Text

Provides 30-day Rept Re 980112 Discovery of Corrosion,Paint Peeling/Blistering & White Crystal Formation Between Inner Container Lid & Outer Container Lid of BU-7 Fleet.Listed Info Included
	ML20207E066
Person / Time
Site:	07109019
Issue date:	02/10/1999
From:	Vaughan C; GENERAL ELECTRIC CO.
To:	; NRC OFFICE OF NUCLEAR MATERIAL SAFETY & SAFEGUARDS (NMSS)
Shared Package
ML20207E074	List: ML20207E066; ML20207G790;
References
	REF-PT21-99 NUDOCS 9903100142
	Download: ML20207E066 (77)
	v • d • e

{{#Wiki_filter:. t GEHuclear Energy C l L February 10,1999 Director Office of Nuclear Material Safety & Safeguards US Nuclear Regulatory Commission Washington, DC 20555-0001 i

Subject:

Reporting Pursuant to 10CFR71.95 and 10CFR21 ' i t

References:

(1) Docket Number 71-9019 { (2) NRC Certificate of Compliance 9019 for the Model No. BU-7 Packaging 5 Dear Sir. On 1/12/99, BWX Technology, Navy Nuclear Fuel Division (NNFD) in Lynchburg, VA, informed GE in Wilmington, N.C. that during a routine inspection of their BU-7 fleet, they discovered corrosion, paint peeling / blistering and a white crystal formation. These conditions were observed in the area between the inner container lid and the outer container lid. This is the ) location where the phenolic foam insulating plug is located. Photographs of the as-discovered 1 condition are provided in Attachment la. Additional details of the specific conditions found are ' described in Attachment Ib provided by NNFD, dated 2/2/99. Notwithstanding the NRC Statements of Consideration dated September 29,1995, pages 71-SC-12, and 13 that place the reporting responsibility on the shipper, GE has assumed the reporting responsibility based upon comments and suggestions made during telephone conversations with the NRC, BWX Technologies and Eco Pak. This was decided because we are the owner of the certincate holder, although we are not the manufacturer nor do we own or possess any BU-7's. Shipments weit not taking place with the packages at the time of this finding.. j \\ i NNFD stated that their current fleet of BU-7 containers had been purchased in the spring of 1996 /' from Nuclear Containers Inc. (NCI) in Elizabethton, Tennessee. All of these BU-7's were / . fabricated within a 6 month period and no abnormalities were noted by NNFD during their inspections and quality related activities. q\\ \\. 9903100142 990210 PDR ADOCK 07109019 4 3 PM 2 LTIOGO

i Director Office of Nuclear Material Safety & Safeguards - February 10,1999. Page 2 of 3 NNFD reviewed their BU-7 fleet to determine if there was a difference in the population. They stated 6at there did not seem to be a difference in the BU-7's physical condition: (1) based upon storage location such as trailers out of the weather in uncontrolled atmosphere, Sea / Land containr.rs, and one in an area that was atmospherically controlled or (2) those containers that i were storing SNM and those BU-7 that were empty. The BU-7's that had been loaded eighteen months prior to this event were opened for inspection four months after their closure, and only minor corrosion was observed at that time; however, =athia: approaching a condition that would constitute a rejection of the package. Therefore, it had been fourteen months since the containers were last opened for inspection. NNFD also stated that no shipments have been made with BU-7's in this condition, and there are no plans to ship the existing BU-7's. It was also determined that the BU-7's at NNFD are the only ones in existence fabricated by NCI, therefbre the problem population is believed to have been isolated and controlled. As of 1/18/99, approximately 15 BU-7's had been opened and all exhibited the same general degree of deterioration. NNFD noti 6ed their on-site resident NRC inspector of the situation on 1/13/99. As a result of this action, NRC management was informed of the event, and contacted NNFD for further information. On 1/20/99, a BU-7 was cut open at NNFD to inspect the condition of the inner wall of the outer i and the outer wall of the inner. Present were representatives from the NRC, Eco-Pak, NNFD (who cut open the container) and GE. The conditions on the inner metal surfaces, that were in direct contact with the foam, contained surface rust that did not appear to diminish the wall thickness (see Attachment Ib). - Notwithstanding 10CFR71.43(d), the physical conditions of the packages indicate that these requirements were not met in that a chemical reaction did occur between the package components. The condition is not believed to have had a significant reduction in effectiveness of the package ined at the time of observation, however, over time, the condition could continue to deteriorate. NNFD has stated that they have attempted to evaluate the condition as required by 10CFR21, and concluded that they cannot determine if the wrrosion constitutes a substantial safety hazard. At this time, GE does not believe the condition of the BU-7 represents a substantial safety hazard and therefore, is not a reportable situation under the criteria of 10CFR21. Eco-Pak obtained the following information and on 2/1/99 forwarded them to us:

1) A report dated 2/1/99 from LEIS to Eco-Pak that described the analytical processes used and the test results. See Attachment 3.

2) A letter dated 1/29/99 from Schenectady International, Inc. to Eco-Pak provided two volumes of a 1%9 publication describing the chemistry ofphenolic foams. See Attachment 6.

l C Director L Office of Nuclear Material Safety & Safeguards February 10,1999 Page 3 of 3 , b. i i GE has obtainxl limited information on the white residue and on the chemistry of the resin (see Attachments 4,5 and 7 respectively). i l contains correspondence between GE and Eco-Pak dated 2/3/99 and 2/4/99. This correspondence involves questions and answers for clarification regarding the foam and paint. contains Eco-Pak's letter to the NRC dated 1/29/99, reporting the results of their inspection of an unassembled 55-gallon drum that they had in storage at their facility. 0 contains GE's discussion of the BU-7 package based on the findings to date. At this time, based on the investigations conducted and the information available, we are unable to conclusively state the cause of the white crystalline substance, corrosion or paint blistering. There is however very clear evidence of the corrosion that took place occurring on all closed packages, packed or unpacked. He white crystalline substance is clearly visible and most likely . is a hydrated form of zinc formate. The failure of the pMective paint is sGil imresolved, including verification that an acceptable paint was used. There have been several changes in the formulation of the foam over the years, and while l physical characteristics and performance have been verified, it does not appear that the chemistry l has received attention. De paint may have been changed without adequate evaluation and possibly without sensitivity to its purpose in the package. Based upon the lack of technical information that would enable GE to develop a recovery and corrective action program, GE respectfully requests the certificate be withdrawn at this time until such time that a root cause(s) and corrective action (s) can be identified. We also request that the GE submittals to the NRC for the BU-7 dated 12/16/98 and 12/30/98 be withdrawn. Registered users should be so notified and made aware of the conditions detected in these packages. Sincerely, GE NUCLEAR ENERGY j Charles M. Vaughan, anager l Facility Licensing /zb attachments cc: CMV 99-006 L

i-1 l l i 4 BU-7 PACKAGING i l THIRTY-DAY REPORT PURSUANT TO 10CFR71.95 i i i l NRC CERTIFICATE OF l COMPLIANCE NUMBER 9019 DOCKET 71-9019 i j FEBRUARY 10,1999 .i

Director Office of Nuclear Material Safety & Safeguards February 10,1999 lb'- Page1of1 i l BWX Technology Photographs and Report to GE Dated 2/2/99 i i 1a - Six Photographs of the As-Discovered Condition e Ib - Conditions Observed in the As-Discovered Condition and When the Package was Cut Open, BWX Technology Letter Dated 2/2/99 i j i

- 3--

^ f Y + 4 g.,, m y z, ~~ . Qa v-trw a 1:. w' p. yIm z e o .. d {f h g__ n. = 1 o. ( [ ( W w Y.. E 5,. 'r' }V ~ 4 ..y. . (, 7 f 5%. L, rg < hj, l e 1: .,.. a.' e ; ;...;,,l;.D. ?::::l;^" l ,[' ..n..._ m y

i. :

A.' - y. m4__ '.:., :.,.. '_q'.:i.l.7 ,7 O .. : i.l,. _. :. L f .j ?.l, f,... .; ;..... _j.;. :. 3 ;;. :: .j ' ? L; h &, ?.\\; l' *)) i,:: ^ .J_ _.;lb;::,l l

^

l _ '. 'f' IW l.[.. ' :7...',f. J j'. [ ~,l j, a e . i *,- [ :.. ;

L-

.., '. :........ a 3. m ; . c _:. ,7;-

L: ':;. :._ ;_

L..2 .n l, i i; :.4. f.,. '.. ',... '. p,_ ,:- : ;-..;} y,".. -[*- 4 4: - 7 ;. f g ; .,'.;;. v.:_...; _; _ l q p.: r.. } ;. l ,.L__.;.',. r.

. y '.. '9. ~ ;;..

' _ _ _ };._ ~. ,,..).'.;. 3 ' ; l

9... 7 -:

.' :. :..,..=,;-

', ;..,,., f l, ' { ;'.

=

b;

..',{ ,'? .y ~ } _' i. : c;;.. : : ;,, ;g .7

. j. -

7,,: y ;.;;':[; [ ; y n ... :. *) : '.._. b /

/,,. J ;,: .. * *,_

L

*';.. l ' _', ;f)l. l':.~ <...

! i.f$..l }.....% lJ {_ lj' ib.. ^

r.': .:.; :..::. r : :L.

% _:3:]l. N :. . ~.; :./". * + * -..... : ; ,.. y.%l;.:.. : :__ R>$. , ~. u.... : u,w... :. ;.:..:.. = n-4 1 f_ Y .,[ ' . N l. : l_ :... v.;... j. l ~ [. '. lE;'ls,' ~ ? ~. . f.:..?: l:, ( 7:::: / i K L f{ " ?..);:. i V j':f :/.fi :.7.:. J:ll 13: c I ..:. :. _ b * :.,....{~. : ;. 3' ].: ..A.,_ .,.o n._. ;... c... :: u, c. . }.f -ll:;:l f j 1; ll:. '. ' l,\\ .'.::' A l.. : ':: -? '.. Y ' :_ ^ l ^ ^ ' ; -;[e..v::Y.J.7j}l,;..: :,jjjj.f..c_;.::g.._. c -.Q_Q.f:, t g-Q i. 5 e .. : n.v. ", e. ", _'. f...; : ;{.;;;).;:. :, :. .,.. n )_.. _ _ ' _[. ~.;;.; 6.,.L L ;.Vf [.;_V[ f" e. .;::3,'Z:.W:JJ i ;,,..,.t.;f( %G.T J:q: ::;:.>: ' ~ K n [ f /lQ;l:'l.O.:. lO f[::)&.. {} ' s.n :.z.. ' ', ' ' w.... ,..A.- -,. ~:..,:9,-. s_l^ '(. e T ,.., s..'.. ..[ /':.' u. ' i, 'f ' ( [. . ; ,l, # { ~

U:. l f,j}.

',. '..' '-: 4. y. ,. _ j ' . U:':.;'..,.[.

_ ?'. ';);: . (,[* l ;ll ;).

g ', : Q. 7 4 E n

y.. e

..k y gl, W c p t ? e e. E

/ i n 1 .o 1 l 1 1 i l '. 7,3 ..h

1 -w. 4 4 a.,. ar.n;T y,.gg .^ - :<.- a 'T S.,- ) p;p ,.) j l . b5 i,' h. n. ...,:,.e,pr . h.:.,. 2 %w?b&.; 50* ? l t Q .. u ? n:~ @l3 ' ia. .e..4plfQ$$ ba hl wwg l ' (d.1. j 7.T,;:.p* ' d.n y* dra g. .v QL', p T:#p?Q; l l T}. l. l r ml y d$ l . n.lyeSW ~ e . J,Y M W i e.$5$.T'0;h 15$5.?f(,q W Qd9 2 'y* 4.h a '{ gM ~ L:$5l+ i~.G ..., cn. ~. 3:n.,/. 5 . f, ;.p.A..; -Q !.,'N f C $h, $

r

? g i M,. i

k.7' ('*

f @f [bkTNhhV. w,sMkbh W.#a.m% - #:*j$ h., 2;% " '&}W y*s/ n l /qq:9mp ; W4 81 l e' (l 'lyIkh',f^'e?$g 1 qw dws s -'. '; -- 4., s...Il9g,j o ,9 i, wim . a..=y' l D JM t". Mif gih?; yy..} -' 4%Q a ::, c./n.m ^ rw.diya (. ',, ' ;]ffyV , ;a py;:;a

,,h *. h,

'*f ' n W:pw e.. w, 4. .s . rg .. u f g c / c:. ,y, t ,, { ~

yy.

,.,.~

.A

[ q g.-

1 4 e' w. d ) ,4 j N ..,,,q.f*ep'.',l%e q,;K:P,,.[ i o qy.i$' f f.. - ] .g#n$ ' '.?. g',k " ' " 3, y%# 3.*c6 .,i... r et. .a b,* ,y..'.r..f.vt,*.,f,. 5:l..;;,.s ,:. ).

i P,;.c 4

(. ?

tyj: ? ,jf ) jr ' s . :'n. h,g,'s ?h. A P *W Wh - u, g.W 4 Q ,1, - !2f 9,',. ;. e g' 4 j +,[;. a. .'4,&l&'(:..) r y..,mo ',,,,,s .3 ./. g.,.

v. -

t .g Y+ ,'- 6 t 5. ',: n * '. s *

f. '.;.1.%.,

,,g "
*t,.. '

..i': 3.. sh ')*, ': o r. j b k..g 5 s .4 a,..'

' ; : * '., j ' ',

' y,.1 e e e., .e s - U '- i W..a,6.. ;.e.,' D.. :- '. W ;.'.'.t: U;.. M. m.;. .s i 1 , f. ,".?' M.,;. ' I;*[v. /*! ' j *f..( p :.(.~.,.. * ) ,.~. .gj.. .......... g ; 4.. u 2:.. p(['. Q.' ':, ', ~:, :';.; ' ' s f.L.;.W::qQ,l, 4... M

g i

..s. .6.... a d-u u n.?.'. F. ~ '.. - .i q>.*... %:.,lt, i j

g..e -

', ?d ' 4. f s,(k,,l7..

a..

t [

E... i. ',

j g.wa., f.,.4 % ,s

4.

a. g . n.'t.4 .e.,y... ,.. ~..;.s%. ':.y.:.. s .e ..m

'~

i y a. a.g..r. # ~- ..p . r. ...g; f,. 1.... .. v v...,..,.. -..,... -w,...r... -. 8 ..,N.,,1 = ,,h. ' Q,lC P; %* A L

* * ** '. *? 1 *t *
1

.,s ) NM (.y*. f,y. ,, [.,..., I j 'k, ;,! % a[f. # ),[e ?

* k...

S,. g,f ..) b e.- ..,g s.Is \\st. r I ;*.e.. :-.tf.,.'f'. E .,,v.((t* 5, c,/ c.! y M. g .e . a~ . '. y 1.... r.. c c.

m... o.

] ,, r

u.*?f*:'=rff..

t. , 4 %...' ; f..}/-. s. 4..,.,. u.*.. .'l.l r., .3. .s'.' ' l%W i 4.s v e ,('.r*.J ; 4.. 9 y;... f , 4 :,*., n'.'*. .e* i. '.4. '. d,, i ) ,a . e .\\.*;g* t,p(.h 9'V. e ** &p ...,;.. : <, y f. %~t.

?

Q i.w.....,. a ~,A y#. t,. +. c - 4 . s y,e. Ve73.,f,. 7'. ~. ' S ]

,;, c* e i;

.6 S,.,,,,,). p . i;..- s .o; 1 s.. .0,.'& l tag??. t$(... 'd *.: 'ry'l, ,p l 3 .s. .gf;1? e M- _ g. ~ ,;pt \\f's.V: ' y47 .;g {l.'~ ,&,sqq g9qq } -~. v... w _. ..g

'O.

'd 1 - - -, f , .k. l g'g_ q g . M 'M i. t

,Ar._2__^du.__..AA.aMAJ._eA,.MM--A M.u J a.m. e _E.w.P. d.6 u.- As*e_44 d._ J. a.m m ura.mh-w_wmua...y ._as 4y a-,..me.u-aa__,2 .,_.__a,. w- = 77 n; A j.. ~ g.8.. 1 ,.u. ,18 A b-q q r.l, m ^ ' ,e ) '% 't * * .l , ?f e,. y . g.

v...

,., } [ f. k .3 g I ', r. ~ 3

d...g' % 4 i4.' 4 3.

a .c' e :. s. q g y 2;. ' p. :eip@~y.f ?.. t k.g;. c'Ydg.n &(W P u+.a&,.....p:$hh':.TQ,ly>s?

(UA]&.x.

,.V. ldll.N: i E ., j L.. \\. c. ~x o ~ .. ~. ix.. g ].y.3liG}%})f. l ' ' 'y.

4... g_. ?,, ' '

)>.y. f' n ML&. ' ), gr.4 m m-< s s. y 1 m 'w .c,~ a ; . rq ;> s. W S 3'. Y\\ .}7 y + u 1 . n. f ' '.;.

l. f,.:%'u'

- }. ' hi.". j. ,l 'p. 1,, 1.e f-tp w:. w w&x..g' {..<f

1../

/ ' e; g Ak.:n. p s. vjQ) s.).. + 4- .p~.a '. r ..q/O t,,, y ,.a..g.y. -. m. . s.- gi% y s..;:'f t. .n.b.

c. A. 3-

+ s. '..E'. j 'l.. IIi.M,'a 1'% gr. ~.;, - p' - .c. "[).. \\ / \\ G_, A'~llk, kY&hh, I #,)- ^ ~ 3 s ', s,. .. ' _ '... _ ',... #*iy. %*ng..A..' /* g .Y

y*-

4 ' pp h

~

y b i g, 6 e

,,.._wm.=' u- ^Aa'MW ' ~ ' ./ g q\\g.g m. uzy - f,e e T. + wy j . y (igT' a y1 i l f' (a 4 f l c'p A.T_%.. 4 l t. ly A-f- e % T4 4, i =C.o M f., r ~ t.d'".' y f;' 5%q t t i t j. J q,. \\y.. .S. 43, l (} ~.I.8 n a, s in 'a f}$ j 1\\ t.t,_ s:.3

f

.h.k4 yh7h I y p gqq ( . %.w .[- $,$} O. 4 - i; ' f,,-

,2 f 5

h2.0 -{_. h BESS"1 r y s +- .y. - . gg _w

e

. me~, r ..y_ g .. + w .., f, ',,. s :.,- 4 [: ^ .? a - m,' u t' _. g

j. *

, ~ - ~ 'g\\\\ f" ~m-gv \\ ~ gg 5? -f o., N, O_.3s;fll55,:221ikl'b' .a. ... T.* \\ .x

1 l BWX Techn& gins, Inc. Babcock in Wilcon, a McDemi' ccTcany Naval Nuclear Fuel Division P O B:s 7P5 ,p ty-ceteg. N A I45:5 07M I (8:4i 5:24009 February 2,1999 99-013 i Mr. Charles M. Vaughan j General Electric Company P.O. Box 780 Wilmington. NC 28402

Subject:

Model No. BU-7 Package, Certificate of Compliance USA /9019/AF i j

Dear Mr. Vaughan:

i BWX Technologies, Inc., Naval Nuclear Fuel Division, (NNFD) possesses 1187 BU-7 shipping containers. On January 12,1999, we discovered corrosion inside the outer container and outside the inner container, of one of the BU-7 containers during a routine inspection. Inspections of several other BU-7 containers revealed similar corrosion. We notified General Electric (GE), Ecopak (the fabricator), and NRC. Since that time we have continued our investigation and representatives of your staff, Ecopak, and NRC have visited our facility to view a dissection of one of the containers. Samples of container paint and phenolic foam were taken for analysis and photographs were taken of the container. NNFD has attempted to evaluate the effects of the container degradation as required by 10 CFR 21. We have concluded that NNFD cannot determine if the corrosion of the containers constitutes the creation of a substantial safety hazard, as defined in the regulations. BU-7 containers are currently utilized at NNFD for storage of SNM. An evaluation of the safety of these containers when used for storage was performed. We concluded that inspections and destructive examinations on an annual basis are needed to assure the continued safety of these containers for storage. NNFD committed to NRC not to use these containers for shipment of NRC licensed material until the source of the corrosion is identified and acceptable corrective action is taken. The enclosed information may be of use during your evaluation of the container's safety. Sincerely, f n 4+< L k Arne F. Olsen Licensing Officer

L I RELEVANT INFORMATION REGARDING 1 DEGRADED CONDITION OF BU-7 CONTAINERS AT BWX TECHNOLOGIES, INC., NAVAL NUCLEAR FUEL DIVISION l Container Certificate of Compliance USA /9019/AF Model BU-7 l Certificate Holder: General Electric Company P.O. Box 780 Wilmington, NC 28401 ] i Date Observed: i January 12,1999 Observed Condition.: At approximately 3 p.m., January 12,1999, corrosion was observed inside the outer container of a BU-7 container that was opened to perform a routine inspection of the contents. i The last time the container was opened for the routine inspection was 14 months prior to January 12, 1999. The outside of the package was undamaged and showed no signs of rust of other deterioration. Upon opening the 55-gallon outer container, a white scaly material was observed on the under-side of the drum lid. There was red rust and pitting was noted on the under-side of the lid in areas where the white scale had fallen off. The surface of the scale smelled like fresh paint. The foam plug appeared to be in an undamaged condition. The blue paint was intact i and there was no signs of scaling. The foam plug was removed and the upper three inches of the interior of the drum, that portion protruding above the foam material, was in~better condition than the lid but there was signs of red rust and pitting on the drum surfaces that were exposed by pealing of the blue paint. The upper surface of the foam that separated the inner and outer containers was also painted blue. No deterioration of the paint or foam was observed.

'i 2 } The inner container, which is centered within the outer container by the phenolic foam, is sealed by a gasket and the lid secured with eight bolts. The bolts were observed to be covered with red rust, including the washer. Paint on the lid of the inner container was blistered and easily pealed off. Areas near the bolt holes and the rim were found to be rusty ; I and pitted. The gasket was soft and pliable with no signs of deterioration. The interior of the inner container was undamaged. There was no signs of pitting, rust, or paint damage on the inside of the lid, the inner container. The Boral insert was undamaged. The containers of' stored material were also undamaged. Subsequent to making these observations several other BU-7 containers were inspected. These other containers were selected by their storage conditions. Some were stored in trailers out of the weather in uncontrolled atmospheres, others were in Sea / Land containers, and one was in a shipping / receiving area that was atmospherically controlled. All the containers that were opened exhibited the same general' egree of deterioration NNFD possess 1187 BU-7 d container. All were fabricated by Ecopak within a 6 month period. No abnormalities for ' noted during the receipt inspection performed in accordance with the NNFD Quality Assurance

Plan, j

As of January 18,1999, approximately 15 BU-7 containers have been opened and all - exhibited the same general degree of deterioration. One BU-7 container was dissected to allow examination of the interfaces of the foam with the metal containers. Corrosion (rust) and pitting was observed to extend from the top of the foam to the bottoms of the containers. Actions Taken: Subsequent to making the observations in the first container, NNFD notified General Electric and NRC. j

- Approximately.15 containers have been opened and inspected.

One BU-7 container was dissected. Representatives from GE, Ecopak, and NRC were on-site to inspect the dissected container and others. Photographs of dissected container were taken and transmitted to GE, Ecopak, and NRC. Samples of the white scale were taken for analysis. j

- NNFD determinal that an evaluation pursuant to 10 CFR 21 could not be made by NNFD.

1 i i y. l l l I

is - 4^ ' t t -.. Q:,:;.z.. s ' ~ 'M s'

gy. - r: r y

..n.. i 73 ,.(: - . }[ t-4 m y ed - ::4 g,.... h.' h ~f::4 l . ?:%.c .~ v,. ,g -. p.. =p. ..' n <. ~ l g. C..,, :..... .57 %

i.. -

.,,.. '. M. n'... ~ l 7 ...r c, - i .x-l .. f,E b.y g]. ..;;.'. y%g '4:Y. 's ^ j , l ape.t ' g: 3 '.:. a ;n :. ., d :, % ', .,,'$.~'- h, a, 4 v. l T 1 ge i;.3. r ,s.Q.,., ;.; '. ; -.. f ; - 3 4 p.g ..t.

