure, I lit : : : fJVWt : : : 1 UfJfJ'It : : : : : ;, ; :'IY'ldl WII lilY dllU lilt : : 1.. 1' Vl. t : : : : : > I. VlllI VI : : > t : : : YUt : : : III. t : : : IVI lilt : : : u : uy LeeC ly 1k U Ult ve : lve u L e eVcuuct u ece a ul Ll le atc eu vu ull e in other worls typicay 50, 000 F , by means- f its o1n connection to another chamber of dentica ! size which has been pre-evacuated to vacuum ! eve ! nn-, a a !-. solute T. 1-iese aff & ,--''Or-,-I L,-e va ; vmeans ihemseives, with t !'te < r ports beino connected if' ! a chain-wise fashiO !' ! between- hc seaie hamber and the con en i nal e acuation pump e n-.

< < e power suppiies, siona ! w'irinc and the process coritro ! secjuence for the va ! ves are converitonaS, but the pressure array Stonai process < no iUvoives ti'e co paris n of the pres: re-tirne-sionature for each via ! t st eo be compared with the resuits for kit n oo d and bad via ! s, and fauit con itions f r a poor seatCu-chamber sea ! an empty sea < u chamber (no v'iol pres rit), and poor Vetiv seetib LtHween seaid chctfftue), SMetied voiuf ! e < nd evauue < !. iot ! meanN.

The hardware is arr n ed to provide a fan-safe in ica ionlf r on good i !ui Subject to vo !) d test conditions, ! !' ! CSud ! no presence of power and a canbrcition.

The via ! vahdation caiibr tion mea s i - ffe tiveiy provi ed eveiy test by use of the k own v iumes of the seaied v iume and evacuation m a s and the pressure arrays on the seaied chamber and the evacuation chamber means, when-c nnection v rves between a ! ! thre voiumes are simuita eous y open. preSSui~2 i~i~ays Ui7 the S al d CharniU r anu the eVc7CucstiUi) WharnUer meai S wi7ei-E oi-li-lCiiUi-S VaiVe iJi : iweei- eii tih ; ~ei : UiUG eS cg~e S ; ; ML-leuuisiy J2 ; ... S, pi Vbt : f IL,", Ul"UWt : l dlU d L ; dllL) i EALIUI 1.

I I I e V : l a ;-) ia 1 : 1 U'a'L 1 : C) i-I c ; a, : [ LW-FaL I U-1-1 1-11 f-C C-1 1-1 b-I-b I---lt t- ; L-,'L 1 :-V. t :- :, l-y--P 1-U--V- : 1-Uj t :-U LL-). Y.-U. of, the known voiumes o-1 ; the seaied vo'lume and evacua-L ; Ion means and the 1 bt :-i : llt : U U ldt I dt JU Li IV t : VLIQUelLIL) t I tl l : 11 I fUtVI I I l (ddl Iz,

Claims (1)

1. CLAIMS vL^gi'iiZ 1 A device thai totally encloses the individual seated product under A-JE) II : - I ! n-l- 1%, i Li I it i% Ai iUu 1 %-4 Hi Ul I f test with a sealed chamber connected by a valve means to a seated volume with evacuation and ambient gas admittance means including micro-sensor array measurement means for ambient gases entering the seated volume during a short test period whereby the presence or absence of a seating failure can be deduced by reference to the results predicted for the measurement.

   2 A device that partial-endoses the individual sealed product under w h e i'J'Liv% ie Ui i., E) ci If 1 1 C41 ILA I UvU ti ; U L,, y i UiUi Ut iL ; U'L ! i-i-U tes : U : IiLs +Ll ! le +LiL-ia+L 7p-a i--LL : i, a 1, If-y-e i-i i-, it U. Z-, ; a %-2 L i i t-V i : i-i-Uj : i-, d, i : AAuali s : %--, aliedHi % J,, U.-IL Ut 1%. 4-It u 1-ambel, 1 acL- : e, : e +he same obje-" :-., ie as L ILI-aseale4cLi Les"w : L 1 1 Lc) iii v L , ICAII i i A LI L) u a r e s t r : l c L q--f%-A ! F o i 'L : i w. 1-1 o 1 ; the inu' : i--v--'Idual suu-lleu'pro,-uut, L.