~

e .~ ~ y' t.; l y s v -- 1. ',i.;M['. . L.. f ~ t ,,3, j . 4 S [.., 6-Q, m - e .y s i, i p ~ j..y... .f 0 l ,. ~ jfj;.44. j .. i } 'i jl,,q.. ~ ..j n ; 1 L,"g .r,aR g, { .,.. f- ..,.. r. r r

?

. T, 5. $, l ;$. *. ' [*.y

q..,:.

y ',,4. ' ' ;. g), g . :,; g ';b,&~h. <..t ? $:'?$ b,%$~fa. -.r ','.' % . W. ..f L. 4, . +. i eg l

M:

r '.. y 9. '* i?,J,-~ ' 2,:=. k ,9.R.y.,.;, j ( ., ' f . c

,,.{
.K}

..,~ -....y O.$ &:. W:., y ggcQ,, lr. n i L N,. ' :.?,_ E : 3' Q% w-. v .::c 4 = -;3% L ,'.i w~ w. jb4 :s. ' i

x

+.,.. 's

n "k

Y. 7::.-17 .q - - ..9:...:.5.p %, ;i &~. 4 =l.~-y* + Y.k..,

4... :,,

n ~ '.y

N 1: % ?'

' 2b-?. _;,,,;. ' i " :3 v t .n- . : M. .s..y.;;,: e. ~. l .'i af' Q-T.s -?:cQ.. Q ~.,:% t..l, ; '.,,a :rR Q. # c',< c..'..<~ a ,r 2 _.q,. { .n: g r t s.-.-.i. - y.,. 6.t'y.... ~, 3 ,!r.e. e .,. 7 ; : '.

1

.s ~._.JTS' 1 Interior surface of 55-gal outer drurn with foam rem 0Vcd - 4 l g-- e pt'

.is '

q f __.[ '.'.)_ .' - l;.~.,: - f 75 ~'.. l

i - J. .y.., ~

e

.j g7F.-- ,#. -

e-yt 5

et { 34' f'W ( '".) Dd \\ [,d, k.b.hh 5* ",.ff 'kh 5 hp $ l y',l l k .G .%'.= %.., 'O0;. r. .:.t.....? w 4 y;.m,e 4 p'a4.)'f,.,:. K s'! ..,s.. 3'.4...;, i

f,e.'ge.

. -q.g. '.....' a.

n, 9. y.:,,,p:. h,; 1. <f.r. ! ;..

i ..,.J.,a~' r-.. 2.' t ).. i. *. " . t....,-r..p;; ,q* ;.,# f,....,4.' u ,.a r 4 L. s. v..;.. :lt ? N t, h ' s.p q,. ?, - -s ; e y ..g,..,, s ', )' ~~ $'.E - M.* ' ' ? N*'* 'r' W - 'e:w 'a 1, s .;,T or 1 - q:..e ~ *... 7. , c.,.,. p,. s - 1f... .,1 - g. $' e:a,,

..." - :.:=,.

,f,. :~. _ t. -., o*- .,L., ^ s n e-

a..

..s'. , e.., a. 6 [..... '. ..e.',- .e 4 - e. . ?,, s ~... - -._- ,., 4.. 5...

o

.... c '..,..g4

.....,s: .. f....

y, .y ... '. ',. ug *3; g y y,,'e t 9.. g r.,: %

9.....,

.. c. ."c. .*$e

f,;..

, % A.[- yg'*. l s - + ;.. _... +a,.g. ?...

.c..

...- y .c _~ ;.

x.,,

....~..;,._, . s .n,;. ,e.t,,g., a. >.. , H; ?. q.t.. .. ;': *[.: *,Vi :'. * . ; ~; _ f

,._[.;

(.s(:ly '.L;.', 3: ,.r a..,v.,.n.s a..f., f, a v. r w y r 7.i.,. m ?.. ~.

y......

,.^-..- gy, n 4(y. > . 4.. p.- r .. A ~ ; ~,, y,. ;.<.. - r gr. 4y c ,. g,... o s. _.. f. ,. i' $h. ' l.. _'.A., I e .,:4...d, E 4 4sr Z.1 >- .m A-W.g A. a y l .js.'>t", ;. t .) [f*7:,&.'-& W.. $[ Ii'.~. &oRf .h.g. Y ,l..' [. ~ ~ ~ - :+,..,<. W..N..l f '.l< '-l 9-W & _e.-?g.*&.&r,. k qL, t g '.. 7 3 .r.,- 4 a% s c

p/-

...ys***..'.'c.. ..). 'i

t... : :

J- $,.'mh."o.6.'...y. .,y ,s e.,. ... - :" 'L :. e 4 Q:.n *" [. s. i T s. ,, r m,,. [., '.,,, e '.4 ,k. ' 3. '. y w+.. % P, ~,.' n.

.. *.. ' ~

.g.y .p e. l 4

I I

.(,... - t p ;.. j $.j=$I. ' ? ' ' . 7 -- T-Np .., ~ ! sYY.'d.'.Nd. .,.. '. 'T {. b I ..._..,,w e"s.>1yw,'1r 1 4g* h?.- gi.,. i n. p, c,. ',-%,,.. 4. .c... -;s q - ** g.

y 5;,.;. _.;.

.y,.~ t gi._ g.. =,, ' *. .-+ M " "j~ -4 ; q,'w'. e, P ] ;*' '?. g, u j,.;*.'.. y, .,r p.. r.N._ p g 1 II Outside surface of inner container with ~ ~ t j foun partially removed. J. m. . ~...... - .s . u-j 2

- ~ l ~

a_

_? s [. .. ~~ .} ,.5 Y $h, %.Mu..hf,?..&h '.E Y W h A g%m.W*'g.iWWw.. hf% %,q; ~Q..M

v. '

i p~*.. A Q v q g ** q* s.* e= ' # 3, y,y"., j.,8%'

19 7* '.

y s ;.- p'*':, i [ A*. .,' --. f, 'M

2 5.

, 3* / i J. s a ' '.. : { Q*i. . 'W ~.+ ; 5,.' ' e f

, im*'.

' l':. 1, _....g'.- . -..T ;:..: .. w ,1 s,:,,. ~ ' [' 'dD ! . *g M , -%, y ' -~ % : -T* n* ~ '.a.* - yp r-o yg. .,.. ~ M* w- . '. h' '.,?,. v" ' ?.' 6'#- l- $ N %= s' Q" age

..A 4. ' h ' ', ~ ~

h." E f 'E.** ~ ?f ' .E Y' ~ ~, =* ,al. l i.%%~kk.~e.%*.@k.-3 Ad 'lWitM'a# h '%,.y, Q A.h,'.* Ia' I } * [r'.3 (.. M

~ -

9. .'s- <....: .: 9'%s j1 IJ h* a. e

T a

1 r W ~. n,y 7,:a$ .4.6 4.....,.?Q;',1, i...,v:. 3.- e w< 1.L 5 l 1 ?. .g.,.'. 9 ,. e.. 3. ,p 3 [. i., s.s. Q; p '.f .f:.+ c. . es .-..4, : :. i,s. v ,g. . 6,.

.s l s.., : ;p.

,, ;A.,... ,.ly, 3...., yu., z 4 s.. c. .w . f, *.. ;... -. ! y;. r, s ?. Q Mg .e O).. x. g**t,. f ) '.:. , n i' < e; ;

r,.

g.- 9 . f. ' u'-,*;..... ..~ _ %e$. ',... C e - ~

,. 3, _. p' r.

-^3~ .. z. - p .\\*g>>xM. -\\w

h..,

g, Tf... 'P r. 5 ., k m._l&, ' '_ a .w .*4 ..*,ye s-s, e. - &. c' '. - g ,,., 6 _ e,' g o;, '.., ' ' * ,... =. m. A..:. --..3 y '. ?, .] c . ~ o y,, u. .<s. s.e ~ r, e... ..,,.u.- 1p.. .y <-y s _ge. 4# -. . y. . ;,,>)- .~ n s' .. %.o ?.( a. -c j '[ Q Q q ', W g.1 $.,1 y. ; , h v.' t ,2 : 3 L j, . p 1 '.h, f.' ?.':c. _ ' ,A ~ c M fp sif W~, { S.['. y. f _ %. f ' f [* MajV', y,L - 1. ., w i .. [. - 9 ,1 p,(,t S,.,. 4 :.,- g. , I [ 7'. T f, ~- -e -s. - m 4.- 8 s.. \\, !5 i ,s. s. p i g' ..f. , p%. y4.. r i e , - /) a n g Bottom 1/3 ofinner container with foam J removed.

..------,,_m.--. ---m _.m_-m__m-- m. ,g, f - I N l i g ~ I 8 \\ x .m x s \\ l y- \\ ,,p y .g :. l:.: .$$/hi a-V. }h - ' ' g l l 's c Ef ',' 8 U.. z: .h %r (- 4, T.i.. ..) :. 4 i 1N. / l 5:. % ) o l e,,, k /,

f

, a = . ;... W.q t O ,r ' u. '_-%_.- ..e / / .,4. ; -- ' :7pq y _,q,,. :- 73 4, m,. -m ,.-.-,,y-w--

t A ,.'d ..9.*..: ', c d a f i.., ,'. *l.N~ I k L- ! ;Y...h'.*~ ' ;

q:,

. ;:.'. '..:.

k s'..

';; -..- c :l,;. r,. } lg * ? * :,. '. ; f ?':' :L * ~;' : -, :' t.(p.1. : V:t '. : ^ A * ? l~, A : - r; '. }}. ; l' .. '.,.,

t :. '. ' ;,., _

~ :..'.., . ' ~

7,

? r '.1 L e

h ~.i ~

46 f*

jf ~ l ' t, ?.. .[ 4 ~',,.. s t. ..,: ; }. ^ :.* ^ ?. : ' L '..L* ' g *., -" > 'l',.. ] * - [. :. l.', ^.,. ', *;_., [. -lE :[ ?.'. ; ph : y * :f, . p" .,., l : ', ;. ' y.. l.%;* ,Q ..~,, - _. ;.;w ..,9,.- j' l.. l. [',',:'.,." s 4:ll R '_,;, y[._.,. %: .g. ,..;_l ;*,k.9,[. 4, ' l,.': .yfa ' I / * ' '.

Q.. ', [:. " '.' ' f' y

.::l l. *..:,.:., ( ' '... ; :l, [I,C.. ',. v .*y... b.'......q'O..'... 's;dre.: '...-'.':,1'. J' 'f,...,s'. y ? M.4.. a,g',

3

e'

a. *;.

'.l ..c T. i - . ; f ;,,.*,.; .l - 'o r d ,.,'.,,.'*f., _ t, }. "., 8_ g ', &. ....a.

n..

.s .~...e.- s(

v w.

,e ..a. '*g*A,....

. f.;$}_ 4yf._:.

.,:,;..,.4p..',*__ ?

c. * -

,r,' [. l _ I : '., _. l i, f, _ r, q' y - .., ;, [- l * '...Q l n. .h..!... l l !._ . *{ e. .. : 4 "s, ,,v ...,y ~ ' f, 4[ i '* - f !;' t,. i. y * .T 'l, T ll

'k....'f

. - [. f - ,}','

; y: : R _.,:

.L' J f.' '

f,

i '".:;,)a?,'[: *. .(., t' '-,' _ h( j,.Y l' f ' f -..,;. [.y ' i;' * :_ .E .,,-,..pL,',[.'. ; ' '.,, ;.. i ,..,.... ' [g r [ ' :. M,- ,,.,, % '. ] 4..4 3 '7 ;.,. ; e. ,, 47 .-.... j, ,y, ' _ 'j T.r;O:,g. n, .',n ... j ' gir . *br. ... '..._,..,,. -,s .e , n ;* - g e. .y.. 9 h. l'.: y? Q : >:j ' *; y *..,g;. ); u;..... : 4{:4 '..,. f: y.._.-:g.,_.._ _ Q:': ** ' ;f j 1 h;:k.,,k;h1;.,y;%,y,.g;$R.s:.5,.3,.

,.. ;* / *,.,. <,,..s.,.

[. *: s>l:, ,l,..,, s-L * . _, i '.. L. ; A -

.:.,.; ; ;; g.( Q, R.:. gf. :. Q ~.. ;:, :

'*:.oh f, 14,. h: Ll .... -ll.CQ .l. .: e

3<.7: ;,.'

. i:.BV.:, j [ 2: f ;g.. '.. '. ;;;:h;..

r..

.. g. . y.., _; - :.;n .y e,;: ,, 6 i,c - h,;.,;h;? q ..t..

. vh y....,kkh;kkh

?hkN k g mwmm.nw w ww@.av.+ h,5%;Q4&f Q T Q M Q Wi .y.r WW O Q k h._hhhhh-),f.:.?hh,u.mgf.m @NN[',i?s$xxm.pw ..,w h,k*g.M N M.m.f@w.w.m.{d NMN.f.

d

Y MN w 3..u:*.*c w. w. y m.a . i.>. m [hhb oy[hkkhhh h a.,:m. ..h'.., . w 'M. g.,..,,, ;,.;. ,,s a'. f.,. ' v.. m. g '.: ~,- W.'...,. Y, -[ 4 S* f E.- e. :. ' v :.. ei e m e:... a, w :.n.a elG...'[..: y :nl ;' y:.#

. ? p +h L :. ) &.:Mf f.L c'L.:* gQ.R.VI;yh,Y::s.$. [::, R:

o:=,.::e x.w.! % es 4: M T:./. a/ y %.lV ' 6 ;

.: k3

. w. m n..g q~.;~,Y,8

.l y.n.,.2 4 f,.* y &.,.l: (m%. :',en,; O y.; v;

d ;;m;N: .,:..C f,;f g,W,'Q :

l C;..Q:..*lG,. : p '. " % :[ '.1 ..,... s(,. y.%.:... ... =. ':;.j v a n. ::.., a . # 1 x._.. ;.. g*., 4 g;'.:. . :.a. 6 :3 p t..w ;. .v. u

q " 7. N, :.,:',.,, '. :. ~. :;'.
V &.. - '.;...... :....,..<...

p;Y i ..e e. g *..~ .. v r ~.: . %. :.9. ,.~.; : c :..,:R.;a / : s}_.,.,1, o. ,,... - l,. 1.' :.. ~.4, ~[, *p. 7._ '..g%. y. '.?*r '":...'...c: . : ;..q 7: g. y.. y..

p.. v.< < :.a

.I, ( '.l' N ; J *f. :' w d., w... . v',a..,.: + ~... -... a. %: W D... a$.~$ '; ?.: .m

u..

. f. w,sh.... m., $ '.f ;f,.,,.N !l . u.. ?..j h l . k.N. l';. .. :, :., R.4. h..;>?,%.e (.k ..w.l ;4 &v...w} /.j;;) .;;;;h '.;;;.; :'s.}y>; 74. g".. : f,,W ; .c ; n.;.p g 1.n - s f }$j Mi%$ ?.;l;*Q: 4: n

l E f.:,l,l;' h d;.l; ~ ' % ?:e.-

W D WW 'Y h...: u .WM A '*Wh. ?.l'_ d h a N k_h,h,h k,. k. g L Ag MWpQ%% a 4 bhh h M # $ W M %n x u w, n M. mSM.a % w%e +4~~M.,, %u @.. g.~ m~ u ww R t y .n3 .. n.n n. w a_gw_w.4(y,p..e n,%4. 8,.. y w w. ., gp 3m... w.....s n g.... eyn.g. 9.., 4. y y 3.y g:np... :. :..; m.,7 n 4 In-place bolt & washer of inner container h&g&{i- ) 29 "Jd.ll&hyh, if",h.Th. L = 1..&. R f iM i W / S

.+--.+>.a.-_u,--.------~~-.~.~.~.. .-. - - - - - - ~. - ~ - -,.. _ - a 1 { I ': - lp*Ef' *& $'*

5

..f h .h,,( f

g a...'s c. p J{ k R* &..$.p?.$.;.g,x,5* p..

. f*,'i g. y., Y.b'r g,.;.ym z. 5,.y.&. *p. ye,f l: .-..U~< ,E

l. ']... -... ~.; _/

y 1 9 ? c.: .u k.;, .-l.: g,p a;

(

e. f.,',..,,, , p [5 '- ,,,7- !...,',-(* .,.;l'=...*. I ..[ '~ l.$ l...'..h-l;'l ? Y f _.. .e.. , b. ?'g -l; '. p* r s . e f g..- e .e ... 'Mr ,,.:,-. ' ? ' k;.,U f' .', 'L n=h )?hd((hi*h ***.:' *.f' '

. g.. gy

.f..=..%- 4 1 6.., ; +a . ) Rf ' * ??, , c3: - ' h*.. $..( Y.N. ,A W $' N..t.; i { hll[$,. fi -l.Q .fl f. Y. f* J 3 l 1,, ?.. I f Y{"l. l '.elg f ,g c. a. p r y, $:o 3, ;;

1'.

t'. - l- ~* .Q T.y,.yrQ.y, y j g.g6*pj.h f.y. u. w )'*.Q..,. ..ly [.' ;: 1 W. ..e. %, f _. p e,..*-fe~n 'v Qy e m y& e. & e 4l Rs G.,;j., % e r.....Q. 3 4 jW,. :u.' g-c.Q r

q. g. [

E.a.. %:C w.e w.l g .a. z W q .q.Qb .yg h. . y.Q.g.f m.. . 7. \\ W.*,,yh;R W%%&l L %? QykgT(!Vg 5 .f .i

y l.

k, W, '.. ;.*, p; h *

09.,

0, ?. _ ;i ' * ' 5;} {

f

'; ' '.-l '. '.. '. s., q. **. 5

e V

_b s .'ve' _ C 3, e vR^." y ae,,.' *:. ',.. s a > -

* ;-[Te r rg *f :..;A .

,e I* %+ ~ g,e.q < ?;

,.a s

E k ', ' *y ' T .* l' i T

e,, (f ; f; *_ h.
... ;.e b

.

f.

b.,f ^ Y.: $ 2?..h 'f. ', ] " 9. w.!y ', D ' l ' g$.q,.0 4,;./ ' 'y 4 N,4

G,*[*M ', 4 7

'?g ((l[p .( < [* ' b '*N 'J ? '7 f...( ['.l.4 { h. ',1. 's ' ',, eh

' h**..

e y.*

s. 4 ^;[.,...-' f,' \\,' s.. ~ ' [

'. ' ffar, f.'. 'g.[' y[/

- ) -,.g g */,- y;n # *J ".fN a 3.,. ;ej,{, w g,,gy.. ary g g 3. $*. [..g 4, y.{. -* f '*i. *t '..,.7l,'..", ,N.,].,e ? 7e .l.g ,,(j.. ....,J 4,%,;;j, d gg,., ... ' *=Q; g * ,p,. - (9 e - p.... i) - g j *g h.,, 't,4,;q.*.h .1 ' ' <- '. il, ',.,. ~ a( (. i 4 .f., :

y.{.

i 7 ' : '. , '

E

'^l . I.. f 'E; ', -h

' 1[

l r . j.,,, y, $ at ,{*); 4 7 g".... Y' I,l. $I li -Nc [ ', l f l f l-4: N-l. ..? Y ' ~ i' ".. ~ l ' _.r .ll ff,l_lf',fl ? l. , f l).. N.};.h' sf f :\\ ' '.= '] ' :; L 'c*h:f k hhjf[- kh.

,Y e.

L k$.

4.; ;.l.lj'. Y Q

.. *. ~, '/, j ' [ Q' N' *%{ &f. ' * *:.6 ' ;. ' ' ' '

'I',Q.ly j *,i- }' U. 'Qs - l.' 'E,,_. ~' ++ f -.,S. m 7 y y:. f,: -w a, e , m '., q.m:...,r ~ y_;, as 4.., W ~; _& * -'.,,y? 4 p..*. ;..y. 2 p:,.,.? p r -g Qs ,,o .~,,....c-u f. '.: ; 3.. %*n,. a, p. : ;.,.% 4 :. ;.,4 .y.. . *., h, e,. .).,., n g O,.? y.. .*?. v.- .I o' n'... '. '- ' Qe. ..... h..,,e

n. R s,:

- } 4..-

.,.s. _dg.. , s !} g' -+',a __',t , -.y s_. y. 1 } ';9.. $' \\* 4;,, ' : ' ; ".%.? 'i'd - ' y, 9,. MeV,Q p, "., j"P O," ."-l- '.e* ... fl,,* g. ;, [..: .s. ^- -g.. 7 C-1., ' ', - l. ;s..,';'..,

. M 3.: .

,e. ...s, ,,..,5. s.k'y,.t',; gy'lg 'g- . D '& ;.4 ;.*. r h{ '...( p,h.'.. f ll. lll. . . ',).g',- l . ".ir, i y.,g i.. } "l.).G )f. ::f.:ff;.. '( ';Il.} l N ?f ).;1f._.l

..l. ' :. r[.

-l ,[ /s,[ Y f, " ,. (' ' /* ..f,

(,

',, [ .f_.; ...,/.,. g h ', l h ; '. }? [ f-l l '.. 9 .f,0

9. ' ^ '.

. l, < l.(.$

'^.... -

' 2 _,.[ '. ? .} q _ f A A:: f ' { * )_' l. -t g 4 - ;,f y. f ;., .t ,,,. - 3 ? J< ~ ^ ) .e jj.... $, _ j..,. i_;, - 9 i ] ., ' ' ',,; _ r_ }., L... - l .Qn

,- - \\l_.'

_ [;., N. - M. . ' ?l~. [,,4 i , ;.s I *.';,. '. ','[..,'y'.' '.:::..;;;;' ': . -' k '. c _. ',,.~..I', l l. ,., ~ ..; ?, _ _... ' \\., ;...,

we y.

tg . wge ' ' '.,..'.l &q - a 2. '[y.*. ~ .. : C. ' - ' k.I-5;I . ' L... : ' ' % ':.. ' ? l. f * .... ?. '+' k. '..

b.,.,.. '.;h C i. ; %.. l, y...

". + l - r.,

s b

'.t

. ' 91,'g h'l _ '. f;... 't.. j' ^ '.,.. '.,. :.

l. ' ~

'.

l . l ' l-l

\\'_.;- - l, ', - x, h '.f . j Sg ~* -. k f . Y ': Y' 'h 4 g c. [ ,, ', f '; f l " fo ' l.

3

. [j ' ?l,, _, '..._ c,v. ,.,... ' go,.. v., q,* : .... '.....,, ;,,'. ;; _...... l. ,... -<:...,.,,; g..,c, , ' *. :' ; i;,

.,,t,,

.

b s:g:..;.[4 4 jy t. e, p., e l. ';;

,,, y. g .( 4y n *j -. %, oyQ R ,,q ' S .s ..' 4 } ;" 1 y '. _;. ; ' ^;

n ':

z.. .t.. ',e. .- ;...;. s;;- , ;,4 a ,,, ; *..,, (. 'g ? J ;*., -..? n .o . ' L.:.... . ~ - ..': -i. ;... 4.y,q, y s., - $.,,,> } ,,. ~..,' ', '

h

.,.i. '..'.9. J e. Q*. .s m. e n< <.. +.,... ' - .s..... .%'...,.e ',,.'.8..

4..,{.

'O.h' - f, g

j. t

] .l [. l.. ,,,. ? .; m. m :e y: w.c e -m. ~~z ,1 2 4.9gyr.q q,3..:. ;.. w :: v;.y ; ;..;. 3.[ ' g; .g. 3 3 3. ._ y :.y y 3g. l_ '.;.+ *4 4 *;

;< y ;

'f. " * ' '... s;s.m _.,_~,._.: ;...,.-

l _ '.l,.g. :...' i l:... t. c " r. w% ' \\/ ' g m; 9 ',,. tl. ~f,y' ; '.y ,) ', * :/., - l ':',; ". ',. y,;. ;.;.:.: 3 y l . ; i. ;'..L.: *

6

..1, \\ In-place bolts & washen ofinner containe j 2 j; *3 y. 3 " 7 ; A.;f 7 -._ a Q~: y :b ', g;.;p.N l:;1.. p '. g ' - cy.. '. !...E

,:; 7 g

".':n_; p. <." p'.

3.:

^ ^ ^ " ^ - tid. "n :~ ~:. ; ;.;, 1 L

- - - - -. - _ _ _ - _ _ -. _ _. - ~.. -. _ _. - - ~ _ _ ~ - - -. - ~ ~ [ .s,

v.. -[.

[%, [ 4 ,a ] $;#,, h [ ', ['.' [.7 g: }. ((; 'J, ,I (: k,it[; [I,[:,, g...:y l; ', ? .Y. h? _

.;.,. q f,Q. j f

_.M fh.

h... r f.

f 'll.l T: ,._ ):..D,(j. ' R ii L f.

f-

- [ [' - i;. ' :k : 5.[ *a;:: { :.(l. il -..Q fl? L,_ a f-G ._..y.. . ~ ^ 1. t ..., y..h,. ; ;,.l..g.s - -ll. - ~.*.6 ,_s I ..;p :l. ._ j.h }.

,ff. ~;;;f

,, ' f. _ ;: :,. y., :y;.: . - 4 ;..,;.^: y,y . ~..'.,.... : : : ;..;_ jl:, *,. t . -., __- y _ .l g .;..g.. y,. g p_ "};'.:^~ ';;-f,(.; f." , 3.,.'.. _,,_ L \\\\ ' :Q.;; L: i;h. l h.! ~:s Y. f:.h. l {.* ', Y. '.., ;:.,...." f. '. '. ; ? ; )Y',Y,. '_. ?.? : ':; a:- . L; i.., - A L.. :i. , %t 6' L.:.$.*' '.4;' > \\, ,;* g ? y

~
k.; -

?,N -.? :...w.y. g '. I'1.f.U .'f '. ' N h j.,, 4$ j,k. [t.. .'.n'...:.a-i;. ... i![...', i y;.

. v. ~ S.. f&.... ;M i.

,,':'j.:'

~.v. ? o

a..,

..4 ~ .e.'.V{A ' ' C :.;T t H. ? :i '~ j ?: Y.Y. :' :.h. . % (Q?. t.... .e ?W 3;; { H

LY.. -.

.'. f W b.

y ~.; * ..N .

9.,; u6

...]... .w.m

e...... -.; ;..

w. . 4: p:l.y Q_ g :. h f'. ;, yb".s.$..,.; J... .K., '}, f} l. l [ , ;....y..'

- l -

, 'l .: q... fi; : ?; y.. s. l.. n 'T y,k... ~n i.)'}h'iC s.,;. ' : ~ :-. ?m-,? l...a 1. T

'. ~... t...3.

T e V l.< ' ~ :^ .', tl. z:. 'r,_.__},,;;,.,..

% :. ; *; y.. :

'b*f, yf,. t's e ?..% .... : 1 : .!,3..;. :,.. _ : _........... : n..: .v. y w ;t3y;;. g y [ '.a 1,.,..f.p. .._.r' ' c ' ;..: w y;. +. :' +- .p,;.t p '.:.~,' : n- ...w ;;.y,. y -

v. ;y

' :. a

.;. y
g,,.,,,..

.' ;'A Y,I '..f' b. \\ ?' .it 2 i f~,-...&. ' i _? " Qi!W V E. !>....*^ y'

'.l j ' : ' :: : '.

T.. ',: .; h :' : "' O O ' :7 ffY ',' hl.e f.. . eh' l ;.... f 'j. " q

f.' ' %

'.' ll.

f '.: {I.'eh' f ;

le f .'] y r. S { ll. ;.?.

),Y.

'. '. g. ' l. .Y, l j l, ? [: .. fh.?, ( :._ 4. g ; ?.e ... 4l ?.:l . :?.'k .l.. ;.... f..; Qy [...g..<~

p..

2*fN.f; u-l ?,g 9.: '.m :.. ..p ;... ty 'n '..:..;.; l'.)l: f. u Y_:.n :

? N;.' N; ' '..,3l:... -

..._.y Y.Y':.l:~.l,.y (*;_..'.oQl %. % %.;3., g, L {:: f :.J,q# ;* ( y. g{..,.[,Y l;,.; '[,Lj,, :f,W'; _.; l.'. 4' . A-o*'4 .~.c.'L l' ' '., : s**

,,.L..?_

j ? :no. *. y *.

3. ;....

..y.., '. _ * ;. y W <;; ._,,,, ;'.. )s {, \\ 1 . 1 / :: ; J.,. ll%:'.: ; ; i,..., ; :,;;.. _...f, G 'l' .~.y . ;Q. .t,,, v ~. ' 4 ? 4 t ~ ' }.-[.,..; : r p..y,Q _ i, ", q.f.,. m..f.3,(._Q.4;,[.,.l;.: (-l;. )j,. .i,.

f.y.

r. Q. v,..'. _. 7. ; .} :', [. ' .l.. f .i 3. .... ~, _ 34 9 : (...:.. _ i ,. p s - _.., q ;, -: _. _s.. .,eg e .. ; ? '. i -... h k. Ys $. :.. ; c. s. f;g.f$.y y. :,.N',,' 'k,l... .. 3: ;. '.. f..: (!.b(; y. M T'. l {f,;,:? :)N. , Y. -'g : : f ' h : *h '." ':., L... 1l ? A k..;.,.; a> 0..

a. :. g::. y).

_. -. f,.j u. r

n.

e...

5.f..;.s.;c...,] f[* ,..;....,..,n.' ,.. f q : ",; . ' g.4,,,.. ; :: <1.%.:.. T ' y. W. ~..;' ' qb*

y SH.y :

?. " .R. ll. ;, ;a...'i'.N.... [ ;. ' fQ **f .h,N

%f:. % y.n j, L,% N c;l '
gic f R ;;?,'"' 5. f,,~n ;. ' L f I

.'t.;._ '; ;lQ Q-;k $ k.1h4Y E { }.ll..?.? :. T..l b;.. ; ( :: *. : : ~$ Li f ag40

/.,

Vv.y ;, i f}.}.

,j b'

^y.. [_.; . Q G.' l' *.;. '. ;,..? ' ' i : l* ' a::=' -l::;.. y.' _ z*..'L . :V 6 Q s ,: (

@ ' y;g <? we '. w,Q: ' }' y.,u t.

.'.. v; q... ?. ' y. ;W. q... p.:.,4 ,.: " k..ry. r L _ ..k ;};.ff _ :.". i.; : p'h e.....;+ - W.:,M. ....y..,;., f : ':. f k.;;l-ll.:

f.., f.

.f, ?:&fll. l ? ..':.l ' l l5llf.. :. '*:'.) _.f.fl5 ,; A.y';.'[:;f),, ^ *f ' i 4'f.k.h[&'l,f.,}lhf.M F.(f:lf., l 'h%[h_c. ?.': 7 iI* ' N .[L-@. ',#U -( 7 h/; ' ^.[.'..{ :.. I ? [:fN '. $/' #:. .1 ?@ J-$ (d'[J,S.,,, f

E *[i*.l(

h' S R. N f. f._ .f' . }lff

Y.

)$*;.1 % ',

1:.t

. l s b. Y.-

1

' C: W f.Q'.jt W:,.i h".[y. m[. p.y;y ':* b; R;l2 W g%y "

l&,;r..:i:Y T. T W. v,.D' n.~ ] ?'j;b;;.\\ :,5_'.d I:

..;If.,.). u ! + [.Y:L f!:

Qh &&M: l r:Qx *i' %;' ' ' p :L' n " b g% Wd'

a. ;? '. _.P.:.

.l*' $k *.Y ' \\ %. .f :.. '* ' s., ,4.); g[::j.: 4:y7'.f ., ?.y:f II;p.. \\. ;,,. c',N .[ f.

v. ypra..;;;<. 7.> ~

) s. . Q: .Nf...' }. 5..i . rc,_n y_.c ;,y 1, sy;f y.(,;; :(s... :.; r.z, R ;; ^*~ {ff. ;; WT y,,&,.. l. :y :f;.. ;g.;4 ;;'f.Q;y"r 4..;' v. 4...:.%fl:l.j h[:!..;.I;?; :is. ., y, n.;.j.,$? f_.9y, ~^L

R.

T:......- ,1 f., I ..>3m<u: b-t . 6 ^., c ; ;g..glw..p:. j{., ;?...l 4.ss \\{:.\\ k.[ '., g : v. l .jp :;. }. ..Qi: : .c 'lG j,k f*'_, * ..'j: ~ R .';l L ~ ' l I h N h . ih l k..: .h. f %a&.mw}wlmvm em. w;4}mw&w:& pyf ~w :s - .m ww g i:;f

My %J w

.f..q.p.:ff. <{ npgfs,k;h% $. f.h.).;s. qwl}ml._Yl.m wm .mx w a f'. > w..p. w f;Q .O.fl._.fjf a,,, ff.. la.n+ L w%( AG;.3; e, omm ..,v c mm w

g. & fm, e n n y m[;. m!.);Lf. w;f:p_:

y;;4}.plim.,.GlQ"f.; ;.. L _. :;.Q f{.y y ;.'.;. f _y :::;[. n. MWY h 4 Qn4g M M M .g n w & W w e g.e M ac. m e@ d.M.W sm ome m onom mmim e M*M k kb-QM f M:.8d NQNgh% M$Q#9f.@AWb$MM$) fb roem partially removed.

,.:... m; y :; j -

. 1 7. ;....RE

.~c..{y', ^, F y, :. q - y g@ g,,. f..

f. L ; :. ;

, ::* [':

' ' (T[3: .[.:

[ [.h ..,..l - }. - f [ [ g.. : [ '." } Y' .. l.... l .j' .l f ' l;.l[_ , 4 .... ~. _;.__ 3: ;...3 e _ ; g. n;. :,. '..

.;gg;;;,_ ;.

7.. ^ g: m :. ~.. v _ 9;. -:.._ ~ ... a (._.. 4,..e,$g.y,p sw ;' _....:;..$1.;.J;g.

..n...

lll ' [ l; : _ h..[ h:. ' -., { ;, I- ' ' l:_[ .l

..k N

..h' y: f h f*;}. "

i ;

' ;; :...\\. ~. ' L.[ l ? %! ' c '.. i 7 :(.l gg;J _[ *: x.)l'_; _Q;2 ._._ g : [.,.. ; : L. i JR ,. ;; Q_y;. w.'.'.: L*R..,}! L.;p}*p[9.J.'. G h z_ _i..pl;f_;ll:f'[;,:_.__Ty.f,,,'..!Q*::.: ..;___.Q+l. y

G

~.y

7... o=;

.y . *.. ; n... ?: s* * ;. *. -},. v' Jr' ..-,.;.,-.._.[; ; ,l p ..> :. ' ~ - _ _ ' _ _[*. ['.'l._'...f l*l [ . ? '; '_ _ Q..l '.. *[. ].' EO. h;.k I ?.f* .[ . y,. $ k h .eQ.L-~ g-l g;..... g,).g,.y< '2 ; ; - h.j:,.'-l((.?

-[. '.3 y}rc pr' Q ;: :

....a. s. S.rl ;.h:f..ih hy X $} p. _ <. .x

.: V Q.T

~~ ;,,

a. :. - > ^. ; ny W;,m*.'y%g,}.it

-( pj, 9 - }: [. ' :.. .. v,....u ;.. - 3.. y-. pg.t.y r. , rg w .r. ' 'l,l Yi ft h .l j { .,? ^ h f h 5 yQ&.,,a f gp?'.Y, s,.;?fy/ g. o.p. $b . q.. .. h. :.y., ,,y ,g yJf" py. .y h ?h'u.~ M.$ ' mY' f.,,..,?*i. R ((WfW j&.ny&fe.a k .l. N .l- ~ 5 d y 4 ll:. fly. k y & o $f{hki$ h l'... r d Q. V. f s, 3 p ~ fY;W. $'Wfr y f l. .t 5' ^ ., f i '. t - ) ?.J f,p+;f;rg;;y j' 4.4 9, f .T #s * .L q" ,v ^ -

*;o.

l...y :. ;. ql g*?$n xj:+ ga . O.

'.. ).1 [.

4, V .f cg.r,m p.}J. ' g*Q '

fC. {,)..,,, ~ a L: /;,; ;

l%. n , :+ v. ~ w.h. 43 &j. .f.f.; b}c4.p,y,L r{ 4 4.Ag)y]1. w a ... : N .s.:, '. .1 1 ( '. 7 3.s ,%ggpx. . 's.M$ 6 sy y.y. Q.$ - i' l f .;.;)f:. H F N Y TC G: '."gr ,3

s

+ s y V..' ....:.p go. ' ?. '+ }

t. < y

s.*, ;,f;2.y jJ ? :'4-?: p:yb.

p . _ 5t. > -l ^ ~ f. 4 h*Y A :.. V.:J.7 4pi(t . {/.... Ch Q. ....:... f,, W:e. Q*i)u. p,.(4. f e

4...

'g v.:..: 139. K.:,u. s. ~..., .. -. 4.;., :;. .g. - a ~ 4 ....,y p L,,

1,' ';.Q:. ;,? f@'5.g

....Y ^. s.,/* .. n ,e" - s V, , i 4. y y < A'q f {.;. i; N. ' hY e' , i... ' . / ::.-.. : -.y .. ?. : ....-- -...q :' '.. '- : i. h

- > *.. L: f

~"

=

n. "

n D.* 1.'s :%,,a ' }% -

~

3 Inside of outer container with foam - 1 f. removed, showing transit on at the top of.. M $.d h5. .. ;E' ,.s. . d .r.h, i g.. the drum

.._m m m -.-_ --___..m J e l t,[g h~. h:

. h.

1,': j[)

, ;Y ij.U Y: Y

.? [T'. E. J [ [.h.f'(, k, A l %.i 3. ; :.".yy, ?l: :.,3h,[.U 'm. :;,..? Ly:;;;y ::.3., >.' 3 3,.r.1 p.;,. s.[. :.p. : ;; y l Q,[::i[::fI!; ![ '.( ^

.w w.,..,

.... i..;.. _ ; j;; w* i L '-;.. a::u.:r. L. : w.. :.~ a :. .+. v s : ::. .c.. m ....;i:. '.7,,;r,.p; " '::;:,... :- ; :. ? J R. ~.

y.. ::

,:.,+...;.i.*._l.; Q:; ~ '.:.. a f, y,... ... o; . ;: l: - :..~."...L.q

u.... ' v..

j '; ~ -: - ..s

7. ; '

, f' }*.,

. a;l.: )j,, ;; /y-Q y.;;L.f.;g. (} s

_ f:/.j__ j.: ,j.((.}? %;;}; j.y'. - }; f.}:. ;..; yy.'j,,,:_.[

gfll;;

y, S.. ) -' '. ' - I*.[ ' '*** [$ '7,. ,4, 'N [. ' _. - j 'L::. ',",

, '.,: .,., :a.,.,. y y -:,q '". " ' '.~ ',

'*;.g,; % y ; * *,.

T Yly y -

,.i '%.., 3: :: >.:'... Q '..'...., * ; L. .' [:;:; Q ?.L _. . *_,y r:;. L. 4:* . ;...... :, : ( l.' : 4 . 'c ;. - ' . r..y. f g l l.. j :. '.\\ :) .'..v;.' '. 'r '. : :l l 'l ^ % '. 'e '.% '.~.:.....:-l .:.. * ' Q: I . 3 :. *. _ :......r e. :...

;;m

-.... 4.. ;z,p; J.. v".. '. 9:..

.;.;:. n c::

.~.. ~. p _7 .. : :.+ .g. c ... :. t. .. ?. u....:. '.., ; >[ [., Y. ' r. ,3 ... - \\.-.... : 3.' :. '; &

.;: .; ;.,... ~. '.;.

^ i c ,.~., t

.'y,...

,..c .:c... :

z.;z ' _ '; ; ' 4'

,.._ -[ .3.,. '4 ' : ' g, [ . syl.,, .;, -..,,, ' 2 ':,,,. ' *; !,, _., .. : m y.;;y. :,..v.. i. '.. ,Q :..., );;. :. .. ;. y :i '. ';;*

?1

,;. ' :w. '.t' .. :,)_ l. ?. 0 .. n)}:..'3,;.: a_... }:;. .j,, l;.{y,. l ;:L ........ x.. : : _,,Li ..,,. 3:: ' ',: '_ ' :,.,._ l .v .,._s. 3.,,: ; _. / /;

_ ;, ;. e ;..

.y ;._ ..._;..;.a .a,_ , ; ;;p, :: .;.,;..;. :,,;.;r i; '-v.; a, . ~... _

., _..;,, ;f[_ ,q'. ';3' :.

~.,.- s :..;.;, .; _ :, :... ~ -,.., ~.

.; ;.,. ;.;3.;;; ( 3

7... w

_l..:.,;'...; L_;. ^* - l. :.- .. :-. ', '. * ';.. :[^. '.i ::,.. ' ll;. v.;' - '. :.. ) '..., _., _. i J.; k. J[.... ; :_ ~_: ),) '., ' l.. ' ;-.,..f ',' V; :.. l'. : [ ', ' ' ' _ ' c * ~ ju l ;._. ,,s.,- ,L .. f W.. [_ ; ' ':* : _,.... '.. c. 3 d {..,;., ' {. ~.. J.;.::. '. ;%,. : .....,3., i,. ',::* y. ; '. *p :') ', ' :L.,.:. ^ :.. * .'..L

f L. * ;.

L:

. >;..., ': . v. 9. ~, '?

~...--;...,~,. [.... .i f 'U.' . _ '*;. ::. y:l.;. '.: u. ':.-.'. /,... ' i b..,, ' ' ' ;Q I._ . e, L ;.. .q . : ; ;..... ; Q.,,' ) :.L:".._....: j, a *.. ' j '

3. ::7

,4. l[ y :', U.f ;~. ? ' y,...,

' {;.::: J T _ ;;

a.l A '::a., , [./

3..

b l.N... ' "; :: _3 h

.,.'U:... R

u....

f: . r

'4

,.' r.;.','... j .p'.

.. v.: ...;.,3m......

l'.'V. ..i. ; [. 'g ~ ,_., ";,[. *-,. ._3 ,[: l:.';.,:V n.:. : ;.. :. ':... 3:. : e y ;;. 3. 3.._.Q;;.gy i ':...f ;,

3. m. :.t _.,.;,,. 3.s;,.y ;... 5. s;v_:y.., _ _ _;. ; L

. ; [ ' ; ;, ::s ?. .. ;: [..... ' ' ,. l:.:' -; .l:.[.. .'l. .; [:. n:: },; ; / - . c, '. _ ,y. . m ; r.. +.;. ; : _ _._ y ;, .} ', l. y., ..._._ s-e> ..c.. .;~., x,.;.. __,':~.

.,, ' y...,'.: ; -

.h.. ,.!a ;;

... -l::;_..,

......::.._.,..;.c..* _. :. ; b.. [.. -. p. '.._ '. ; y _ .,_..;,'~-n"! . '... '.: -l

A;.

g.; 7;;.L. [;.. 'f, }} '. J g_ [.;.,. r ,[ ._v .'.?- iL... ~.

b'

- l L. ^ ..q . '..,r:'

' l.

,,. '.. ' '..;c; .:.5., '.:... .:,:'.;x-l ..a . :7

',~...:..,,,'..'d-

.'w: ' *' h ~- '. : % '. . 'e '*;.z,'. 3 , " (.. } ; _,.. ' _ . (: ;.[..,..., . ',_ ; 3.x,

,. ;..).

-l _l* l p': _.,,,. ',, * .L.' %. _ q ,. i; _ (_ ;,;;.! j.. y a .. p F : ' : 7 m.,,^ ' e u.: s;e'n:... % :[:.,.; i*,y.~;.i ..f..4: W - :-: ?. ? ' ~ f-[a;.. . 0 \\ ' ~

. l... t

" ;l (( L q." y.Q]:. 5.l.);< l l. a..;{;$, T. ' ' 'fW 'v J^ , ; c:... w '.. n w n[x.w.. e - m. w' wn q] &.f h

%)h,h

~ Q $+ % . ' [ ?: ' W. ; kW: lh Y. ? .'.f ::.f L '.' l u n, Q m. n [, m+f l. m9;a. 4n& : ?

j

^ wm e. .~ ......... c k;5 ( g.:.;*(f.,;g: v,., n : w. j.. :.. ;..,M;_ : ~. n'.... '. T p. ' :.. .,v

, f4 Q 1 ;; L -

. y J. {; y 7 g y.. 4-y: 3 ' e *;,,.:.. : ? ;4., V.. ; ->, ~ ;. '.);; :

o.. ;4. y, ; ":f f.3. c%. )... g.;,,,,.. <f$,'. 5 l ?,

p l 4. L;-- ..hf' .,f b.] f.'h.'

??Y.l~

,.j..... ;; : ;.... 7..;..- ., g,,

.u

.\\t; 2;I Y l':' Y :< ' / ..Y ': A . h::.. ; h f l

s. h
*y e jg% _ z,..y. $j.., - a: ' )4:

ns

k... * * "::Q.V.,,p.k:hlLi:

c:[.:p. y.; f:N$& * ? f$h' y b? _ b Q$: fO {I. 0 .h

%.g &: h h?

) m m; c - .v. L..y:x.< e.w,a%..,.e. g, m. l s~ .w. 4 u. h N)..h ; Nq, h.m p u, a?.h, Mhy(*.s.5 ,,I., l

D g

,.q. 4:.

3. 4'" ws 4..

~a

e' v

f E8 Ih.s..m .y. w m: ;;;; 4 . : x ;.;c . :g. r c.

e ww w

lf . fm w s, %~,9 m e. W g~; h j xf % - [n 1 kgf h%&L i mi . u..., :.p.n.. ,u p., mf.: :. s..~.,, e n + -... 4 f Y ?fh{ c h k g_ & w # W_ y.. h 9R,.L, & M.n % ~ ^ Y3. ~ , :f-JH.LP:]C.%w. 9..; .' C y 2 L 4: c : :.~, + 5',f.c [x :: :.L;3.. [.')cf', Qf,g.1.1 w.m v 2,. 4 3}l$y& .c o;.. ? 2 ,e g,,9 ^ 'Y ~ ' Yf l ,, s,( ) k ^!

a; s. ;

..,. v.. w;.... ?,' [- ', /, 5 e , ). hl * :.'. : :...c. ; s..: ME o -

9 g, '.

,p, - $.3 :fi.,.J M(;: ;,

s.,

I showing the flange and nuts for hold-down.. ' [..g y. ~ Outside surface ofInside container, 1 + V-i . ed i 4;. 41 :. C ' i-. + s n eu . w, w. w.. w l u

a -% ass,,- mm, .-m O I 1 ,+A e . J-G.o, +f *z us ,g, $...,.,e :- - ../ } c' & j r,a fo-g,, <.,, 8 9 g

[f y

~ - {n o, -? , p.* - 2, ) . e'f{ 4 -f' =.. 3 ' ' l, i

W t )..

r ,j:. -- '. -* g .., m. ' y, , \\ ,1. ..e s - - l. -

'. M' ' u

...s g_,f- *e[s.r. e -.? f i....