   A test with a sea ! ed chamber to achieve the same objective as daim 1 but over a restricted portion of the individual seated product.

   3 A device that has been specifically shaped for the dimensions of an il : : < : ol III i < : > d, U I. "lldiiii. A : > í i I. "i liö e ; i I ; :'áiliö V I. "iiV á ; :' "iáiiii individual seated product to provide optimum volumetric capacity of the seated chamber means and seated voiume means and equipped with connection valve means permitting only minimal i. ! ierrriai eiiecs on openi g uetween seaiOu Ci ia-ier ai\-i seaiOu vOtUmo an\ ss of) terwise consistent win i eiti) er Ciaim i or Ciaim -.

   VviUiiiC di U d ; : s Uii iir+tiSU wvi i ; ti ; > i.-ri ii. ftiii i B : iii ivi widiiii i vi uiciiiii/.

   4 A device where the product tested is a via ! and following daim 1 or r -) -Ui C.

   5 A device where the product tested is an ampoule and follO'vving ! . ;.-- < -- ;- *') 5 A device where the seated voiume evacuation and gas admittance Iii dl i" I ; :' ; ;'öjJdl dit : Ii ï I I II I "ödíöU I. "lldi i li. Jöl Ii ì ; : ; d "VI I. "ldil I I i means is separate from the sealed chamber means of claim 2 prc)'---L--j I if A device where the seated votume evacuation and gas admittance means is separate from the seated chamber means of daim 2 ; ; :' ; ; ; : GiIt ; U "I lal i iUIVI 1 i ilVai I ; ; :' Vi "jeiil I I I - I a ; m 8 A device vhere the seated volume evacuation and gas admittance means is separate from the seated chamber means of claim 3 A 1"- h UöVII.,, \ : i Wi Il ; ; : i \ : i ii It : ; :'l : : dlöU VIUi i i\ : i t : VdL. UdliVI i i IU \ : jd : : : ; dUi I liUdi I"ö 3 A device where the measurement means is separate from the i I löôi i ; :' di IU li i i i löd ; :'UI \ : II i löi Ii i i iöól I ; :' ói ö < : > I : : í-idl dLt : :' i I VI i I II it ; :, t : ; diöu i-% UU v i It I Li I I % A V% Jluifle- evacua'LIUI i ai iU YCA-,., C4Ui 1 if LLO] i ;, V, seS) e < j C) iamer means o < daim) 10 A device where the measurement means is separate from the seated chamber means of daim 2 1 i n device where the measurement means is separate from the seated chamber means of daim 3 12 A device where the seated volume evacuation and gas admittance means an'-i u) &num; measurement means are separate irom tiie sea) eu chamber means of daim 1 ! iuiii Lii'V ZIIVC4i--U ;-IiiC21iiUt--i iiii-ICLiiil Ui kliCA-iiii 0 A-J-I i-% Uu i I ietizi V ; ce WL e iiuill Li I ; LiiU ill%--dbUit-. iiii--iiL iiit ; ; aris s sepaidt , 3 , a 1 e-u4 c ; iL i a m ! k l-ir lr inia a 1-1 s : % Ia ; l m'I n A i u i--u4ev : ice'the r,-ieasuremel^t+L i-I : 1,- > Z-, epa, aLe irrul i i Li IUu If-er or cia :- & eale J cariILU i-i A Aev : -r-% u \f-Vi li--i i--Li ie i i it-, CAZUi t-, i i it-, i it i i i% Vc2i is : ! o-epairC-4L-U i Li iU I U f iC-Ai i I I ! tV4 : 2i i, : ? Ul kIC-Ali i i ID i i-% Uvvi i i--i ii L i i i-,-b 0 c-, i u-, V : % j i u-1t I e e I u jca, ca% At I if LLc ; ii CAI Ily CAf IU'ri a a s u I f---1-iL-i i-i U-C-Ai-i,-) iri--Ul-i I cham :-uer r-rieans oT ciairn i