~

f.,,* '* D ~ r, *', 'l W

.7f., e6' -.' s j y.j ' .l..- - ' - e-e ,,k o=,. - y .4 ."s,..* .l, 4 %., g',, 2 s ..s, a

8..pn,c o.,J [ '..,4 6.-

y l,.?.4. .: s.;!> y /A e i -M,9 ; s ~ s e ( M ; $;'f g?.% 5. d ? M.. G ; f T.' /...':G. '

f '

% 'W' Y_ s - y. 't-7 M f 5 N 4 .h. . a c ~.' M.j,, 3' '- N d. U.., .,4 % 7 M ' Q . $$ s l.l.f,l.i ~; b.f^ l*i. e,. 9 .o ~ ~ 'lf j,'2..'.,- '%q 4p..,*:s, w:<6 m... m.'.~ e : p['...,, '~ .<:,[.y' 'y o '. "- *- L-g.Qp fp..,' ' i: \\

/. * f*

h:* s l: ' E 1

' ty;; gAl Q...

i y a,,. / s -<m f Q d 'A ;. ? '?e e l . ).s! ~ '. :; ~..r. o . ;. 49t.;fj! - k g { '; L.j aw ,f v .4 . e -- ' i r %g % x,. ..f *.,.,...:',, : < ,i*.

v..,

, ?.;. b' f 4 %,R ., _ _., y.. ~1>, _3,., h.~ n.'. e.i. v. - ~- )

jf :_

.?.,~J-r- -s. r.

u u.

,yy. 1 ~ ' >'*r. g ., 2

. s i r,. "

~ f, .. ~. a c i

y ya i

t g + ? ) r e q. c. l ,0 ' tt' ,. s,c. i. -~ ~ 1 , 1.. ,.,, - / -. * .s .. g d',, ,/. .~ .,,.? ,} ? ~ is r ~ .s -r_,~. t l. ~ g a W .p s

x..

7 &, y #a',3.,..-,,,,_.,,,... v,~4 1 apes J E l,e '. ;.. ,o 8 -4 W '

.5 a.r'

.. :s.- N. 21**;' f.,.. ) y.,,N' ~f '.1, '.'p s i

f. })

k-$'*y.~,,

[

. ~ \\

$9 1

. e.. . r o,9 y o'..,.3

g.
-l' y ',,

. 5.N" ]

f f

c a, ? Y ...r 's - 1 .. c...,., p. l.. E r* (. f~u'.',..,-> ., y, a e ') l o, w

_[.

l'y I: ~ .%e y.. *', s .o., . e. > y: J' $3,fN.$ <*a?,.,*' N,,/.i.4 2* ~;y. v. -:.,.. M '1',)l; *,f . ~c >.t u;nc.q~ d ef)?...s ~,,,e--

'.y.." if~f y:n G. ^i '&; :

p. ? ',.v,' u.'. c

'% y

a ,s. ~. ,-?.~.. A - y,;. w q. '.*.,?fb".? .'" Q, l-i.f ', h;'; ary ? . i." L 7 i .., v

n. p mn.

e wwsmd* ire' w,. 1 J n WgnwSQMQf# i p;4W W YEfaQ:\\;).W.a.,.% y,n A,yQyWWw - a M. p ps. p.:g y^s m.,; s m; Q. g. % % : gem.y 72% u ~ h?kg['ko,'h*&~W.S&.a.h.fhh'a. >. n..a. v.,...n.,fl m m m.. i 4 1, Y., h er Y w.T w p,, n..:., ' i' - i M hh.,)s ?n lA.w.Y.f.:.*??.,L a 2. 'm f 3 $a. g 9'$<',? Y D.fY . yk $ f% W. L'Q&.s '.;, # . ~ w'.~ l .?: Rf f YRW'W - ~- h f. 4. ~ h

/.

.':f'=' $* 4" J %.$! bfb .h ? 2 \\ M: Y M'. $?sd. $NNeN#MiWi?gf~ w..m. %t.oa - >ser. . u. 4 i 3 ,,g =er4-N'OT- ,_,,www"7'" .-g-r"'" .---~--#'" -. - - - - ~

i .J '.>; ' ?- E N [. I . ~v ) .s.. . ~,. w. .3 "_I '_. '[

' _ 'O

' ;_ l '.' ^ .c I' _.. ' 1. c. [*_ _ - l '...;1,. 7- } '.f i ' '.d -,, ;~ e.. ' - ,~. , g. ^ . r,,:

;,.13 x...:......

g. .,.,. ~ -- +, 2 -...., ;...:.,.9 I ' .J,] .?',[. - ,, 7's '...,s' Q...s);k:s;. k*.', ?y '.,* m.*g*.,,y, %.. y * > r%f.;,on. - ..,3 . M ' 9.[^.. ' b ..;,4 ,,*j,*.,,_.,..r* q:~,g..; ;; &p p y;c.,,,n,;: s:.,. Q*

e. /

...y

...'.;* s,

-Q l Q. ..c Q;j,*,) {, ...'.; Rf ^' ' e s m.. . *y f*,L q *, j l - g.

y.,,

%,,,,W-:>.,: '.g..j n.y.~j 7, -' ;.!. 1.:,' %:y *fyJ;&;. o; l. l .._ [ _ y j .f -l A,.,. ',m..D! e.%.,' '.r ^ *a l .JQ((E - E h*'

'I. pen.**'*',E.4 v 57. '@

4.r,g.. cg,; ?y n.. f';. l . ;.y u.pr g r .. '..o , 1: #.. .k4 f y ;);.

4..,3
< e tr.**;>

3.s ; ....p, y.,, 'a. G}.*.. p,,e.~. Q y.. t* .;9 .. ~ p~l;y!. ..i.; zy '.:_s;.g.r,,f, a th}i(.. -g.,. 'W. . f *: '. ';,k.

'v.:^y*~.

.-, ':.,y.. ;; g..

z. t f- ^

...... y - e 6,;;;..,. _ e., J. E. ;; *c. - s. .7[f.,h'" "

7.fi*g 2 ff.1(:g.,,;.N{y* **[$Y.'.f,- : #.:..

,f. i,6 ' ' : ".;..,4- [4.'. r.. w4. - '.

l* *

')* 1 s. sf W.*,." 1 C'%' fQ,, t ) 9 *- % ' .w,s. r q. e[*d Fj'.

y

... c. f Dc$ c.s ...e

h.

ff 4%'~n;l'<l'm' 9 :~ "W..i ':.*yM.?..W ' y%

h. *

'g'*

i-
.' i N;;

O. et. : :r g:'. N 4' ;.e.3, W*'*:. g,.E.h c y ' ~~-. l j

..E~.

'f

e = =. ;

'V ? ' 4.,;&.... :.* A.,.. a ' a' . m, 4:.;. ;. pP,d:.,pW..,,.., M,.. l -.:.b: .c Ly,q: .; 9 - p. r; e., y,. e,;:p. *

r,s

,*..,...y. ? (.#[.,

. r .s ". mi. C : % &...V Od l:.'.-*'. %. .9 ....u_, ..* y ~ .,.y%'. 4. r.. *+,; m .-..;.~ -:.g :.. .l4 .. ~. $ s ;,. r - v+ { w& z'..:g.', ..g,' % ;/.<".;., ;, ;. - C-y.* ,,. ;l .. '. 3'g.,j.:

7.....,.. :. :,.'.. f.;. g3.; . *[l 7)...,

5 . v : y :g * 's;,. 7. . g,. - .',, *;;;.. 't. &. : ......

g.;Q > $.C.%.h

~. ?,;r. ; mj;,. gyq,..,, s. < e.. -p..;..;.' p ;..g ~, '. ... ;* ]l J, =..* s; - .~ ..F.:'. l

y

..,.p.. a. r- ' ' &s.; y u~ c :.g ga;*m. .4 l u . e4 n m.o.:;. v :..., - - c, :. ; ,.;?.:.s, a m..,.: ...,. p. ;),.. r.. ra..q Q' :.W,, 2. ~ 9. v.w ...s.(.>.<.-........

'q%.;;.A;v..,,,y..

1 .,.w.y,. a ;v.s.?. y.1...'.:o:.. n g,;:. s'p,g%< \\r.. s .l

:; ; p..

, t.

py e... s . d < d, p.. .c.. ..',e... ...%,v'... g, t g 4 .s r g. y k(g.,....,,"* ] 'll I, 'p,, 4.;,..kg

f<Y.,

e 4 l -I. [.. ,$'I'. f. I #). ) ' I, If(7 ,r h,.,,,[.,I[.)d,f:'...k . k k. y *[ /c ' =,,,*J '..I .\\ ? *ht.[ 'I Jh

3.. c:

S. '[W. K (N;, a.. f.,N :g*oy .{, '. E. j . [ ?,o.. g.. u.

... u. $.. y...

c p.; \\,,13 .J. M,. .. rj .N, "*f j I J. $ m").. ty m wuc.; ?(;*J.. u... / ~ m' :. . ; +h.[ a,.

v. x ;.mN*. 4:a/ ?}hii ' '.

.y ., [aJ.:c,j'H.. ,f of '.. V' ?.S 9:' 0 hr.h. ...'y'.f..Q, ll. u,'I..,,*ll:f'j?l;.}l.;.5 ~. A y$:i."i, ".'?. : '. 2.i.?e:. [ 4,f*'. 'N'** te.... % w:;' c.1*

",,

y

N. 4 e %. '. ' *. :; ? ? e .W,'.

- @; * :4,.,

s. tv 'h-L ,.- N:..6.Y : '.$ :9

s... p.yt ;,l:

~..

..t- .. c.s. - c-..:~. " )g ltp yy & Q.. A -...: ' N.h'. i k. '.:.. c. Y ? l*c..

l -
p **

..,..'n y g. ,p:.:;3 -... y ? ...p..,.,a;w t. 'J 'i ' - ). M.. t.w ':&.% L i. Z:._.;.:W M.*.': F. .l M.,;..- ' ' ^ -l_....l'; t. %;.. L V W:;'g e;% : L M,..',. @ &;;y;; i. :. W, .;..%.. r

n: <.: ; j.

'.. *=....*

p ;,.,.,.... F :

- ~. 9:..;- - ~ . T;; o t,a..c: ,, 2. ; %>ft .c ^. *; *. *

s A _ J.5% hs-s'

.h*.; ; ... ? : ? k. d ' Y)s ;*.. r ..'.. l'r&:'N ?.Q,f "f., ' - ::,. _ ".' p*s.'.', ,;-l:. f:, f f.Q.l.l. l:.

f..:.

.'v.g,.%.,.;.'*:, e .,,l.;.s la* .,. l. ;. ;.L;;. ' h: .%*f,. o -'.. Y ., *: 4., g",%x ;.c:.... ~. > :. n :~ n t.r:;:L; p L.

r

'. : 4 d:. t . ' 4.:~, ^ - s.P ., ~ **:.. tyw: ':q.:a......, G. t,Y ..' e.

n. 4,.../..y.f..:.,m; p;.:..N f. # ;%a.,' J... :. ::.. ';. ~ - n.."

. :.. n.-:

. C s

c. l

- * :, n ',,i. ..%. '. r.,k.,, ;.g..,. ;.... J.... .,Q f. -,,'.,m.. t y - . - e. f -. g..*? c%. :p .::..l.'. s.. :; g*. n? q.s,; -q.,....:;' l s f *q ".:c

s. c A

'., ?s n'.Q', d... J. . ra, w .,'.g.g ;.p.., y&. 4

d. '

4 .. 2... P 1 w,.~ f~ %,.. f; . -.n v ..,.,z:.;z., :: ~ i, . h. n.. ' <l;', . V.: .n s. U.3 ~;, ?,,. g, f ; 7 ..,,,t.,y;, 4 .. 7..,. ; ,%g. p :,, '? :. : s . - e .,Jyr %e : ;.,.ry ;:e.s n - s .a...

..g r.y ' *~.

p L s.,.4,.c& :f.4,. y,. g. : ' 2 .s.. e . y)';f*Wlf I' ) ? .. :.)

j,'

+. ,,h...'5., c' Y. ')a.s.l: :l.? l -n...l ', L. ? [, *' ' ' I. l' ?,. . *,.........:.,,:...( ch,,e 6.*** J.)} ? [ f j %,'e[, ' &;. {w .. ~ rm ~ -...n C.:,. ". ' g*?:,1 ': '.

.9*p '. <' ': :.. ;%. ;.?

..b E . * **y.f{. ' e.[ L fN.3.hd[pl{ f.' - h. j. J y ic 4 ,.:P f' j ., y. y# ,,.h 4 , ~. o. y % q.7g,

n. m WNwMe@f-[M' ;;,kh Mg^jk.

MME%d,.,dth,,, L blk h 4 l,iM8,[hp%... M, J.'y'[', } t 4,. a nnes{f lw l MhCBMig_p..;'gj A"$ igg j u..=t. _P.g.g' .g ,7, p r. g

, va: -

3.'.,'. .J. ? Top surface (faces up) of foam plug. .. ~

'.. ' ' '. -] P.d. ,,1

] ',,,

.( (. P ~ y_. 9._ '. ' &y ~ i ~ '3 ; j '. ?_ ^_._.~.._[ _.y

^

'*f. ? i ' :-_ _ i... -._. _ '- ..g:: - ? [ "? ' 9.. 1* 1., ..!,g.; .y \\ ... - ' ~..__ ~,'s ,s

p;

~ * .a. x; ' _. ;., jy t;_ q -7....., .y- - h e. __ e '.' aP , :5.... ..... -, 3..., - _i ~ [' _ [- . [ :. ' ~. . p * ^

l* *.[

, *..,*}., g'. .lL : - '. ~f \\.j ^ .. c. g.. [,' I..

1. 1

) '- ** '.?Q,.4, . h.;.s,.. ;, q ; . p.,,,., - ....; p . ~. q .a* . g 1:.1. n $~... a._ - _,c.. , % L. n l..;., g f;. l:. n. :...%.>;a. *.' g,;. y q'. -* ;,. ! O A ?: .,.;*;. :... :.. ~. y ;. s, 4.*,

.y - s.

' * : W. ... ' W' ' ;- j.

.. -.~ % ; r:?, :: _
1 p ' ' *
y. -..
l 9),% -

n .1 - ~. f. r-q$lr, 1l.'8.s. y, ' c ..,%,g.g e .s.*. $ r*.i *.,>. :. 3 '. ',. _ ', ~ ',. g C' Qw .J'__. s r ?! *>.Q'!f.: '$Y? g & *k '? f.? l Wrg l,T h' /. 1j . f..$ 5. *j +.,, ;l*Y.( Q *- Q.',' '.:' ;.tG ~ ** '. } ;.;- ] '. ~.-* 4 1- ' Y.. * ).. ' '

.. : y

,. ll k y '.,; g* " g I ** r.$..., !.. *4 g .. ;. 1., - ' re.,r. v * ;;.9 A s. n . 4;e ' 'y. -:,

9. e

.'l-*e,- S pr, -*A,.,. si. -

's ? *.i. * '* e.*,"y.

. s, ^ ?

. ::.'. '.? =

. 's .se' Tfe f

l'

~. D

t f.;*

,' ? G.. '. '.;- '? ';.* fE * $*; :, Q.*.6 I..' R.'..,py., ' .' i, i ...( yfs -, p%*,. ' ..e, o y,, ge,.. 't : ....p r . K' : _.-n'. &:.,y!&,.:*:'l;:.

- S,:.l. ~' )4

'... &S S. ' *.(,.' ' ',.e.

..

h :h!s. ' N: A

' '..%i
^ '

s 'f

1'~...Y,+

w;;n..,i. R;,.gh;.'**y.. _. ' J.. *. y '.p.'.,.,. .y.e. 3 M - ~ W *- - .,..[..'.' ',.j;_. + : .. s. ^l',.h<y{,l. ! h;. -y ~ :.). }g.p;,4.p.[..;. n [......... '... _ : [_, : a ;q,. . :.y. -. "t .k- ~

., g.]

n y.;. . :.e. u._.,._. f. . -. 1 g: y z. g.... ; - l,. [. [:l l*..

..j* -

- ' " -" !. b. ?. 2 .. sc _ a.N:. l.T .:.,. M ':.. *.. L.... - . :. ' 'l'L.; l...... _ *j* ^.. u

. ~ -.

7 'a ,In y )f. :,;.. ;- ,.. '. p$l ' *-.~' . $.Q$ '

f.

'n. " 0 {,. '.Q l-:f.. l.'.,5(r. Q ? ?; -*[-3 or

6

../. k o...-' - ' '..'^'.e g '\\ - Y 'h '- {. : . 'L _ ] s. r3. *... - .J. ) ' & ;.9 S. q.

% ;., -l.,b :(- i.' ' '. :., '

., 9 ' ;._ :.. L ' ' '..L lpftj[ ; ; ..J u. . ;. '. Y.. _

.$ '~}prJ.i%.h._l;..*.(v).... ':}.s... !.Eg...!

(, I:, f _ * ; 'r'.'... Q.. * ' '. A. ; $.M ~ if * " ; >l l . oc f.. -....... .Y.,.h*, .O ' U'.' j.o. :, V.h h. s .}.;n$l'r.o. ' ':ge.w'k'. l -W

Y."

.N .. v . w r < ew - /. .~ ~ r T*. n ?.: +

~

c.. ! s 14.. } .. y. ;.,;. k N .jl f'. . ; lW :2.1.v;,./. h $!.r.: h}.,.. h;;% W. .u .x a. .. r k.h n - T..:. '. (. &p.,(?MN..k h....hq.%. .).y... g$q[f ;O W.c ,9[.[h.* .I 3 h.MIY.

q. 3;(. / ' ;.n.. '....

i :; ..e.-..: N l iq% W..m.. 3...m 3 3.c... 4 .. m.. k_ if M &.Ml ? 'W.ls. 9 Q ?; !i. J..,f. %... % y 'i. i y.L:~ [ c.

1 & W r $

.!p.r ;,;3 p;:l $, g?;,f, h..;. .^ k g_ *. N.' J:t ;-. vf .C;' *. ~ r p.: L2 p g.. an %f f. . :... ? '. w '., W.* ; %.C@.T..hw *g_1.h:. o - = ,_ ~il. .g 4 :: %_...- gag, * *Q. vy' ~: .9.*... : : : -L4. - ; o. 1 f s G:'.W.p.v)L v .+ > :<. ... ;;u;;;" '. ' - '9;

4.,r q y,,:rg.

.r _.. l ". t.g;~(:...':...r s 2 F.:: n

.n-v :- ".

. p.4 =- ' w.,. - [*.. } ,y e N ~ 1 ~ l L' ,$h- @ $.? e $%;$JW.* h( 6.1. g 4' ) V W-= :sph.p :

c. 4 3. i... J (.:.7 h Q* y

$p: %.:), A.

^ * *, *qQ %g.kx.-. ' d. m, ^

m. :#

A h. . ex:t.a y.h.s&y3 %:. :.~ Q n.. g_

W, w*7 r.

m+9 L . s* j 4: W L'; my W;.Q.i w.n3h.' . f$.k.g %h k fM ..h'}... 4 ,. j r.

f.

..c ~ p.s..s s k "h,sQ h $lgy.:.' l

12
:... t g 3, -

.. m.Q .4 he W5 J. s. .t y i, + M,. y >.:,. M D R.- g y) 9 ' _ g', pQg@QQ q.f.(g;f. ; Bottom surface of foam plug. ' y. MP - g,e .t. . Pj: l. j, ~.;- ;.

x

---w.i.

~n _ - ~.. - _,. _. _~-- - -- _,-._ _ -~ _ _- 3 i e l. ., b' s i ')'.g,.' ' '. f ' ^.' .L- - W* ' 'i..' l l ^.' I 'R'y n' d * :,'.;. & l# '.e. *.,- ', ? ' ?,

4. f,

...s'.' ';w= 2 ','.. :. '....,.. ;, h '_A Se E 4 .d. .lh, ?.%-lf,g,f. ' f.:lf, j' ?,j,/[f..hl1, l, I,. l .llf.l_~l] & & )* $ $^

l

,f k' l l '.'. ' s ' R..v *...* *.. I ~ Y.lg 1: '.e _, "'. NF = 'I' l.h,D$.4 ,p *g.,.",; - l; ' ' ', 9..., tg ..... Jr.g P n ? 'h : 1 3...; ,e s, ' e. t e M .c /g, e 1' 7, rw ? ..f., ..,T ',I r.r ' ,[...[.h',.R Wd 0'Y;::. M '.\\, ',',;, 'l

J.9%.' (: ..q.Qs.A3*C:n. E' M-5':;:2

... 1. 9*' ^ % ky.h M.@}h p :7,. G,".:_d' Y.R[Iak e.' ll(. > ; 'g,,}f '?p ' ;'.. h.,, e.,j # < *.'(V*' llf..p Oj' $Q. a n.. 'V.*- s'.**'. * *f'

- ?l y,'*

V. f. ' lY *' '*... ;;

y.

,, g ' 214

y

[. _ p*. '.}{,l-y ..h' b, ' ' in '. r. .: l e <C- .o + .' l, ? l' ie f;'l$ n _ Q'

s'-

S - ...t' [,.,p' l'. .#' V

4

.:*i';.'4 h?. '. 0 l' l _ . $.M ?". = * ' yM ['c.,, 4" % - '. '. /f..,. ', - * 'g to 1 ) l- }P.- [' P. k, k,[ */ ( :- [.. + g' e p W,,w.,..,J s,n m'I.m.c : ,I .m.qx"* #~w'

w'}*; ;

'. '..,' ;,' ' ' ll, 8 2'

x.Mgle,6

I* ,g y e' s ~5 j he N? . ' af%, .',.fr x,.... g.n g,' ' *.. ylc'.,. ' '.. ; 4.'b,0 . w p'7' h:'h.,.7,, J -..y, f.).n.s','.. e',, - ;,.. .":,e

gr*, ' i3.;
f X ',

d.. * ; -:., * '

g. y 4

1.' p~p. . i)./ , 7. w' 'I. i 1 y .. fy< -' p"? ' ';p,4,,,m] '*.=.. '..3.. - ;. l.-.*..; y, /g.. '3 .i; 5,h+t l . 2 F.,, e4 ,,g. g i g. >", A ye* ,,j ' '. i. 'Jq "., t;. ,,C

-;..,,. i: ;

.g .!*.*,2' .e,. '8' .c g., =, * ;._ - ( ; e.f ' *. ' ' ' l Y .p: .,, ' ' ; n h:. ,'_;+.M: '. y e,,* , n,[ k 1

v.,..

._,;3 ' * 'i. _. ,, q;. 0.'. W'. ' , 'd;,;,;,,,l ,N W[' g h 't .. ' ?,. ,?' ^ .a. 5 l

8,

. f, ..'l .,I... i.<t. I . jg5 ( l g.y.,f' ' 2. C ' [ d .,I _'.jg* '..'7= '};.'

. L ]

a:. - ' %[ (,..,* r. 4>r - 3, . ;./ I,' ' ' g. " ' &, s ch k. ', /. - Y.*.*.*. '. .t.* ',b..[.. * ' ' .., ]. 'h ', O i ?- [. c 8 . '. jB ((?: ' j, g}.{. -.' c r, i .5. .,.

4 e*".M."*.':

,' _.9 y...?n ....R n'

. *.l',. :

} ', : 9, l. .L,. ~%. - :' ,,, }t

)

. f.:.' * ' ' _ c. *,,,-;z'.,.,- ,;p.V.'> ~.*.%, /,o, f. - .L.,# ,..N...,*g'- ..,*3 ; e .'.*..e. y

3.

~-.,c_ ,-4s.T ;qm...,4,. * ".e

4. Tavi -,. ;.

.,3 ._.3,p cd 4. w- ,.'g.. A.., _M..,, tg *

N,::s,. U f:.y'
y:.. '.. O. N

.#, n. ,.3 i I ; '. .b f* 4. 8[,, .- 4 ? {.. /.. -,; ; i.. 1 -,',/.,: l- i'

&'.x.Y g 6..%..sn'*.: 4.t y j.'.*

'f.

R 9es;*. m.':.

O ,; e *, ~. . fr.% - .$. __1 ,o g lR,. N ', '.7.,.k.f p W '{.. - ? ,i.a <r, Q. (,I _'f.'{.. ' :' '; -lW,,-.,,.4-~ %:. l 4..* ,~@..1. s ;, j; '. 0 j.'. e ,,;ese;;; q: - e o 4 ' ', :,, &. ; t., '. k..' :l :. :...,'.,;iY h 't ;,, f...y,, ' 9 A .r. /.,,.,9, 4,';.*. g4q, ,.. y 5, - ,g,; 7,

l. '

sg '. l; p.', ,.g. . h, - y' Q.Nk. '.f. I,* e. l $, :

6 k # I ' ' i. ; ' " 'l*.

. e t ; > 4,'-l,3: - :.;,.,

E'..] I h *y*- ., [' 7[. .[. I:, .[* kg 1,. ' '.,. a e _ ','/..In[* $ 'I",. ' y, '. ^[ T '. - ,4,f'S A* K

%.\\ - (

i s .

., g ',. Q. *

. ?* ] fis >"y.* gn. c., >.-. '.. ',; ;';. c .% :*- ;, e: . '., b. im p,' ! - .4eme 9* v g. *. r* g-e, sf 1 ..4 n.. ,Y ,-t. . A.r, g.., k', ' ' p s n ';~.. 'w' 'k)mll t: Lp, l.. ?.$.)~; !Y '. - ll,Y' '.,lY.

4' s, k

,_f,) ,.. f' n ~ c W_ gl.n, a,.;lst'~. Ol.- An', w. ~. :;,:

9..' x' :n

v. ~g =:.. '.. ;..

'W

t..lm'..[-

c. ;;.. ~ n

. n @ n.::.s.. ~. Y. .~. .n - W+g&; ;&,s, v.~n;;3 n,..*, wg;M[m,i.y.g%,;%9y&n'u. p::.i#,'Wj n;. : 3,

m.

pg.. ,r:.n v.y.g., '. f3.. 3 ;. E Q.'g ..;;;e b V;g M. J _6i M. g.H g $ + N!nd. g p q.. a%Pm. W M ; '. " u" n.t s:4g$v.. -n.,pe, :' l' 3.,,, ~i a+ "o,. x. : %. w n.. i,, n '.,n.d :.,... .,. n*: d.: c*,A.ll...n. v,(.) : : y.;e ',... 'o ' :.2 e c ., s;.

w..

,.,. f. .7. f.j %n.o 4.4 ,,"_-3.,. . - if.... '... ..4..'4 .s. .. % ; / _^.. 4 t y,.... ",.... s ' yeyo. z '.9 : '. Q 'lf. . ',, C.:..i J' ' . d.

4. :g,... y." ri -.-

7.. >.m. , %'. .,4 2,f; M, .. T M - v. ',. e;,, __d..- 3* 'A ! ;.; ^ y,.:- [ ff :..G. 7 ,,.:i J;~;. 4...P - g,L..:: g ,,,I ~ 4 :; y. 'y%. gN, *e.3. ;,.9.tm..'.y,

%"W:, :'. ; ". ;..,*4f.L..;

^, ;, e 7 W '. (.n,.:h. xf.... l._ Q'. ". ". ' .Q ;;4... ;,1.. -[G'4Lf..,*[. ':.[IQ :. .'. l' . :,...y ' g...

z.,.

.... 7 . c 7-

w. s..

~ qp..... ummesegg$e$r W_fi) l,f m.k'.5e c 1 4,h,h Y.0 _.Y. Mgy_ps~,)al.??nlcl l;f.h.n h:. ~ ;l;'.lg-l: :l{: mgeW h; 4.;. w u % ;- ;:%d - Q..%g,)f. 44,, 4:.y 9_h hf } $ 'y:;;.f.; W l .N. .i Y g %gyyz51 qq

.7: .

.ygyLym; . y;;y \\ ;y;q%m;{L&,.& q. m d h. d,5. W;; 3 2 & :.93 p. :. l w a & w n m) h k h i O. M $ $ m QMQ ? %W wmmMc a v AWWy MMMkN56 h$f . b wmma n d w.a m. gp . a + w n m.aa.n.n.o?. nmr E O:fYW i M W,f;f 'I',h. h. &' hh, w;.' 'f x.l g\\:h.:s. ? ll.& f lY *R'.$ f l %W LYS T ?,Y: f 3 f ^ V, &'~' G M [& n M W:D d N ;!. M f* W AD& 1

13

$.bN:k N E N, lYliii.kN Inner container lid, bolt, & wuher, in-B WM WMS n. 1

~ ...._...-n /- 'd .f ^ U Yb 4 [ f .?: Gg'.s ;.p *.}g g,g*g.'j.y-ldy:v'[ wt;f*l& & - h' Y f.?}.. } E Q[$h.;' c ' f; *;.*, ' i - ' }.

/1...,f ? : f.

h l. v.}.'. f.y.

9..

kN c'

A*

,. ; # - f y:.J:.. L W 'M.F W % M$ V ', j.Q ' :j.f, ;. ;. :. ? 9 : ?.Q & .F ' W ^ f.* U. : $ 3,f,yy.y&. ? J:(. s '. ; ;' V ' C } :;-( l 9.:.. 4 4 .gQ ', .. g.. p.b Y #, -

v. c,

s,; f 4 'ky'. J._

~..y g.y &;,, e 3.,.y

~ :. ,.,) j. y, _,y* y :c.t:

^ '#a A. w.. - - w

. M ,7.f y;- y% .w ;t.y *.o.....:......... ',* :,. c.h. 3 ..ee,. n 1

;.o c;

{ g. 2 m .S. . ;T . ;, 3 f. 3 ,Q..s_ _ 4; 1 _p*~-

g;,.~SM.h $(;^ M.: g 4((V[Nh:.[p.y.',.3.[,3.( y,Q,

.$, ) 3~t 14 g " ~ . ' 1, -. '.y .s I% N:

i. 3 I.7 M j.f. k (

' i,q ~IT 1 Eh@%y::y.eQ '% % nefs* Q,Q; .:}.. s.g .=..T.6 .4 h. - $ '~

k. N A W

.. ]l v A'.*s: A.. y A.'<..;?. ;,yal.....:-) ;_p h. y ; %;-q:.. ^ %,*;i n 6

V o..

?; !.w )%h 6% W.e% ;... b. 3. g*,. alp # @...w+ e. tam. ;M....N..rA.....?. s?...;. w a f .f y...,p. >. n u g.. v f

}.

..s ,i..... j$ y}., ~ " * ' I . y~*.. : h.9 q lQ"..yl _ .1.* y . i [.,'* ; ** ;

.y.j '. 7;..{ *,e.

^ %.. ;.:: ' _ ( K. ' *:; G.*' ;*, ... f. y.,@..f'* l :. y.,.,- J q*~ ,,..v...,.._ '.ii e,,.t ' f.gk,,j:.,.:; r.f..,. g Jo '.g ,n .%.7" . g > x, p - de

, '. % ',

.g n.

n,

., r;,.c.. .';. n;:

y,. _,

l .s.. c L; A s p.y, \\. 1, 'A'. p.-,* .n; ' s ge> ,.d a..- g w; e, $"*t '.M, d."y ; C,. ; '

y. Ds,y ag;.it;j..L*,

~. ' g. 9' M, v.', A,Q'. - :. Y ::__.,: J....:. ' .. _... ':.,, ; J v ',.,.. 1

3. 4

. *s...: .. %,. ; _:";j ?. ' f,A 'i y..g:yr,, C, . '*; }*.ll. &' ?, l;

A.: fflg* *:,f f ; '

4,, .."?... .i.. , }, ! -( J. + lf k.& Y;(l'.l g*k ' A}.I.. ?,,.*L l.' ': ' ' [:.' ; ;.;':y '_ _ _~ E '*). 1,;._, ?..

[

' ' f, R*':.~.'*by._;) !; 'lp f,**l.

b :.):.l_

y. [ ^...l.

:.. #?. _ [;.., [,. ' ' {

.e.. ; m, f? \\..

-;. gy;. }..ls{. j' }. _

.,l e f,.I * ' . *k _ ', [, ,. [, 4.; I, .I:. ' 2 ' ,"..f4. " ' ; .[. .;g. U h ;h'f.')..h*jg # *;..h hh ',,, *. 'd. [ * ' h;.j. ,,, -. I[.

.C.,[.f:' E['

A Q,,f ' /N.* %*.=~i'

!

h*

6 ', ' ;. M sr ' [.# t ~ [; .b... .. ge.. .';...*-n,. - jTt [ - ' [ '. - - *r:.. 3., .y s.3 y r pf c *., -l ; ~.: . ge 4 )., . ',...:*.;"E

g.,;... -

g-4,. ' ' 'e

., Q ' ;.' (: [l.([ f.f. e. 2,..,N l: ",. !-[; Y.).'j :.

hh.,. ~ A._.'&f, ,y.. lr!.&f,.eh}; 'j .~-k .e ? 1 .,. ~. -..q.&.. ., },,*- ..m. - n:,r] g: .N <? ;, a w.. .. R._ * - ** ~.. _.[f. ~. sg, q .. ;.. I. :..p;.._..,...., n.,.. ;4 f,,.. ) % :........... sw'. ': s' r 4 h.. g....,w.. ; t.y. - } :... fj ....=i. 4,_9... i q._ ? *w.. n 6. l". o s e .y.. e n y

m &{ w..} %

A.w...g 4. *+M .m' '..;. ; s:. Q. ;%.,~:) <. k.a v mWm_.m,..;w w w w' .p. .w.,

... m. 14. e..... n.. :.,.. : *...,. }.uww, o.r.w.

.. w fI; g*.

m.,.,.. +w.', w f n, y&, ::r

?.w,~~:a 4 '., c.: e -.. . : y:, _; )..' ~. sy' * - ff:_l.,::..'. a;a t.?;; k D E 'f: f f 4:h. 4.:>,u a..- .y e M t r- }N. f f G._f$ k.. m;:2yhk hY .: ::n.. .a

f. y.,w,b.

&{ ' Q ff,7 *i.',.GA,,M.W. pw{f. L. .v.. l; N /w ;'.wlv f w g:/./.- w%. e ~. w +. : wn m.R 9 Y';..,53 fL..M ~.r / .g c. 3.f.) h M ' 3. : - '. ...!*' Y *";.;i. f: ~-

.7.m,*;

5,.W. o,. - je....... .. N.

1...,u'o-

,w,. e.. .5 .I. 0 W:. f '. l.

f,.' bi N.'

.?'b ':.. x.. '. ' i .,$$h l Sk i, l :^-l::.."?-k? W hI ~w,.n n.w y Kl'_l. :?. f. L? j

,_ ' W y. $ :l.l. : ?, )

w ., e m a. n; y.. n.. ~ y, n,&p {l: Q h. % & y ~ ..m. .m a . w .x }m, 'O .y;? l h gQ yng~d,}$.[f- . jf.p},4 g}f 4y4 f 3 '..? .3: f ' g(,g.p gen f.;.: (g.;..( Q 7 QQ gQ~$g Q }FQQ s a $ n - Q...;$';.j "; y_f f _j- .f ). . f.f.}Q ... ll~ l l~l[.l, nhh f ~. f: G r A:..& e';hi.m.:;.y; m m m.=y.j yl2; m.:z w.~. ex ~ we% N:.l: l';. q&....y g m C. .r e+ m

3 ;?: y -: A.Y-...."u'W...;'.' *.. :,:. V * :1 : ' '..:, l,

.~ ',l. '. G l;. Q. - 'f?. j%.. m.'w'Q*4. y...l.Y.,n....>;. [,%,..*v,.* I .l. : -

i i

.. ' l " '.I I r

A ^ ..g . m y .,.,. u;., - 't: -. q. T._ y.*.g: p,: *i. ';, ;f :l).,; ' l; ' c.,. _.... 4. .., _..... T.? *:: u : ):. b:.

&y -

. 3 , ' n: .~ n. ' y : 's ... ~,.... ~.c s.. "..I + e.t : .u s , r; u.?..... g. I b; .f

Y..

+. g... n n, 4 db.1H&;E.(4,kr:kl$.%.N [.jh,..: ; f l";*. l lc.c. < <.+. v x./ +.- .')l.;. l...l : '. :.K.ll. '.l:,,;.ly m. s.. ? t .gc _ '*','p9.'...,,'_ l Q.<.*,. .?'*'d'. ). a' _ _ ' +, ' "{y';;;.. -... ~., /. i * ;..,.,'.N*, '. i '- } 7. ;.dd*.'t, ', '... .u j ,.._y .y#..:. m> ( ' y. ' : j' }..: ' }. L, L _..;

g..;,

. yg. y';(,;n,.... :[. ;. ,. ;; L : f,,,.,:(g :;.q:~ ;.y ;:.. - : g, e... ..at.,

>y '

m . j...... ::. ; $. s, ;. ,.(._., a:....:L. ;;y: ;;~ l M.;p&y Q,qlW:t1. g,J;.yJ .e / ..r,.. .w. j p,p w w

.. ;...e ~

Same bolt & washer as shown in #13. w ,y+ .(ps - p ...ntw /, e. : : ~ .s v. _ _. ;.,. ;. 7. v ..r....p

8 l j 0 v.c w , 49 0 ~' bt N,.e..h _ y Yh(k .i l fg.. y e .n .r* ,. J %,* i.. v ,y,- 'l A . ? ?.- [ f .M ,.3. [k ._'l-4, f.', 4' s . thl 4 j ..j ( *f ' ., 4. jr e. ( .[ C# ~ - 55'. 4 .,. ;, 9.r. j 4M.2 ?1 g3

h ' Yhf..;,,

f.k.g$h

e. ;f.-

~ ' 5. *.

1s
b,- T,, -:..

y-. * - :. y 4 p,.' V

a 4

.r- ' 'V - ..*V /r bY i hk'. . J-t 4 bM,,ft {'f d $Y. ik.x . l _

;l}j.

a. -~

kgM'i)4,)

~ MN W

4e pw.1 mpe mg

. 2 e

%w. . g < S.,' 3..[. eg#'M ...Q,M:. y . s.a.. A e, a, yUlg sf'd'i.*-i[,.*2',f a' .h g! V4'Iy.# c l 4 - v W f y, *,hp. j -14,. e,.,. .{. $tdk[Q3p 4, \\.,.y;.g^IN{ ~ }1 'h px?d, ') i t y 4 yc.'Y$. \\ Y )V 4 .n. , :.?;4

1 -

q.j',m /leq 5 , ~ e ~,, , 'x,. ~ ~* h ~ ',..;@l.W c.*.M'??{a:' "$n.i.# ' \\ n... i ;'*.,;., 4./ Y ;4. v s.? M.,,$, %*A.., v .a ' NM'~ .;i; gf / '.Q,A*I?f i'fSE /AP'O h ' %'s. . ) y f1 ' 5'fl,~;g el.. Mk' ,.{ ~ Y-

J.

r ? -- ' .,. s,b c-A % ). . X7.Y.." y - .:.w:.,. w a ./: r.. .t x t.;. .i( . ; p.- $5' Yh'Y'} .f.$ $N*-h y ~.&^ ~ n-j _.. W; ? v.s .- x ?.tt. :p :r. " ~%. : ~ i ?'t.f 3%q;,m* f.f.}, 'k;,,[fI .) -m ~.

c.

~..; bhah 1 t

rs m,,,.,-

...... :.a : w. ';'.:W:k....::",.:.,. s,...- f:'e' u t. ~. :..

15

"[*k,: gD,, ~E d ~ ','. 5( * ' ' ' * ~ Inside surface of lid of 55-gal. Outer ,7h 'l _..

s.'c.ee S ^ i:

container. 4 " ' ~ X. .J

p. Director Office ofNuclear Material Safety & Safeguards February 10,1999 (- Page1of1 Specification NCI - BU-7, Rev. 0

E 1 W " 3.5 g NUCLEARCONTAINERS,1NC. arzAssrarON,7N SPECIPICA110NNo.: NCI-BU 7 PROCEDURETYPE: MATERIAL AND EQUIPMENT SPECEICA110N DESCRIPTION: BU-7 FHENOUCFOAM SPBCIFICAT10N His page is a secord ofrevisions to this procedure. Ramm* fadicane a briefdescription of ths sevision and are not a part of the,_ - - N 1 AFFECTED i RIMSION DAIE PAGE (n) Rend &REE i i e' j 0 7/28/95 ALL ORIGINAL 4 i 1 i I l I l l i 4 APPROVALS q i ts. % A. M tnn %.W n O)OL-1 / - 1 i QA MANAGER OERGONS MANAGER FRENDENT 4 4 f i i i I j j l

Page1cf3 -NCI-BU-7, Rev. 0 t 1. This specification shall cover materials and procedures for mixing and applying foamed-in-place fire resistant phenolic foam with a density range of 7-30 lbs/cu.ft.. Materials All materials used in this phenolic foam shall be as listed below. Any substitutiens not listed ~ shall require approval of the appropriate authority prior to use in a specification package. l Material Snecification Component Wt. % ' Phenolic Resin Schenectady Chemical Company 65.8*0.2

HRJ-l1825 Surfactant Dow Coming DC-193 2.00.1 1,1,2 trichloro-1,2,2-C Cl F 6.6*0.1 2 33 trifluordethane Boric anhydride B0 8.0 min.

2 3 Practical grade or better (-50 mesh size) Oxalic Acid H C 0.2H O 8.2*0.1 2 3 2 Technical grade or better ~ Fiberglass rovings - Coated for compatibility 9.6*0.4 1/4" chopped length with phenolic resin (Owens Coming 405)

NOTE:

Phenolic resins are required to have a chloride content ofless than 300 ppm. Prior to use the chloride content shall be verified by an independent laboratory. Storage Requirements Phenolic Resin 1. Store in airtight storage containers, j 2. Maximum shelflife at an average temperature below 80*F is three months from date of I receipt. l 4 w

Page 2 of 3 NCI BU-7, Rev. 0 (a Maximum shelflife at a temperature of 40*5'F is six months from date of manufacture. 3. NOTE: These dates shall be marked on the storage container or manufacturer's certificates as required. All Other Materiata 1. All other materials shall be stored at room temperature in properly sealed containers until ready for use in a manner to prevent contact with moisture. 2. Shelflife should be as recommended by the chemical manufacturer. p e.otacles f Receptacles shall be secured and anchored as necessary to prevent distortion by the foam and should have vent holes to prevent voids in the finished foam and to provide gas relief, as defined by the applicable drawings. In the event molds are used, they shall have a mold release applied to the surface or shall be coated with a permanent release coating prior to being filled with foam to facilitate the release of the foam from the mold. Container components in contact with foam components shall have a coating (i&, zinc epoxy primer, etc.') applied to act as an additional barrier between the foam and the. container. This coating shall be applied in not less than 4 mils wet thickr ass as determined.ath a paint gauge or less than 1% mils dry thickness as determined by a dry thickness gauge. Surfaces shall be inspected prior to the foaming operation by inspection personnel. ' NOTE: Zine epoxy primers are currently being used although other coatings may be used if they prove to provide better protection. Cleanine Before Foamino l Receptacles shall be free from foreign particles prior to the foam material being applied. Temneratures 1. Receptacles shall be at room temperature, but not less than 60*F. 2. Chemicals shall be at a minimum temperature of 60'F when mixed for foaming. 3. The air temperature shall not be less than 60*F. Mirino 1. Add liquid components to the mixer tub and stir to a uniform consistency for a minimum of 30 seconds. 2. Add all other powder components and mix to a uniform consistency for 1 to 2 minutes. 3. Add fiberglass and mix no longer than necessary to achieve a uniform consistency.

r Page 3 of 3 NCloBU-7, Rev. 0 4. Transfer the mixed raw materials quickly to the receptacle so that the foaming action takes place in the receptacle. Placing Fnam Material i The mixed foam material should be spread evenly over the bottom of the receptacle so that the foam expands in relatively level, uniform layers. When multiple pours are required, the first layer shall be tamped as necessary to control the height of the foam, thus controlling the foam density. Sequential pours should be spread evenly over the initial layer after foaming action of the first pour is complete. l Remnval of Rracing l All bracing, molds or accessories not part of the Snished product as defined by the drawings shall be removed after foaming and hardening are complete. l Watamenofing Seal all holes in the outer surface where applicable (e.g., vent holes, nail and screw holes, etc.) with RTV silicone caulking and caplugs as required by the drawings. All molded foam products { or exposed foam surfaces shall be scaled using tworpats of epoxy primer prior to any finish coat j of paint as required. l QA Prior to production of each product Quality Assurance or Engineering shall establish the correct weight of the foam materials required to produce the correct density. Quality Assurance shall verify that the density of the foam installed in each package is that which is required by dividing the difference in package weight before and after the foaming operation by the volume of the foam cavity. Patching i Voids in the finished foam surfaces shall be patched by filling with additional foam raw material and allowing the material to expand and cure. Small imperfections may be filled using automotive or other compatible fillers prior to painting. j Records - A foaming record must be completed for foaming operations ofindividual packages and shall become a part of the final QA Record. This isord shall include at a minimum: foam components, weights before and after foaming, t nd QA verifications. i i l

i.- ' Director. l Office of Nuclear Material Safety & Safeguards February 10,1999 (, Page1ofI l i l LAW Engineering Test Report Dated 2/1/99 s 4 i l t i 1 l l l

- _ ~.... _. -. - ~. .--..~ -.-~... -~ ~ 2-2-est esS6PMIEco-PGu Spec. Pas 8423 543 421e e 2/ 36 j FEB 82 '99 138 83 PR LAhl EH3 It@ SUCS 784 357 BELT. P TO 1as235436EEr7 P 82/15 3 LAW ~ ]( LAWGIB8 Group IIember 3 ) 7 February 1,1999 Mr.Mks Arnold Emo-Pak Speciah Paclaging i 1251odma way,seits a sm,TN 2M43 1 i j Subject Anshuis of While h and Paint Chips i M Speede% Packaging i Eumbeehema,TM l IJ25 Projoet188mS7883 Phase 96 t Deer b6. Arnold: 1 In occardamos wrish yow Purehese outer Number 514, Lew Eagneerug nodeskul Services l (Leis) has completed laboreenry analysis of a _ white resishes and paint ships abinined tesa a j eentenner. Tids report oossains objective, test procedures and soeuks. I i l Objeselve of Study The objective cf this analysis was to *= mis = the white residae and the palet chips provided to deteremns the meters of tbs residue and to determine Ibe organic fbnctionality and inorganic content of the paint ship. X-rey Dnnonom (XRD), X-ray Fluorescamce (XRF) Spmy, light i elsument EasrEy Dispersive 5;_r1:;, (EDS), and Founer Transform Infrared (FDK) Spectroseepy were techniques used in this malysis, i, TestPressemos XRD Anahuis e Tbs whies resides was greemd and pleosd onto a "asro" background quarte plate aseng a non-crysebline a4:ssive. The semple was them phoed into Ibc dif>+-e=r and a specarest acquised over a 2-Deta range froan 2 doyees to 10 doyees. De snaple was opua to reduos pruibrred OricIRatiOS Ch LAW Ecginsestse ineusetal Services 2001 Yeernent F.and, Sets 200

Charlser, f0C 2e20s P.O. hear 19057
Chartste, IGC 20219 70635F4I00
Fat 706-as74s37

' FEB B2 '99 13853 FR LAIJ EMi l>0 SUCS 794 357 8637 TO 142Eweesr7 P.83/15 4 anspotaseek m y,e,rpasimesir emeneryv.vses i AssMask ifeefooJese MuseoN (- { XRPAnahsis The son.due was plan =1 hto a polypropylene sample cup wilk a Preises flha bosom. R was than placed in to XRF sysse and sposes sneerstod ming a gennesiuan (Go) ::: -i target. f j Basemental peaks were identified and the spacen plooed. The XRF analysis neothed for the j peine ship semples was idemmat t. en aw=. m ship,es pissed into the empio emp, pakt j side dern. Dutt milection proomsdsd as above, spect abus seconday targem of vanadium (V) j and gennanian (Gd) mal a shadium (Rh) primary target was used. F11R Analysis For the, the whies sosidue was unsumined under a.;., : -_'- __ :;: and a single men removed a j and placed onto a Nacl window.1he window was then placed in a Specta Tech IR-Fins Aeslytical microscope ansched to a Nicolet 520 opdcal beach and FT1R analysis symse. A ~ d spesensa was acaguired as the son of 32 scans with 2en neolstion.1be spectnen was j ---1,__.: with the Nicolet%smsmal polyssar and beestial Castings libradas of reference 4 l specta. The FI1R analysis of abs paint ship was peribrand as above ascept that the paint aample was both 1 ' - --W thimud and solvent maracted to pewide two esmpte types for 'W h* e e i 1 EDS Aanlysis i A single white particle was removed as above and placed onto a coeductive, adissive surines. c l The senple was then placed into the Field Emission Scanning Electros Microscope (FE-SEM) and a spectrum was acquired using a light element EDS ddector.1hs special peaks were j hhi and the spectrum phes=E i i ) Test data is contained in the Ah I Test Raoules 2 The white residae was found to be etystalline and to contain os@ Zine (Za) and osygen (0) } according to light skenent EDS. XRF analysis detected iros (Fe) a well, but k is suspeceed of coming 6ami the rust residue within the sample. N XRD spectnen was found to be mainly j casaposed of zine fannsee hydrate (C.HAZa-AO). FTIk analysis of the white residue also j found the ihnchomalky associated with a fonnate. 2 4, .~

-. ~. -.. -.3.