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   13 A devicB \tvt'Hre the seated \iotume evacuation and gas admittance means and the measurement means are separate from-the sealed chamber means of daim 2 chamber means of ciaim 2 means and the measureme t means are separate from-n ie sesieu charriber iTiesriS of ciaim 3 15 n usviCe in'Wi iiCii the messuremeut means Oi Cisim i are srrsnQeu ss srinUiai or iiSK secnois aouL n ie common sxes Oi n ie seSie charribet-and seated voiurne means 16 A'jsvics in which the m655'Ji'&commat;ment mesns Ci CtS. n* ! -srs srrsrte'j as annufar or disk sections about the common axes of the seaied as annular or disk sections about the commûn axes of the sealed Ci iSiTiter sriu sesie vCiuiTiS rTtesriS '7 Ai-.. : . : ... t :-Lt < ----.-.-.. . --t . - . J J. :-- --.-..-..-J t/-t UCVi ii i Wi iit i). t i ! ! iie < a & Ui S ii ti. itiCtt t \ ) 0tn) < a C et t eti tCU c'riamber means a] claim z -- )-e-J'-t --' -t--lL---------. ft----t-i C ! b ai ti ti tai Ui Ui0t\ bc U ) & e) L"-'ui. L) ic'-.'-'i i ii ! iUi) dXc : & ui Li it ; caic : chamber and seaied volume means %-, i icii I iut : i i i itdi i, Ui iidii i i D ) U/-t'-i w iS ii i < V) iii i i. i io i i icaUi Si i ii ii. i i i'SCii i. ! -aii i !-r a ! S eo i c4i iM'-i r-~ % a v i%, t-, ii i VVi iii-i i Li i'Z ; 1 i iZciUi Vi i it'i iL i i iu--ii iZ-y Ui, ic ; iii i i i cUi i--C4i i c : ti ijil ; u as ar'tnutar or di & k sections about the common axes of the seaied CitaiiiUt ? ! dtiU ccdicU vJiiJiiic iiicaii X n A UvieG ig | wii-"cih'ha r* > , aSüremmcni l,, çars 3sr a > ; lll C a, C ! al rQi Wg as-irr, bi, a,- ;--,-d, |si'sectivris abcçit t,-ie cvilmsi, axes vF the se < c, ss snriLiiSr or \iSK seci. ions SijOLit u iC cornrriOr ! sxes 01 Li ie se3iS' chamber and sea ! ed vo ! urne means . /-t'- < &commat;ViCB in Wi iiCi i the measurement means Ci CiBim c sre srrsriQe as annuiar or disk sections about the common axes of the seaied Ci iSrner 3n seSie'v'CiUme means êiwu i. i-YVi ;, $,-ie", asLirç"earis ; ir vl > llil'Qre Qlrci. ^ > iiPX uS ai l r or diis, SeCtiui] S abou. tiLiG Gi-in] i-i tsci ; I th sepci i as arit*itj ! ar or disk sections about the commori aAes of the seaSeu chamber and seaied voiume means vi iûi j iUCi ûi ìU úiu Vi.. JiUII i\ : ; i i Î\, ; û. i i0 as af-it-iu lar or-U- ! : 1, 5 ! r-I seG'Lllcji--is a'L-) ou-'t-'Lll,-ie c ; of i-i Ul Li luseaieu L.. ! h uöv tvtJ ìl i yvi iivll.. i jë I í Jt ; GiUi ÖI i It : ii Ii. i í iei̲ i Vi \.. rIUII i I I oi ç cil i di íÇ\.. A I %. A -v i I'L d ; :, è : : ii Ii iuidi Oi Ui ; :, i'.. ; :, ëi,. ; lIUi I ; :' diJULll U lë i. "UI i ii I iiJi i dX ; ; : ; ; ; : > UI li iç ; :, çdidU chamber and seaied vOlume means ar-id sea ! le-U-1 vcj ! lur-f-ie r-f-iear-i. 5 as annuiar or disk sections about the common axes of the sea < ed iiaiiiijci 0))'-i bcaicU vUiuiitt ? iiicaiio 23 A device in which ths measurement means of cisim 3 ure srrsnged as BnriLii r or' iiSK ssctioriS Sicut Li ie ccrnmcn axes 01 ti ie sesc û Gii ii iUiGii Vi \.. ii. jj\, C ; \... oUVi i ûvvui.. li iG i.... A' ; ; i ii i iVi i Q . \J vi li i\ ; ; \J < Ai\ ; : ; y ;, Ii ialt-ingLeir v I if I VVI li IZ-I i-I u et f :, ; e I Ll l-I I I LAI i i% L ; ul ii-% if l"lll I I Gil i Ui i : A Eis (311 ii-it-Jidi Ui UIDK ULlUi i,) CIUUUL ii it : LUL-I liliui i dai : o Ut Li it c chambef and sealed voiume means I) n A-J 24 A devi e tn vvhich the m asurement meanslof c ! a < m 1C are L'"r h uc ; v I\", ç ii i Wi iii. "i i U lë Illçd ; :, UI t : : i i iëlli. i i it : : di I ; ;' vi i. "idii i i I v dl c ; arrange as annular or disk sections about the common axes of thE.

   %, i idi i iut : i : ii iu : ptii : ; iitju vuiui i ii : i i iijeii i" :, A AF Z-li v I Ili It Li 2'C, III Cd Mi lff-i iL Iiit ; CAii, % ii C'i 4t ; u %. A I iU Ui ti Ai i C i i C--at- ? nu ! ar r e4 ; c, ! 41-zm-4 & I-- --O I If I I I % l iFX % Li I f r-A L Li i ii i ii i iUi i CiAU. : > Ui Li ! U s Si Ci iSiTi sr sn seSied voSume i-i05ns - \ : > \ : : ; úi\ ; : ; U \... oi iüi i iU\ : ; i üi iU, =, c ; aiC ; U vViUi i iÇ ; i i iGûi i i-% utt'V ii. ii i Vvi iiui i ki it ; i i ltd : pui ti i it ; i iL i i itcii iD Ui iidii i 1 cii t. : aintc2-1-igeAU-Us % Jlr-J*. l- -o : : + + ! -. c LL-UIOK CV%, Li% Jl 10 CtL/UL Li IV % iii i ii i iUi i CiAtZ3, Lii Li ii-sa ! e :-4 e- !- L i I I I C 4 1 % A V % * I U I I I I I A % i I CA I I I k-a

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   T A- ..-. ... : L. jH..--.--l--*--. r-'.- - < - -Lv 1\ ueV n.. JG II t VVI If\... lJ I lIlO. Ilod ; ;'Ui t : ; i i ioi Ii i i I'VOI Ib VI vlOlll1 I I cii c srrai"t'5 aS anrtuQr or tSK 5cCi. iort3 at-yO'-x. n conimGi ! 5Xc : 5 0 u ! ZO cievice ir-i which Lhe irleasu en ieni n-ieans ui Gia"-rl vi, cii~ 25 A device in which the measurement means of daim 12 are . j'-' (. I'-4 VI IÚI I U, J\JI UI ! \. A '-'Ú (\' ; \. A Y \. JI\.. U I 10 ! IIGUI h. : 1 2ô A aevice in which ihe mea : : ; ufemeni means ûf ciaim -í 2 afe voiurne means -/"\ U v i < ) t t-YV) tt t (.) i h tti ) t to tL < t tCCt) i i icttt it t \- Ctt C ? I'Yyi ii%, i I Li ii-, i I t- ; i I ivi it I I ivc4i io . ii \, icaiiii i, : ( : Ait,- !---.vUiLtiiic utcatia vuiui i ilc I I iticit io VUiui i Id Illdeu I ; ;, 2ô A device in Wrllcrl { [ ;Ie measurement means of Ciälrfl í 4 are 4/A dbvi ig ≈YVi i tl ie i I, eaSi Gl I IGI li. I I IÇCii IS Vl. a. i"I ç a G CÁI ì GH I ( ; \. A û0 di Ii rUiúJ VI YI (\. ""li\Ji i GiUV,... H LJ Ie ; aAi vi U iG \ : ; C ! i ;.. ; vuiUi e m ans z A UGVCE iil willer} r~neasul~emerli. rrleans UiT eiairrl i4 aire a e i i i y 9 u G S i i i i I bi i a 0 v i u {S r \ S e 9 t i v i S c i v G u t t 0 &verbar; a x i s v t t h ç s 9 ci (9 v VÜ6G riáiis