~~-.-~- - - ---.--~

-( i FEB 82 '9912sE3 FR LAJ EH3 IND SUCS 794 357 BEJT TO 1423543EBEr7 P.84/15 i aoose apostwirw m an. y r,,e n am at i. &SS Muster fortee-7ess mese os i j The paint matsnal was detsnained to contain hiorganics including sitioon (Si) and titanian (TI) I along with less enounts of ansamium (Mg). Traces of aluminum (AI), calcian (Cs), potassium (K), and ehlories (Cl) were also found. Of psaanst significance was the abecace of berima (Ba), i selfur (S), strontiac (Sr), and chrendum (Cr) which wars semend to be present via the MSDS sheet ) provided. FTR aantysis confirmed the paint to be spany compound wish as amine fehlity l which could be indicative of the cesslyst composes discussed by the MSDS sheet. Based on the above analysis, the whits seeidae comenins aiac and oxygen and is a form of % istmate. Zins formate is created via the reaction of ziec carbonare with formic acid. Zinc 4 carboasse is used as a pigranat in rubbers among other materials. Fansic acid is used is j electropisting, coagulating of rubber innes, and as an aid in regenerating old rubber ammag otha f 8pP cations. li 4 4 l , The palat is an epoxy winsk has nitrogen h61 sroups that seald be indkatm of as polymaide assalyst. The inorganic memorial found in the paint suggests no benum sulhae ou serontiam chromase present in contradiction to the MSDS sheet which suggests thses should be j presset on the order of 10wt.% and Swt.% roepectively. These ccsapounds are typically used as i pigments *m pa*mts, with the strontiem chrcoats usually used la paints which are corrosion 4 resistaat. LEIS appreciates the opportunity to premde engineering services to Eco.Pak Speciahy FM { if you have any stuostions or ifwe can be of ftriber assistanas please do not besitate to can. sinom*, W ENGDEI3tDIGINDUFI1tIAL SERVICES y Anhil~ - b IAdmun %= *===== F.E. "H Tedimical Center Manager NICE CertiGested as Corrosion Specialist G ios Ptosidset 3

JAN 27 ' 99 15214 FR LRJ ENG ltC 54K.5 704 357 8637 TO 14235436007 P.05/15 ATTACHMENTS l

.~. e. t 9 a .I t I 1_ f l 19-Jan-1999 10:09: 25 set /acq ran=10; Ai=1 Pl=1 P2=2 ,( 5523 p FNeset= 100 secs yj Vert. 6130 counts Disp = 1 Comp-2 Elapsed-100 secs -i 1 $i St w@ feite sie El tv ' ei. 5: a di I g (-- 0.000 Range = 10.230 kev 10.110 --) Ui Integral 0 i i i i i i _ i i 309076 I; i 5 10 !l a< i

e I i.- i i - t 19-Jan-1999 09:55:46 5523-w Preset = 100 secs ' Ef Al=1 ~ Pl=1 P2=2 y Vert = 10722 counts Disp = 1 Comp = 2 Elapsed = 100 secs 7 $t 2 E. ITi khite Residue 3; gi 2n 5; Zn g, Fe FeZn e Fe FeZn 1 ll( 11 L ll O.000 Range = 10.230 kev 10.110 4 4 Integral O 318735 = 5 1,0 g; I k> A m t

JAN 27 '99 15:15 FR L N ENG IND SUCS 704 357 8637 TO 14235436007 P.0EV15 MO o 9 o o o o o o 8 b 8 E T M N mT I I I I f i I o e, 3 (, u in w s fw* 2y i 8 $} -a w e s / set's o ,e _., E-3 -$ O u,, ea l l i l N ~ E-o O o .= mee g r ., ~,.. M Bri /T90's He e sti /oce's I m- "E g-4 g2 = /=, c 33 H. g g_ , q' g T 988 /196*F

\\

~ g E.s 5 i)" o S I I I I I I I I I ,i o a o 9 o o 9 9 9 9 9 9 9 O o D O C O D O D o F m O b W N o b N d mN e O M b W W M g3 gw v4 e

%5 ' g EE 3 pg6 g;h jy$gge i. T l~ i 8 A0 30000o000000 S6 3 0987s54321 U0 4 1 - - - - - - - - - 0 /4 3 7 S5 O A 1 i T1 2 N: m H IL i CW 2 S i 1 N 4 0 Z y i 0 6 4 0 1 0 i 0 3 e 0 L H i 0 2 1 i C

PE 3

i T 2 h 0 S y i 5 1 i 00 J i i 0 0 2 o 0 5 0 E3 y i4 UD T: 2 J i IP S i i ER I Ji I E T j i I2 6 J E i H2 7 0 T W: y 3 A i

4 j

R D1 2 , iD I: Y E H i M I E T N T i i AMR i iE O 3 0 F 4 J i l 2 9 R. / fJ C D9 4 N 8 II 11 i / 31 1 20 00000000000 6 5: 7 6E 00000000000 0

T 0864208642 NA s2 0 9 B 7 S 4 3 21 4

FD p11 1 g

E Ysh@ @.L i %gg-i 4 l l1\\ 0 f 05 g I 0 00 f1 00 1 , 5 1I i 1 [ ) 0 1-0 , 0 m 2 c ( s re b muneva 0 j0 W 52 y 7 m n EL sgn s t 0 l e 0 a o 0 ts C 3 la ( ir t e s tu u d tW n I d m e o n r 0 e f 0 m e 5 a t l a 3 F m r 1 o -3 F 25 m 5 u i L c A l a R C 0 5 52 ~ 0 i 2 h-i k 0 2 0 8 6 A 2 00 8 6 4 2 4 1 1 0 0 U 0 01 0 0 0 0 ( 8f

m

RAL5523-1 FlatenedGrayMaterial y

0.6 - g 3 0.5 j ,.i V.' l 0.4h fI I ! I mi 0.3i \\l I h' o< k ) -h 0.2 - 6t 0.1 i 0.0 _ g,4gAddition Result-Epoxy Resin + Mice (inorgank: Example) 1.2 - N; y 1.0 I I s 0.8 -- { g, 2 y Q 0.6 j Ei O.4 2 I f f O.2 i i i i i 3: 4000 3500 3000 2500 2000 1500 1000 '500 Wavenumbers (cm-1)

g v" gg5 -( l i lj I iA* d i0 e, 05 f W i00 f 0 ) 1 l j j h 00 U 5 1 J ) 0 1 i0 0 m 2 c ( s re bmun Q k e va 0 i0 W 52 0 l b i0 a 0 d 3 a ta M ye rG den 0 e i0 n 5 e 3 l F n ,Q 1 is 3 e 2 R 5 y 5 x L o a A p c i R < E M 0

j5E i55 -

i.k:k 0 0 6 4 2

0. 0 8

6 2 0 8 6 4 0 0 0 01 0 0 0 1 0 0 eg !4$ hE

e i

RAL5523-1 Flottened Gray Material

{:[ l -t 0.6 "J \\ 0.5 -- tl Y.4 0.4 2 wl 8' ,e e ( x; h D3 \\l E i mL 0.2 2 bI E! w 0.1 1 0.0 ~ 1.0. Amidoemine Curing Agent (Epoxy Curir g Agent) from industdal Costings Library i +E 0.8 - q ~ f? e .g 0.6 - g! t ~ k E! lu e, a, Q 0.4 - [ J f!: t t 1 0.2 - j O mi h? $1 4000 3500 3000 2500 2000 1500 1000 500

l Wavenumbers (cm-1) i

c7 d I wn s 4O I. tyi{L$* -{ ~ 0 0 0 1 r *. 0 .0 9 y; 0 0 8 0 e 0 7 0 a 0 6 0 0 0 0 a

0. V 1

e a 5 k le m a n h a. C / t V 0 e I a 0 4 0 aj 6 4 g 8 [',

e0 m0

'g 0 T0 i a 0 m e4 3 r k - Q o L el g F n a y e 0 f r 6 fo P 0 -e 0 e tk m 0 a a d mT ~ 2 i m n s u n C V l i e A me0 0 1 u 0 4 od 0 6 0 ri 6 4 f s U 0 e 1 eRV 1 e n 4 uk k oi d c t ia lu l sB o e P s 1 S e 0 R 0 3 D R C 0 r 3 4 1 7 4 0 k5 t o sd c5 y 0 1 7 3 8 4 aL at l o 7 5 4 2 1 l A n e BRAD

C i. i-1. 19-Jan-1999 10:24:16 o _1 A1=1 P1=1 P2=2 5523 p Preset-100 secs Vert-SOOO counts Disp = 1 Conv= 2 Elapsed = 100 sees ti l Paint. Chip a h i h ct ri K I { g-Ca St Ca ) { Ca Mg Cl K l\\ idLCa) lb kn g Ti 1 MgR I Cl 0.000 Range = 10.230 kev 10.110 -> o Integral O 278398 g = i i i__ g i $4 g-b5 } h i m.

e. I^ ~ l Director ' Office of Nuclear Material Safety & Safeguards February 10,1999 {' Page1ofI i i i i I i 4 GE/UNCW Analytical Results Dated 1/19/99 i f f t F I, i

(j)MEL R IHJECT 91/19/99 19:59:32 ) PM 1 y cn :

u

" 2.02 CO :, H, ~ N% e c 4.1e 9 py' e ,- 4,, g e r 8.44 e e HIGHS 01/19/99 10 59:32 CH= "A" PS= 1. 4 ILE 1. NETHOD 5. RUH 65 INDEX 1 CALIB e HALYST: UNCW 9 e ONC UN RT ARER SC RF g

L 28.8

2. U2 682/838.ei 202355.903 e

4" 30.6 4.1 14611844 01 181278.462 A< 52.6 7.46 7184229 02 136582.3 i04 52.1 8.44 19206624 03 368649.213 e e 21 4. 1 46829747 g

L

?A27.95. CAi ?. A7 ( 'H03 181270.462

4. OS PO4 136592.3 7.47 304 368649,213 S.42 CHAHHEL A IHJE0?

G1. '19. '99 11: 11: 29 j FM i p 1.48 C AceKc Acid Y'N' $tilL ff' i f ep exatSc paid My C. $NLOG 40tAld 4% WC-ANIGHS 01/19/99 11:11:25 CH= "A" PS= 1. FILE 1. NETHOD 5. RUN 66 INDEX i AHALYST: UNCW HnME Un RT RRER BC RF 1 G. 1,48 9198691 91 CL

1. 25 1.99 252847 31 202355.902 TOTRLS 1.25 9441529 1

Q Ip og P 3"- ww

i Director Office of Nuclear Material Safety & Safeguards February 10,1999 i ( Page1of1 l i i i i e t 4 1 MSDS for Resin from Schenectady International, Inc. Dated 1/18/99 i l l t 1 e I l l l i i. 1 i i I d

Director

Office of Nuclear Material Safety & Safeguards

. February 10,1999 { Page1of1 i i l l 1 Attachinent 6 i Phenolic Foam Literature - 1969 L ~ Plastic Foams: The Physics and Chemistry of Product Performance and Process Technoloav, ) Wiley-interscience, a division of John Wiley and Sons,1969. i i l I

grm co ee rat ut:40 rr8 tha W. P. 01 TELEFAX LEAD SHEET SCHENECTADY INTERNATIONAL, INC. I 2750 BAu. TOWN ROAD

('

SCHENECTADY, NY, U. S. A.12309 l PHONE 518-370-4200 FAX 51b382-8129 To: Heather Uttle FROM; Todd Makenzie Ecopac Specialty Packaging DATE: January 29,1999 Elizabethton, Tennessee FAX: 423-543 6007 SuajECT: Phenolic Foam Literature COPES: DFM

Dear Heather,

Please find following several pages describing the chemistry of the phenolic foams. Let us know if you require any additional information. Best regards. Todd Makenzie

Chemist, Polymer Division First of21 page(s) l l

E t 1

.+ Ti L ..r. k ~. ~ 3l I.y.tyn. lf.p W ~ POlXMER ENGINEEnlNG AND TECEINOT.OCY f 3,f Of product perfortn nce andprocess technology

T Executice Erillon D.V.itoutin f,

8 Enlitors: R. B. Akin, II. F. Metrk,J.J. Scavussa,

]

t' .f S. S.Stionia,l,J. Zukor i o E n CHEMISTRY AND PHYSICS OF F0AM ~ FORMATION ' h' nxTnEnc n ERs in rarERMAKINC ji ,l,

== Edheeky O. A.Battista rn. AMENT WINDINC,ADeve4epeeed.kfanafselete Appliepeines. . k) i m llj,- .,A De,< o.v.m. endC.s.ce=e.fr. O?l tEiMrOResurnT Or Et.AsTOwEns CALVIN 3. BENNING Esitedby cerned Kr TERIAI.S (3 Mennes) ENYtMONMENTAf. EITECTS ON pot.DIERIC RfA d 'l I b Ne'rTeclinofoCFResearch l Edistel by D.V.H*, eta evid R.T.Schwarta FUNDAktENTAE. AffrCTS (W Ft#EM REINFOstCE*D P. f* gOrl20!*teResearcleCenter.!nicrndianalpmMPany e r tA5 TIC i COMto$iTES EdMed by R.T. 5ebwarts and 18. 5.Schwasia r j,, Af AN.nf ADE FIDFRS,5etenev emiTecinis8estr ts valumest ~fi-Editedby 31.F. Mart.S.kl. Atlas and E.Ceewie i l hls (3,*Innical m Tite SCIENCE ANf7 TEC#fMOI.0cY OF f0f.Y1 felt Fi. M F. die =d by Ordne I.5=cethes (*,;.- ,1 Pl.A5 TICS FOR El.ECTtHCA1. IN5UIATION - f EdisedbyPoet F.Wrules ,f 1 l EPOXY RE5tM TECitNOf.DCT + f f EditedbyPsid F.Wrnies MMSCfHICE a affvfrfon of Pol.YUNEn1ANE TECilNOLOCY tea *n , s,*,7. r % f. Edised byPowlF.N'"bss b; elefinIPNoravidsa gg Pt.ASTIC FOAntS.YnimmesIandff p l c.w r.ne d.: 'I ggg9 g v1 AMitions1Vetomes he Preperselen

t g

l f L I Q 'I . l,. ( e + m - _ ~.. .swi ,e

F f y. ro Principles of Foam Formatiam Phenolic Foam o) r.o. CONTENTS 413 - ui ; .m I. Intrailection............................................ <.......... 424 e>

11. Fornmilation ovel F repoemeten........................................

424 3 A. Fosnuble Besins................................................ m H. Blowing Agents................................................. M C. Catalysts...................................................... 427 - D. See fectants..................................................... m 111. Compeandlas mail Fenmang......................................... 425 IV. Metatiemship between Fernwletion Vertabler arJ Foem Properties..... 429 A. Betredeetion.................................................... 430 B. Fesia Morphotogr.................................... :.......... I. Deesity. 2. CeRSire. 3. SkleEfects. 433. V. Mechanical Freperties of Phemel-Fermeldekrde Feasm................ 433 A. Increductio n....................................................435 M. Properties........................... ,Ger. 3. Meisture end L Mechanical Freperties. 2. Thermiel a. MesseurevaporAbeerpoian. 4. DehavierTownedChemicals. 443 VI. Meclamisms of Char Fcemessen soil Thermal Deceanposiuse........... 445 r 161tourschy............................................ :... -.......... i ri R

1. INTRODUCTION Methods for foaming phenol-formaldehyde resins have been g'

known in the laboratory for many years. However, before 1941 the foam was little more than a Inhorntory curiosity and had little com-mercial value. During World War It phenolic foams of unicetimisr-structure were prepared by Expanded Rubber Company under the l trademark Thernwr.ote. The foams were 6 8 pef and were niainly used for buoyancy applications (l).These materials were expensive and therefore were later replaced with polyuretiene and polystyrene foams at lower cost. Recently, interest has been increasing in the phenol-forsnaldehyde foams as heat and sound lasulation for curtain walls, as thermal instdaten in refrigeration (E), and as packaging-i materials for delicate instruments (E). Phenolle foam is a rigid, thermoset. Intesconnected- (open-) ce product that is low in cost and dimensionally stable and has excellent ~ y I flame resistance. o, w 4,3 B 4 .m.. mm.. m.

~ FOttattRATION AND PACTARATION C5 4 rittkotrC FO,uf has been found to produce resoles which are slower to react,therebr [f . FOlB1ULATION AND PflEPAllATION allowing greater latitudc In foaming (4). The preparatioi of expimded composites from lhtuid phenol. Various methods have been used to mmlify the fundmnental ii r irm Idehyde condensate resins is known. In Europe and the United phenolic resin composithm to meet specilie demamis and penduct &; lates most PF foams are made innn the base-catalyzed emulensation requirements. For example, poly (vinyl butyral), a thennoplastic d These resins are called film-fonning resin, has been incorporated into the resole to pennit D r traducts of phenol and funnaldehy e. the complete expansion of the foam before crosslinking (l.anteninal p eschs. In the Soviet Union, emphasis appears to have been con-entrated on the acid-entalyzed condensation products of pheno - (5). Other Alm fonners, that is, polyvinyl neetate and polyvinyl nect l have also been used(6). Polyisocyanates have been suggested as a orm:1dehyde or the nocolds,as they are called (Section V Chapter means of offecting the Aeribility of PF fatms(7). Funms made from F t,wirme II).The preparation of PF foams from lignid resole-type resins can he resole resins containing silosane.nxyaikylene capolyiners (1-10 wt %) l are less brittle and have improved cell stru.ture. The siloxane l i summarized as follows.To the lirjuld phenol-fonnaldehyde resin s added a foaming ngent. The foaming agent is well disperse copolymers act as a foon sinhilizer, crosslinkingcomposmd,and resin d in the resia before the addition of the Imrdener, which is an acid. When a modifier (8). Soviet workers have concentrated on the use of rubber ad d carefs11y calculded mnonnt of the haniener is added to the mix an containing a maximum amount of nitrile groups. Foanis containing rapidly stirred, the exodiermic reaction of the resin and acid, together novolak. type PF resins ami nitrile rubber have been studied ex-with the action of the foaming agent, causes foaming of the resin. tensively. He ratio of nevnink to nitrile nihher influences the This is followed by rapid setting of the fonmed maiertal.The heat genernted during the exothermic reaction is an essential part of the strengtle properties, the ' elastic properties, nnd the thermal stability of the expanded innterial. (he relationship between polymer process (l). Depending on the strweture of the resin, the foaming agent, and stnicture aml foam properties will be discussed in Section VI, Chapter the acid, the reaction rate and esponsion enn be regulated for n dura-3, Volume 11.) tion 1: sting finm a few seconds at rooni teinperature to severalImurs at clevated temperature. In conventional systems, the entmusion is complete within several miimtes and the foam can be handled for fur-These materials are used to ehtain a smoods, even foaming action y, gy,,;,g gg,,g, , lt 4 th;r treatment 1-3 hr after the reaction has subsided. Alany variations g that starts at a relatively low tempernlure where the low-boiling ) of thae techniques are recorded in the literMint(1,10,13,21,22. 2; litpdds are Arzt volatilfred and progressively increases as the P' exothennic reaction of crosslinkingbecomes more dominnut. Without A. Fmmable Ilesins these mkled agents the expansion would he quite erratic since it wof Phenolic foams are made from commercial casting-type resins (vis-depend entirely on the volatilization of water out of the snixture. casity approximately 251mises at 23"C) containing 1-2 moles of for- - Essentially three groups of sub stances are used as blowing agents. l maldehyde per mole of phenol. (The ernet ratio of F/P detennines One group comprises the alkali-metal or alkaline-earth metal relin cud foam prope 1ies. As a residt, the ratio of reactants of a cathonntes and metal powders which are disteihuted in an extreme l d d secret amlis usually fmely thvided form in the PF resin. Deze athlitives react with the , givers commerchd mn'erial is a close y guar e mid of the hardener, enusing evolution of CO, or II, gases.The gas is considered proprietary.) After the desired degree of condensation (usuxity a DP of 15-30 units), the basic catalyst is usually neutralized fmned as smdl bubbles (hubbb h depends on dw d sub-division of the bhowing agent and the degree of dispersion in the with lactic or oxalic acid aml conceritrated under vacimm to venmveusmally used as cter. Arpienus solutions of formaldchyde are ,,,,y,(9, ggy, l d that %e sed pp dagents comprises organic compoumis having starting materials, ntul it is necessary to remove this water an whicle was produced by the condensation reactirm. As much as 2 Iow hoiling pointe pentane(lo), n.butyi ether (10), chlorofluoro-5% .t I alkanes (12), diethyl ether (II), and otlierr(13). A unigine variation water may remain in the resin to nssist in funmmg. A combined sodium hydrosnie-harima hydrox.de catalyst system g. i l

? s. FORMilutT10N AND rHEf%ILATION st27 is ynsExouc yo.ut Imt because of their stnmg attack upon metals and other materials of 3 c. f this second group of blowing aids is described in Czech. Fat. construction, other acids which leave less noximis reshlwes in the fE 15,1961. Espandable polystyrene heads foams are preferred. Arumatic sulfonic acide (benrenesiditmic,

i !

" 05,342, issued on October are added to the resole, and the heut of cmsslinking and hanlening loluenemifonic, phenolsnifonic) are most popular (17). El l auses the polystysene pellet to sonen and expand as a resnit of the The problem of corrusion at times am be emphasized out afpro. I 3 d liardening portion. Paul (13) states that phenolic femms being prepared widi acid tra added to the resole, and the lient of crosslinking an .ca:ses the polystyrene pellet to soften and expand as a resi t o t e cablysts are espected to luwe a high curmslon potentisI; however, d fh Et volatilization of die pentane. Dese substances evaporate beennse dilution-of the acid in the resin system and subsequent isolation of -Ei of the he:t liberated during the condensation of the resin and in this Ilic acid in the foam prevent corrosion.He mest serious corrosion

ruan=rcause foaming of the phennlic resin.

"CC"rs when foam is generated in contact with a ferrous mebl, using 3lf %e third group comprises organichlowing agents that decompose hydrochloric acid as the catalyst. Under theso conditions,a protective conting should he apidied to the mehl surfaces. Foams generated l (t2 hberate the espanding gas) under the inSuesice of the heat of reaction. Such materials are diarcaminobenzene(14), benzene against nonferrous surfaces will not canse corrnsion even mRer several diatonirm snifate(15), citro nreas, urethanes (16),anoisobutytonitrile years of service. Likewise, foams prepared in slah or molded form (ACN), p.p'-oxybis(benzene sulfonyl hydrazide), and dinitroso. and subsequendy installed on vadons surfaces h ve exhibited no organic gas-liberating agents cormsive efects(13). pentamethylenetetramine(4). *Ilie IIproblems of residual acid in the foam exist in specille cases,one provkla somewhat better contml of foaming, especially where highe 4nsity foams are desired. solution is to trent the open-cell phenolic fonne in an atmosphere of l Of lesser conimercial importance are standard frothing or air. ammonia. he resulting composite will be neutralized. j ispectirg tecimiques which have been used to expand phenol. Isocyanate prepolymers of TDT, pentaevythrital monoolente, i fornialdehyde reshis before cawlyst a klition (this process is similar and dipropionate have been suggested for pimincing low-density to that described in Chanter 7 for the Imlyvinyl alcohol-formaldehyde structums with improved compressive strength aml water re-sistance. When these prepolymers are added to resoles in ennjunction Tomu product and involves the same phenmnenon).%ese tecimhpies 4:nd b increase ceH size and produce a more resilient sponge at with acid entalysts, the exothermic reaction vaporizes the water residual in the rescle, foaming ami crosslinking the mass (18). 'l lawer strengths. Ilesolcs catalyzed with barium hydraaide may be stabilized by He acid catalysts can he eliminated if the resole with isocyanate If cooking to alent 5% or less free phenol, and then blowing with CO. prepolymer or diisocyanate monomers is heated to 200*C to effect to convert the hydroxide to the carbonale. De synsp may then be crosslinking.De expansion in these cases takes place with organic {! - [ concentrated to 90% solids, before which the barium carbonate blo:ving egents, that is. nzodicarbonnenkle. { Mlutures of organic phosphoric acids aml mineral acids have been concentration may he reduced by Rifering. Addition of toluene. used with polyhydrie alcohols to control the rate of condensation and sulfonicacid then yields more durable 3 pef foam. Novolaks may be femmed without water or st'eam eveh, tion by cure (4), and peroxides have also been evnployed to crosslink and cure the resole. Calcium pernskies, metallic pemahles, and urea per-blending a hard resin with diisobutylene and a silane surfactant, esides are also operutive(17). In all cases, the rate of crosslinking cnd adding dinitroso blowing agents and a enring agent such as will be direcdy proporthmid to the staldlity of the peromide. %Is i hesarnethylenetetramine. Shmilady, a novulak resin containing a blowing agent, a fonnaldchyde tkmator, aml henzene subnic acid means flutt the more stable peroxides rettuire Idgher temperatures t hydratide may be heated under pressure to produce a foam (17). tocure the foam. J C. Cattlysts (llardeners) D. Susifactants [ Achl catalysts initiate the reshi condensation or polymerization Organte surfactants have two (smetions. First, they maintain foam reaction and are preferred for ambient temperature foaming. Mineral stability during the curing reaction. His is donc by reducing the "f acids (hydrochloric, sulfuric, phosphoric) have been wklely used, E: [

+ e Ft)lt3ft#AT10N YARIA#fE3 Ai D l'OAAf FTIOFENTFES V cf is rrtEint.FC FOAAf irfice tension of the reacting mass awl hierensing the strength of hu M SchWMHmhdihMmew k< o litivid lameline during expansion and curing. Second, udditmn of - and suggested applications of these two standned grades of fenm. Por , rs ;

- - - 8',*,

}l mf ctants to phenolic foam secipes results lu more unifonn distrilett-l hl 7,, ul ioncf tha blowingagentand gar - hbles.Forexample,po yet y enc 5 %,,g 3, a g. thers of monolauric-sorbital ester send ethyl-phenol-ethylene oxide heleWinn efln Ril. g; ondensates have been desedhed as being effeelive in improving cell ~ 1.ightweiglit 15-2e nce. Suit.inde far Very f.ee eeH sk,- laveturo and foam sinbility(19). In geneml, the smfactants with the Innin i ptf being in inukls ont ley slintely dan-1,igs, sneinstdst R iigh st performance are the mmhmics, and llmse stable in strong "udnnes inte nudds er tien <>UW. and util sierige y erfis er ti e, '"Isinet insin metering gated lie diere. s o ,.idicmedia. cuvities er fwr bming ist Resilieset mesel re-plants. -r-l rwo czamples of typical formulations might be as follows: (1) himlerlat phy C!) &lageviet, phr Fonnialile resin 100 Fesseuulele tenau 300 ,,,,"E,g' Smilumtidi:mimsiese 0.7 Tween 4tP t Neestamou susfaciant e.1 Structural 4-5 min. Sultalde far ben-Centse ceH steve-Insulatinssin hulbt-Tettin X.3otrer j Is.pn.pyl =<her s FlienolanKamle actil "LG g,,,,,,4g g,,,g,,, g,,,a g,,,,g,, ,,,,., g,g g Acid tstalyst 8-83 Filler mesnillra ratorikt 1.0 g g ,,4 4 i ""*b'"*' ' """I' ** cavides er for i== ming la pipes, etc. Ah - n ei :a c hu arid c ts hiweisht u as eten. g,,g,,g,g,,, cores for s d- . ach so w.e s. III. COntFOtlNDINC AND FOAhllNC P*'""'- For small-scale production of the higher-density stavetural fonms Q""',"'", 'g dd" l (4 pet), the additives can he conveniently mixed with resin by hand. Vsssels are usually made of corrusion-resistant materials, such ne enameled Irem, polyethylene, rubber, cadhenware, or stainless steel. IV. ret.ATIONSillP HEBYEEN FORMUI.ATION The nmst effective type of paddle or mixer is a simtula. After the VARIADE.ES AND FOAht PROPERTIES ~ g l ~ hardexer (acid entalyst) and blowing agent are mided, the etmipoimd A. Introductism l is timruughly stirred and mided to the mold. Imw density phenolic foam (~1 pcf), beennse of the very shoit Omnging the ratio of ingredients changes the foaming character-mixing time allowed before the kmming renetion occurs, is not istics and the foam properties. For example, smnM iguantities of non-suitabla for small-senle pemloction by hand mixing. Iland mixing ionic surfactants k Iphr) nid in the prodwetion nf small uniform can be used in the laboratory (up to I kg). Rhowever, larger spantities cells. As the etmcentration of surfactant increases, the fonm becomes 'I.the excen and a nmre msWentinmluct is olitain resguire notomatic mixing espeipment. A comprehensive descriptitm P owmg agent affects Llic tiensity of phenol-formaldchyde cf mechanical mixing ettnipment is contained in the literature (l). c ne same maimer as that observed in other systems, that is, Mapid foaming is essential to imiformity of texture, particularly as camcentration increases,Ilic density decreases to a niinimum.*Ilois am an when making a low-density foam. %c reaction is emothennie, and the I is the amnst of maxinunn elliciency at which low-density foam con-heat generated cxmverts the water present into stenmi and also speeds '*I"I"# ""b'"u ceH structum is obtained. Sistnificant increases past the resin reaction (3). a s amint usmt in on increase in density enusedby collapse, In a demonstratitm of the process, a 411 ft' cavity,8 (It tall, was filled du. %e simeture and concentraten of neid in the formniation de-with pheinolic foam in 55 sec. The time fr'um first appenrnnee of the tennine (with the resins) the tiegree and line rate of crosslinking; tint vi form to the end was 15 sec. With a ligider femm the time was cut in Is,if the reaction is tem exothermic before there is snificient buildup 8 t t =

P s. FORAittlATION YAft!AB!IS AND FOMf PROrERTIES 43t 1 FIED'Ot.tC FtMM 28 viscosity or gel, most of the blowing ngent can be lost because of y niling, or the foam sets before vaporizatiota of water and hIowing 18 - 4 cut is completed. Tltts results,In a fonm with large holes and = stres. Ifless than the rectmtmended amount is used, the resin is 8 - ll 2 5 . t sufficiently cured and the foam shrinks and partially co apses. 1 ~, s oi g 5 '? ' ~ 4 ~ O . FoamMorphology I In addition to the variables encountered in various formulations, i3 g 12 performance and cost of the foam are also determined by its {, ensitye dcellstructure. g g . Densky 'M I6 8 he foam density can be effectively controHed in several ways. H 7,,,Q 2 ly tite use of different resins, products ranging ist dernsity frosos less 1 as i ' han 1 to 20 per or more can be obtained. Foaming time will vary frunn 85 L a n 25 c. 5-10 i t matter cf seconds in the case of the very low density foams to E4 ' ni.4 for the higherdensity products. o.3 Fxmable phenolic resins, each capable of producing a specific ' foam density. are availabic commercially. For esample: 38K-2 M Mel4 *t 5 o 20 40 to se too ao es to 2e c 2 Deustty ef fman aletoined.pcf M N M # M 9 to e e se m messa Btt1,1150* l I-SRtA-27sl resin,wt 3 M b8RI.-2739 msin,wt 3 13 HMI,2780* Denshy-cosivosMoon curves for litending Benellte fossnable pliesiette URIA-276to 65 ri, Fisere i 'Ueten Cach8de de," resius. Nt reinae heat famn the foarning mass or g; A complete range of foam densities can be obtained from various increase back pressure on the foam will resultin increased fomen den-ascm y, con ons ' mixtures of these resins [ Fig.1(22,23)]. A second approach is the use of varying concentrations of blowing NT. Mms, for a Nn Gmn fonnulation, minimum density and l masunum mufonnity would be obta.ined by foaming a large mass of agents. For exampic, a complete range of cellular foam prodeacts hasmaterial in an insulated open-top container. Masimum denalty and heen marketed by Dynamit-Nobel. Table I shows the formulations I:r th2 various foamed products. For wider varianons in der sity other Iarter kuT En&nt wmiM lee ehtained by foaming a smaH ruass naving narnsw cron-secuenal resol 2 resins are used.This is similar to the Union Carbide approach I8atmcIs themet a wh ch foam would have to travel. %ese same m a un a ce meta me t ll.. - TA!!IE lillef.II) J'f N f g,.i phenomena are observed in the fonsued-in-place applications ofpoly- [ (10) urethane a.nd pyranyl fomens. i Density,slena'

2. CcNSise 0.04 0.07 0.1 ingredical The size of the pores in expanded phenolic resins is determined 300 1eo los by several factors. It is dependent on the nature and qtiality of die

,l Resin.g blowing agent, the reaction tesnperature, and the hardening behavior. n-remune,eni' 10 7 4 O Acid entalot.em' W-10 D-10 0-l# t

Tilt %Qiac FDAM retorsanEs tas 2 ttfENOLEC FOAM V. IdECIIANICAL PROFEltTIES OF FIIENOI, h r rato r.ml degree of cure) of the resin.%e use of sniall quantities FOtthtALDEttYDE FOAhl5 j by nontsnic surfactants promotes small, imiform cell structurehing 4 s mnotixg smiform distrijmtinat of the blowing egent und al.c resu thenolic foams have sevemt basic deterrents, which have limited A_ Foams with small, uniform cells are mnde with blowing aids that their more widesprend use: (a) nt low demities (< 4 pel) they are as bubbles. ra s:lable in the resole, that is, Isopropyl ether mud Fium 12. In brittle and friable: (h) they alesods moisture and therefore cannot be [ .ractice, it is freatucutly desinible to have available both line cellused as low-tempemture insulators without vapor barriers; and (c) the N fl nd course cell foamed pnedocts from phemdie resins Forinsulathm, open-cell structure leads to a K value of 0.28 DenNhr)(ft')('Flin-) at ins pires are re<guired; and for foams needing an adhesive or barrier low density, whereas the K vahte from czynnded wrethane (aged) is e* ble to produce onling, the coarse cells are desired, beenuse it is possi 0.15 nnd 0.16 and from polystyrene it is n.13 %e advantages that ' tigher bonding strength beenuse of improved penetmtion of the ad-phenolle foams have over other low-density prudwets are (a) a very low cost potential since the raw materials are inexpensive,(6) l sesive(19). Wleen properly fornmlated ami processed, al systems. l ti ly execlient Name-retardant wri>pesties (especially with horic acid reganlless ofidowing agent,should yield fontas of smiform,re a veEne cell structure.The method derivatives), and (c) good Jgh-temperettere stability in comparison are schematically represented in Table II. with PU and PS foams. In our discussion of the mechanical properties of phenol-formal-TABIZ 11. CeM Sles and Fannielaakm dehyde foams, we will discuss three systems: (a) the Dynamit-Nobel Akt. Ges. process (10) and product, (h) the Union Carbide phenolic fonms(3,5,11,13), aml (c) the Icechim (linngary) foam (2). %ese sm.neen size L=se cell eine opumm.- three systeens were selected hecause they represent three approaches Smfacient to making phenolic Innen through a cmumon process step. All the eneresse Decrease ^ variations appear to be in the fannulation, not in the process of ex-Camilyd ,3 '" pansion (modilled foams, such as the Soviet phenolic and rubber-mmlilled phenolic loam will be discussed in Chapter 3, volume it, Docteme is isprii.t where the relationship between polymer structure and foam prop-g Aeld weser weier mse erties are emphasized). 8 The three systems differ in fornmistion. For esnmple, density is adjusted in the Union Ca bide system by proper resin selection from

3. sun Efects a Immily of foaming resins.%e reactivities of the resins differ, so that

%e thickness and porosity of the foam surface enn content hwierthe amount of hent Ilhernied in the renetion, and consertuently the l degree of foam espansion, can be selected according to need. Since properties and insulation vaine.%erefore,it is important to regu atethe skin by ammm intenially generated heat prmlwees the foaming action, these resins h f the Istmation of a " skin ** of higherslensity resin surrounding a oamcan be foamed in place in hollow cavitic-or produced in farge core is due so the kiss of heat which occurs at the foam surface. "mokls" for subsequent conversion to slabstock. A thin skin of high-De-density resin is always formed on the exterior of the foam, where heat k pendir.g on the specilie applientkm, the presence of this s in may ormay nit be desin losses prevent vaporization of the blowing aid and water. l l The D-N pmcess uses a tailor.made resin (T-610-S) and adjusts l h out the foaming operation in heated containers. For examp e, w en { 1 the Isardening agent (mized acids) and the concentration of the. f.am is generated in a cold metal container, a relatively thick skin is l Isnuzd. Prehenting the met.1 to 100-180*F markedly reduces skinthickxess. Altern blowingagent(seeTable Ill). ,j The Icechim fonm la prepared from a resole-type phenol-formal-conductivity of the contanterwall. dehyde resin having a density of L.15-1.25 g/cm, a water content {i her.: 1 coxtainer will have a relatively thin skin because of the lower(L 2 o,

i.' illENOUC FOA3t ftt0CDtTIM M su rIEENOLIC FOAh! h, I IkII"es for Prenntles L.orge piecks (1m'l B. Properties Tant.E 111. RetSia'acad".111 The phenolics are rigid thermosets possessing excellent chemiad d of D.N Fleenolk FenniUlet and temperature resistance. %cse properties nre also exhihned by 4 the expanded phenolics. llecause phenolic foams can be produced ne'isity. over n wide density range, the material shows a corresponding wide g 1.5 3.75 5.0 a.ts gg,,, 4,e ; e.n4 e.0s 0.0s 0.1 range of properties. Phenolic foams enldhit one unirgne pmperty. AH {' commercial foams have a high percentage of open cells (usually s ru ;

$a 40-60%). The percentage of open cells decreases as the density of the j

8 de incmases. WanW kams fam ebhH Mmdur nessaiT-elo S).hs i to-a.tuers 3. .s.4 .7 73 7.6 OA9.5 r [$$ J. MechanicalProperties between 10 and 25% and a pit of 6.5-7.%c foaming agents are metal Paul (13) has described the properties of the Union Carbide powders (AI, Fe, hig) with particle size less than 100 mesh. ne ex-pansio2 of Icech the metal and the acid, but also of the particle site of the metal. Cat - hydrochloric acid-catalyzed pheimlic foams (21) and has emphasized .i g ;,,g ,,,,g gggg;, gg,g g s<lyst mixtures containing orikaphospimric acid and beinenesulfm Ic of the foaming snass results in the ehmgation ofimlividuni ceHs. Con-seveuently, phenolic foam Ims n " grain" similar to that of wood, and acid produce the lowest. density uniform foams. Ilorun(2) has com-pared the Icechim foam with other connnercial foams in Emnpe and p, simngth wiH vary depetiding on whether a property is measured parallel or perpendicidar to the foaming direction.nis is shown in has in:nd them to have similar properties. Two other commen:ial phenolle foams that can be class, died In Fig.1, which gmphicaHy illustrates the variation of strength proper-I ties with foam density. these three areas are: The mechanical beluwlor of the D-N foain described in the manu-g,,,,,,,.s technical bulletins (11) and by Dr. Weissenfels(10) is

1. The system of Itezolin Inc., whlef, utilizes one resin and vari-r.ble foaming agent concentrations to produce densities from summarized Isi Table IV. A comparison between Fig. t and Table IV ri.

shows the mechanical properties of the D-N foams to closely approxi-EE ! 3 to 11ptf.

2. Foams used for Alling cores of large castings, offered by mate those of the Unimi Carbide foams and others. Comparisons am klaridette Corporation in 10-15 pef densities. L'ostenting for
ygg, pig g In contrast to many other foam plastics, the strength charneteris-8-10 hr at 140-2tNrF is reconunended for these foams.

tics of phenol foam are not influenced signiflcantly by teenperature %esa two systems utilize separately packaged resivi, foaming agent' and humidity (11,13).%e relationship hetween compressive strength and temperature aml relative humidity is described in Figs. 5 and 6-cad curing agent, wherens the Union Caibido and D.N systems m-Vibratism strength is considered good at manimum compression quite only the addition of scid catalyst (17).Lately, small-cell, fire-resistant foams have been commer amplitudes of 3.6 kg/cm' at a density of 0.08-0.1 g/cm* %ey are formed by the intraluction ofa polyhydroxyl derivative andby Plastugel(24). % ( enne memr er a polyamine derivative o; a polychlorinated diphenyl of poly. The K factor varies with foam density.The Dynamit-Nobel pheno-phenylbenzene into the phenol-aldehyde condensation stage of the lic roams are reported to possess excellent thermalinsulation prop. l preparation of the resole. The foams are stable to 180*C(24).%eycan be rendered fu resin itself having low thennal conductivity, aml (c) the low density crlies, because of (a) the even, line cellular sinicture,(h) the phenol j 'o conting them with silicates, such as alkall or fluesilientes, and dryingof the composite. D.N foam has been evaluated at several densities i c* (25).

~.1 l A. TAMIX. IV..stechanical Pragmentes of D-N ri enalleRes6n Fee.m c 'S TilENOLEC FDAni ii. Densay la N i i.

a O.tki 5.05 a.05 0.3 i.e.

i 7o, _ s + -i.* sdeet' 3.5 174 4.ps s24 -%r 32. - sec. as n/=>vn, _ *** a'*4el alafia. Pcf m Ilcui ingstrengets l n L de" ' 18 41 5.5 45 20

MO c m.sm 1

8 43 80 Tit 2 33.4 T twI [ f",.se te. cm p m.sve m enci. ru [ JJ 4.0 g3 7,g c'- I ?1 kgferit' f Sil G5 88 110.D 29D g E,e g { 1.0. Psi 4 Ng si. ear e s h 3 I,s

a

_, _ + e E o GR 23 4.3 .L.6 s+g ha/can 88.4 36 SIL3 35.4 - iso yst 20 in cee ch [ g.96 ' s.17 e.15 e.13 ~ ,e,. i. i. beg eon /cne* 2 4 6 5 19 12 14 IlsinJim.' O.156 0.44 nage sage ..ii,ii_ e; 0 2 4 6 5 le 12 14 Fee.n core densier. pcf Mnickedinnenetstresigik O.DE 0.09 0.08 0.0g Feasn sore denster.,d hgende.or' lin in,fia.' O.156 9.334 0.108 Olet y g kMleet' 129 835 115 See ,,,,,,y,,,g, 14e 300 1706.4 1100 30eo SR50 120 W r* a 5-Psi . sn e. -asimJ e. Tensile strevigth kII/cm' L2 13 4.4 5.4 I1s. ~ 17 47 as 77 k 200. 'P" '.I psi t,, C,

,j

e ,a s, -r. r.ir_ a n s N e 49 i ,[ g,, _ tw is q 3 on ~ . p# M *7'l 20 i.i.i.i.i.,o a >= .i. ... nu . 2 4 .. i. u u t e. w e 4 ,. e h5 r .,a rsci.r.s u.ch ac.I,.p..ecsofIIO eandrrestehennlic Eampief=.13.ss) g m = C) of Ii j j j j and over a range of temperatures. The K factors (kent /m hr ' D-N foam at various menn temperatures are recorded in Fig.7.

-o 7

g Far practical purposes, the oldect is to obtain a phenolle foam of ,,,,,, q,,u, w low density and higli insoletion value.The K vahies of Union Carbide. 1 i i e a r i e est eos e.os aos ett D.N, and Icechim femms are equivalent at the same density asd cell structure. In general,' the K value is 0.28 Bttel(hr)(ft')(*F/lii.), com. f i pared to 0.16 for tirethasse seid 0.23 for polystyrene. A swmnation of Figurw 3 Tensile sere.igth er ewn eenumeretal tilieneolie feimmia. s--Restnip8e .O i e-singleresta +a ieeJar 4. 8 the thermal charneteristics of a typical phenolle fanni is shown in 427 5 i Tchte V. f 1 1

A 6. ~ Pl!ENOf.!C FOAH FROrDLTIES <!S is. - g aso a i 3 oms .rda. J-o.ser r tu m iso / - -j to 3 g = ~ 4'- f. o. sion . s k ooM - l R 4 - 3

y

-d... 7 -g [y y 3, = m f= ,. e- ~..m e - t t i },, esa s ..? seat a = = 1 / 1 i ~1 1 1 I i E0 e e em om oos em e.g ~ d.000 ereine/cetic esmometer esta compensive streesti (psi) eri m.a teams (ch isc). -br rie.ve 4 13.22..-Mets. ne.st. O.000 - i t - i I - I

i.

,10 < -

esor,

-m .m += 5 m ' - eA.f,,,,s ' T

- -c l"'"'_

ri.nirev ue . sos..cr.c .rna i,e ner.m De -1 g g,, 7 sea v -3, _) - TAntIV. Theri tchr cierinses.frtie ntnester ea. .g. -4 assWm' o,,,nf _ 'i n ar,afe=*(pen. e.ekscus)-e. ts.t4) i "**' *""'h'dh"F* ***'" k'C S y 5.n24 c.n27 gj At-150'C]l At 18'C s a m n m m e-e c.nt35 -sens.+1sn g,g,g,, ,g Apptsentenn erene,*C fielecinnstely between eewapewesive streesdi, foers itensity, snel reiselve Theenial.estativity,"C 13e Figere 5 F-iMusensionalcbuse,bhec -g.3 14 elays at130t se - 5 3 -g ,,, i,,,,, i j Phennlic founs have ozhellent thermal stability. At inw tempern-m I' ~I se tures (even -200"C), essestially im change hi mechanical behavior = j j 'y* ~ has been noted. Phenolic foams are ilurnhle up to 130*C ned retain 90% of their strength properties at 13tPC tuuler continuous stress. j se 'Ihey enn tolerate 180*C init for noly a sleurt time. lleynml 180*C. th ~ , og g,,,,, foam structure enrbonites and shrinks. 'Ilie values for change in p2 - W 73,cf length (percent shrinkage) have been summarized in Fig. 8. The i t I 1 I e f I a d'" ' -20 o 2e es ao se aco trossoleo DO*C mmi 130*C represent shrinkage values for phenolic fonens o SI-G pef (or 0.04-0.1 g/cm'). As afie temperature is increased to 1*"'"*'" *C ris.rea neisis nssischet neencompesasw=*easth.temperahire.asnteleasity-430 .m.. m m-

m 4I FilEN01.IG FOM FR0l'EnTIET r-

3. Moisture and Moisf ure Vapor Absorptfors g

, rb no rutwouc Font PhenoIIC foams have an interconnected ccII strticture tha i 7 - m-oo4 stres ph, ac t,,,, nitts water vapor einite readily.Tlie h>ams slowly absorb waterunder - i i i. - i i IJE 6 - e o.it sha* r====n *== conditions of totni tunnersion. l'aul(13) has shown that G E ""C cnted with skins have better properties, since the " skins'* significant-g ly redtice the rnte of water ur moisture vapor absorption. Figure g,3 g and 10 compare the water nhsorption of the phenolic foams made % 4 3 from the Union Carbide resin system (Fig. 9) and the Dynamit. N ~} [,_ _g-qagc_ system (Fig.10). 3 j g ~., .~e ,,,,, i,_ t 'o~ a,

4. liehaviorToronrnlChemicots t 2 4

s a 10 12 14 Phenolic foams, tested for 2 months at room temperature, showed D"* **1' = wknas chemicids. For anniple(M), these Osense he lee gth (%) of plienelle bne aner enpos ure to heat. hmns am u"fetant to 20% hydmelshn-1c neid, 50% sulfurie acid, te w ng ustmuse Fisere8 ) d 10% nitric acq,.md 80% phosphoric se,sd, as well us to the spread between the shrinkage vahtes for low-density (-x-anhigh. density foam ""d hydmHuonc acid. d i st.ic potash is obt ined if the foam is subjected to n repent 16-hr cycle. At tempern-k 1,ml aged utmsum to causue smla se ution am enu tx.res nhove 400*F however, dimensional stability falls off and shrin - soluHon destmys dm h>nm simetum, aldunindi die fonin is msistant to anunonin sulation and inany snit saltitions (neutsul, ac,d, or alka age increases as exposure time is lengthened.Phenotic resin foams contain trace amounts of volatil l i ne.ts aRer expansion and hardening. These can be condensation Phenolic funms wem alm usistant to the Edinwing organic soi-II"*)- water and traces of resid:ml acid In many areas of application,vota-tilo components such as these are timlesindde and nuistbe mmoved. vents for 2 nmnths: phenol (90%), nulline, diinityl phthalate, custor Volatile components are removed by heat (nging the foam between 100 and 130 C) or by treatment with amnionia or mnines to neutralize ~ as u 3 i th2 weld. Table VI shows the time at which volatile components havebeca remove rs "h""' i"S l**3 g $8 w swe % "u ll cism cf removal of vulniile etunponents also illustrates the open.ce et I.s 1 structure of the phenolic foams. Y,# 1u g 12 Tt, g ie 3 TADIE V1.11eemyn! of Ilesidual Vehtdes frews l'henolle $ 18 Fenni et lotrC 33 E ~ j,a i Mhies SpeclAcetravity 'Thwest lessin Flwat specille ~ s ~ before drying 100"C;,

we3nha, genvity nner

~ ] einys 11,, liens trentaient 8 III 200 Jdt fB SEE 100 708 WB 1881085 g. g ,e tu Its 3ss 40s les see no tm gesteel Espeswee t6me, br 0.01 150 1 18.0 D.03M Esposanetbne,hr D.pl 1.50 3 18.9 0.0324 (6) fe) 0.<W1 3.74 1 ILI a.051 0.06 3.74 3 IX.I 0.051 Water esul anotsture vnenr efesweptinse afphenolic knes (if.CJ (ne(.13 dieu et lon11. stil,s3 C. 19sure5 (n) 5=1mierston in water eif 2 per Ioain. (bl Weter abswri 9.10 0.24 1 17.1 0.081 rt 1.In 5.24 3 17.1 0.081 c

,A 44I CHAR FORMATION AND THEftalAI.DECOnll'OSITIOff h' I8 I8MOIIC N strtechareg aher evntwratinu aithe snivent the inams again slmw their 4 3. i i i i i iis s

I original propest(es.

.m 33 l' 4, ~ I' VI.htECllANIShl 0F CilAR FORhfATION AND THIDthfAL s s,.e S - an w.=9 2 at a ~ DECOhlPOSITION -Y ~ One of the great attrilmtes of phenolic foam is thet it is fire resis-I 3,,, Y## tant. When a slah of phenolic fanm is Intrned, line Rame causes a = light black char to form at the point of ignition.Tbc char insidntes th 3 s E fans fran further Imrning,ami, if the Same is removed, the phenolie 4 - "3 Team will extinguish itself immediately. Phenolic fonms have been known to " punk" or contimie so glow mRer removal of the Rame: 2 Recent fosens seende by Union Cmbide, Ibstigel, aml Dynamit-Nobe I. a i e i.'i i i i. i i. 14 stop burning when the Name is removed. a3 4 7N The thennal degradation of phenolic resins has been the sid ject of numenms studies (27,28,20). West directed towant an umler-standing of the sectuential processes ocenrring during cure, posteure, degradation, and char formtion has been facilitated. ta Between 250 and 400*C water and formahlehyde are clieninnted i 12 by further condensnHon or climination, as shown by the disappear- ,,'[ ,,,3 ance of methylof groups frma the infrared spectnem(Fig.11).Cadmn 3.1 400-600* from the 18 dioxide and enthon monoxiale are climinated at (es - ,,8',',',,,,., henzophenone linkages amt from the phenolic anmps at 600-750* (eler Innnntion). Ilydrogen is also climinated during char formation. os The cheenical ecputions sluiwingi; the proposed rentes of decomtiosi-o.7 -n

e3 tion are given in Fig. 11(28,2$1) and ehnr formation in Fig.12 BE j oss *-

7; f o.4 (28, to). Olt Ogg 03 Ogg .3 CH. "=0 02 - Cit,Ott .g. t ., s.. t...... 1. I A c. , l_ t 14 i 0 I 4 7

- r*

l i $1 t Water and seelsture esper absorption of phenoMe femmis. (dWater als-Mer absorptiest fier storage In mir witis 93% RIl at Figure 19 sorption omiseneesien (DN). (b) W Oft 0 13 So C(DN).(Ref.It) CH OH + H.C= 0 ell, mineral oil, ether, petrol-fuel mixture, benzene, carlmn tetra-i g a i cidoride, acetic ester, med cyclohexanone. They are, however, re-vatura sistut only to a limited extent to methanol, ethanol instanol, ncetone, ll in thesc l* methyl ethyl ketone, and dimethyl fennamide.Tiwy swes:lvents, but the swelling does not ca l'esteurfust remettavis ylchlfvig it.CO+1f,0. l Figute ll ? y

-JAN-29-W FR1 02:49 Ptl f* ** P. 14 l s e sa4 ag t 1. B 3 s u ('E !kj if9y* 3{ 8 y 'i"I~'j 4 IR 4 fil s d $ $ $ $' ' '4 (5 E M Il a g" f 5E$I .l ~ Ig 5 4 53 2 fr!*!lDgf I Ik !n$ j f E. iji .'i 3 #d !hi ~ile.O p d1.h< s eIIp.,$ l. d h I }

S,i 44 8I i

!!h$f Ijk b giifII f 1m iulsmaa%=d4=J,amiln4,n ff:+004b.i d 1 1 s,h a f,d sg id a4 o. ga d 5.- z jd.! 'S, s 4 f e % ;g f j el-l}L4 } a( d e = .a f1g d cEtF i 1.E i l ~ ~ 3 1 3 o n..~iu a+, e sa, m,.a,e a u a. h. e, b a s = n,aasa a aaaaaaa 5 dddi AdddAdddd i Y liiddd$$$ $ $$$$$$ ....,.,. 6 6 % ruepassa supmaoNmp PMs{ fused 31oan5M O 3 stl 0310 HQ f emu HQ + HO .y3 O=3+ ,3 f004 [ u=='9 3 O ' o: Ho NO i g HO HOO3 Ho HO O 5

.4

- m

L I S P. A R Y. ?..

w. n wum am.w.c.y cnm e

,[g: N u.t. c; e:u,.r,.e. .J e se,.,m eF.v.v.u m g! ta/21/7.t. ru' {, POLYMER ENGINEERING AND TECHNOLOGY [.Y PLASTIC FDAMS:thephysicsandchemistry il 0,$ of product performance and process technology $\\. 8l Executive Editon D.Y.Bosato. y j @i Editcru B. B. Akin, H. F. Mark,J.J. 5cavazzo, i J S. S. Stivala, L.J.Zukor voimutin STRUCTURE PROPERTIES, and o [. sTNTHEnc FIBERS IN FAFERMAE1NC pM,. APPLICATIONS Eated byO. A.Battista [ " M_l L 4 Ayyllestions, FILAMENT WINDING,lts E..i. - . F, and Desism I D.V.Resete and C.5.Crove.)r. ( REINFORCEMENT OF ELASTOMERS EdisedbyCeverd Ernes .h EE I* O yf, EMv5HOMMENTAL EFFECTS ON FOLTMERIC MATERIALS Q velames) ' J-7 Edhed by D.V. biete and R.T.Sefawerta Corporefe Research Center, International Paper Company FUNDAMENTAL ASPECI3 OF FIBER REINFORCED FIASTIC COMPOSITES Edited by R.T. 5 eleworta med IL S. Sehworts g,.. -rt - D d -l M AN-M ADE FIRERS. Selenee medToeireelesy D volesws) Q' .b Edleed by IL F. Morn.S. M. Atlas med E. Cornia .h TIIE SCIENCE AND TECEINOLOGY OF FOLYMER FILMS Qvolessee) h Edhedby OsvGle J.Sweetles -a FLASTICS FOR ELECTRICAL INSULATION Editedby Feel F. Bruins EPOXY RESIN TECitNOLOGY ~ Edhed brFoot F.Drelas ( Wii.EY-ilITER$ctENCEa dMWen of POLYURETHANE TECHNOm London Synheer Yeownto Eatedby FeelF.Brules John 1FEey endsene New York n, PLASTIC FOAMS.VelemesIandH g [ Cd,se J.noenses b." AdditionalVolvenesin Preparation t a L t 3 i

I 229 TOf,DfEl 'IUC7VRE AND FDAM PROPERT7Er O phmots enn be formel:ted inta foemabla resini withon tracting V. PHENGLIC FOAhg from their prop: sties, it m:y be pessible to produce lowest struc-tures having properties competitive with those of urethants,with the A. Introduction added advantage of b eing nomburning. la Chapter 5 of Volume I we discussed the major phenolic Work has been done on the pswduction ofphenol-rubber compost. 2 processes and products of the West. The literature in England. tions for filling propeller blades (1). -a Europe, and North and South America is devold ofdetailed studies en g the offects that polymer propestles have on the properties of the foam. B. Phenolichesins The Soviets, on the other hand, have followed a different route.Their In Enssia, expanded plastics based on phenol-formaldehyde sesias work is concentrated in the area of homopolymers (called FF resins) bt-Mby se ellhpass whod% R and their combination with nitrile rubbers (FK). A book published by The most widely used phenolic foams are those obtained from 6+ V. A. Popov and V. A. Kondrat*eva describes some of these processes novolac resins, and their combination with acrylonitrile twbber and C 3 cnd technology (1). Phenol-formaldehyde resins are very well known and have other high polymers. The Soviet expanded phenolic foams are also evioyed widespread commercial acceptnnee for many years. He based on novelac resins and are also brittle, like resol-type foams. valuable technical properties sad the high thermal stability of One of the basic differences, therefore, between Union Carbide and Dynamite Nobel foams mwl the Soviet foams is the starting resin. phdhelic plastics have attracted the interest of many investigators, %e diference in resin structum results from the method of preparn-Information has been published on various methods of producing tion; for example, phenolic resins are primarily polymers of phenol phenolic resins; these include the mechanical foaming of aqueens dispersions and the expansion ofliquid resin systems based on the and phenolic derivatives. In their simplest form, they are condensa-heat cnd catalytic properties of the hardening reaction (Chapter 5, tion products of phenol and formaldehyde. Under the influence of Vehame 1). In spite of all these works phenolic foams generally have heat and catalyst, the phenol and fonnaldehyde condense to form ona basis deterrent which, above all other failings, has limited their high-molecular-weight structures. The structure of the condensate more widespread use-at low densities (less than 4pci), they are depends on the ratio of formald'chyde to phenol and the type of brittla. Research directed toward Itaproving tins property has caulyst. Base-caulyzed reactions had k Hear-type eldes sabh m t evidently resulted in proprietary systems having acceptably good water. As molecular weight increaser, solublity in water decreases. compressive strengths. Some of these systems are described at tenge m the Soviet literature, and several scattered references caist in the These resins are called vurcle and have the following structuse: j, literttwre of English-spea.nns countries. . mon Brittleness has been reduced in several cases. For example. ,,t"." ""c" ,,, ewen noa 7, cidehydes will react with polyamines or alcoholic hydroxyls; the

a'.a A

- sme m"-. rddition of polyvinyl alcohol, ethylene glycol, and other polyhydric u a cm,. ricohols has been noted; and long-chain dioles,like polyether. glycol y I or polyols, provide a plasticized foam prodnet. Polyamides or neutral proteins are also useful as modifiers to substantially improve cell structure uniformity and thoughness(1). In all cases, the best method Ier cbtaining improvements has been by adding the polyamines, l polyamides, or polyalcohols to tha u sole at an elevated temperature ();ss than 200'F), after the resole mdensation is at the desired level m, o, oe *" In 1963 new phenolic resins baseu spon polymethylene polyphensis j were announced by Koppers Company and said to produce flexible ~ structures which are homogeneous and which combine toughness { cn, with the other desirable properties of phenolics (3). If these poly- ~I ~ s. ^

n, g g ' rariusn mucuns uto roast rnorsarres g'-l 28 ne resels structure is determined by the catalyst and the ratio of ' I ' l ' l.' i 1 is jl dehyde to plienol. %e methylot gmup is activated by the basic u i i]3 gl italyst and the phenolic group to yleid reactive condensat on is hl g olymers.%ese sesole resins are soluble in water, alkali,alco o s, 3u g 3l nd ketenea, depending on the degree of branching or crosslinking. g32 1.23 Acid catalysis leads to novelses and produces methylene bridges 33 y ' gll h f d g - irectly. Thesmoplastic resins of low molecular weig t are orme t to '* [ gi lirectly if the ratio of formnIdehyde to phenol is greater than 1.1:1. }g ~ Ej f I or more moles of formaldehyde are condensed, the reaction - **~ >roduces an infusible crosshked product. %e thermoplastic is l bl or dialdehyde or a mixture thereof) may 'ee added to produce the 4 - e4 alled a nocolac resin, and addition I formaldehyde (or diamine or - 02 2 = I e 1 1 1 i o n .herstosetresin: OH 9 to so 3e e OfI Cat. perte ruster conteel, plir OH i 1 a + M,0 8N 88'E IMPEE% Wb es a fusectiest.(rub lperegetagg, a n. + Cfl p - i n l e, in cll cases, the choice of catalyst and its removal or neutralization, and rubber-blend-type foam consists of two stages- (a) prepah i bility of snixture, and ib) charging the mixture to molds with subsequent l when the desired degree of reaction is obtained, determines sta Res:les are much less stable than novolacs, but so complex are the foaming andhardening of the composition. Formulations of expe=Jed phenotic (FF) and phenolie nitrile reactions that the conditions of preparation are the principal detesmg..(FK) foams contain pheno!4ermaldehyde noblee4ype resins, acry-i nants of stability.Therefore, the Srstbasic differences is in thechoice lenitrile rubber, hexamethylenetetrasnine, a hardener for novolse l t sIresin. Soviet phenolic fennis and foam blends use novolac re: Ins. resins, sulfur (vulcanizer for the rubber), and azodiisobetyromitrile n! (AIBN, the blowing agent). Table XXV cantains formulations of three R C. SevictStructures Phenolic foams based on novolac resins have the same deGelency types ofcommercialSoviet foams. g! l d fragile. as these based on resole resins: both are very britt e an

- - - d"*"d M*""' Mss) j Soviet work (l) has shown that clastle emnposites een be obtained by l

tha comidnation of phenol-fornuddehyde novolac resins with mery e-C***"d ** % U-Pensbyweisht nitrile rubber. The nitrile robber is a plasticizer and an integral part i Tn d hvet e stubber p esty.f of the polymer structum (graRed copolymers). According to Popov [

wf P astic resin Heusseine 5KN-40 Selfer AIB M feasia.g/cm
l d t re tnd Ksudrat'eva(1), the noost uniform and valuab e pro uc s a l

cbtained from surferials having a maximum nitrile content. Anincretse in rubber conte f"oo iii si 'il i "3 rr.m 0 1.1 3.s e.s-os-i thermt1 stability, med compressive strength and, conversely. In na 4 yx.4e soo no . Increase in specific impact strength. Figiere 51 illustrates the com-i pressive strength and impact strength as functions of the ru' ber

2. Preperaden o

contentin plienotic foams. The phenolic foamable compositions are prepared in the forra of'i

1. Formuladon and Technology dry powders. He ingredients are mixed In a bmII miti for several

%e industrial pacess for making novoinc. type phenolic resin Gl t f j

^ t NE M

mt.ntdx sntucnnte Ano roAu etton'sasics

- =_ i 17 hf ig I . Ilie Anal powdered mixture is used directly in t e oam n i t. ^ ts rv - ,] . tion. Fd-20 and FK-40) are as 32 rubber-modified phenolics (types d by two-rollmilling u tred in a ball mill (dry ingredients), followe ll

o:> pounding with the rubber. The mantiention on the two-ro

' is kept below 70*C to break down the rubber and maintain m ,pr % is. am-zo r=sa { e mixture.Three types of compounds are made by this process;(ball milled 32,g y_l l d . (sheeted off a two-roll mill or calender), pow ermill mixing), and strip (extruded tubing, rod, o

2 ;

y 11 rer content increases, the problem of smiforrn t ierature control during processingbecomes more critical. h I )ne of the deliciencies of the process noted by Popov(4)is t e S h I akage encountered in the early stages of molding when t e h der (FF) shdnks during melting and before expansion. T e ,j s uded rubber blends are more convenient for Alling articles since 75

possible to select the seguired density of the foamable resin s

, i, is or hollow rubes)to All the interior of the mold cornpletely. Wts sj l ?oaming(1) f4 ll I the Erst E ~

3 t

, Tha foaming process can be samnarized.as fo ows. n 83 i ' o cf heating (80-90*C) the foamable composition sonens to a h 't I cous liquid and shrinks in volunu. Between 90*C and 110*C, t ed the mass expands to the predicted 1 2 I t e is raised to 3 1 nf , wing egent decomposes an sume. After expansion is cod.;&te, tlic tempera ur o e 1 i a e r l. 5'E, tween 150*C and 350*C to cure the phenolic and rubber compost-layer of 150 200 250 soo 350 4o0 as. "llie curing time depends on the thickness of the Te*c l ii p nded snaterial, the structure of hardening and vu can z ng Fiswee st selen tap t et ,,,,,,,,,,,,,,,,,g,,,,g,,,,,,,,g gg,g, y) ditivss, and the conditions and types of heat treatment. Aher the d the process of pro. .mpletion of cure, cooling takes place, an anses an increase in shrinkage. Shrinkage is more pronounced for 't icing the expanded material is complete.P;viev and coworkers (1,4) have pointed out that considerable the higher-nitrile-containing phenolic femms. Figure 52, ou b obr hand, also emphasizes that, as temperature is increased, the degree of ess:re (depending on Hs0 and AIBN content) is generated (be. cure increas,es and that highly cured nitrile rubber-modi $ed phenolic hi es, seea 45 and 75 psi or 3 and 5 atmospheres). Various tec n qu d ich as bleed ports or small vent holes, are used to elivninete voi sfoams require the higher cure temperatures. One would hope that the mechanical properties of the phenolic f id pockets and to relieve the excessive pressure. d he trile mbbenmodi6ed phenolie foems (FK-20 and

0) woofd improve as the tenopernture of cuse is increased. How-

. Refationship betaceen CuringTemperature and Proper ever, at higher temperatures, thermal oxidative degradation begins, fi as is seen from the results of tests on the mechanical properties of the Process studies undertaken by Soviet scientists have emphasized i expanded plastics in Table XXVI. For phenol-formaldehyde foam h i l ic critied effect of cure temperature and composition on mec an ca r:perties. Figure 52 shows that increasing the cure tempera ure l (FF), the compressive strength diininishes sharply with an increase in i t i' I1i

f**% rnENUC FOAM UT the temperature of cure of the rnaterial, while the speciRc impact c_. E n viscosity and the static bending strength undergo practically no jll ( o h a 3 change. Thus, for expanded pl.stic FF, a enring temperature of150" e : for 90 min is sullicient. Table 7XVI also indicates that the El 3 g ]w properties of exposided nittfie rubber modiSed phenolic foam im-yl' g ~ prove on raising the tesntw:rature of cure to 200*C but deteriorate 2 with a Inrther increase in the temperature caused by degradation of S I h A D the polymer. %us, phenol-rubber expanded plastics cured at 350' i their properties to the more brittle. phenol-6,! ~ o o 2 3 g ~ approximate in EI formaldehyde expanded plastics. %e data published by Popov and his coworkers (1-4) indicate dmt et curing temperatures up to 200*C must be needed for the nitrile g 2 8 phenolic blends, since such temperatures increase the degree h 5 cure and improve the properties. Since a high curing temperature is i& eg not always possible, one would conclude (on the basis of these rate curves) that a longer curing time at lower temperature would yield P T e ( U beneRelal results (similar to peroxide curing of thermoplastic foams). ~ ~ 3 g a E E s S N

5. Frvperties ofPhenolic and Nitrife. Phenolic Foenir Depending on the rubber content'in the composition and the
}

amount of blowing agent, it is possible to produce phenolic foams 2 /D R having various flexibility and clastic properties.The basic prope ties ) a E ' d E 2 o depend on density and vary accordingto use temp i a E ?, R wi are as follows- [ 3 b d D M Type FF Feeni (Novelae-Type Ptmeal-Fermaldehyde Foesn)

r i

l o Q X g 02slem* en Density tLs stem' ~ g Tensiteserene h s 4okalem' o E j Cosopeessive strustli { a ~ 0.2ks e=1cea' e-g speciseimpact strength 9E% g Lineersliinkage at100*mAerI4 hr E g E d Water obserptioneher34 hr DJ kgrin' 4 A n g-nenunt-.?mier e.ostkeallenhe*C as. o ci With an increase in tersperature, the speelAc impact strength dimin-d l y o 3 E 4 Dl 4 ishes, while the compressive strength rises somewhat at Erst i U j and then also diminishes %e linent shrinkage of expanded plastic FF increases with a rise in the temperature (Fig.53). g At 180-200*C the process of thermal oxidative degradation begins,* y,g g g { the expanded plastic darkens, and its strength properties diminis J: g ! y'g' g g"g j 4 ? The limiting working temperature for expanded plastic FF must be g E jfa #j 3 a g g a- " E if d ~" m 4

<m THENot2C FOAM RSS rot 5MEtt STitUCTUltE AND FOAM ritoffJtTIES The mechanlemI properties of expanded plastic FK-20 are given in 3j c- 'A re o.8 g g g g 3 TableXXVII- ' io! u - TABI.E XXVlt. Propeoles of Empe. led Flame Ps;-to wah a % of 0.05 0.1, =s t a Ann 24 W ge,,,*ind. ) a swsebe.fh.g 5! e4 conipressin nrensin, specisei.e.ctnr s, ke emic==' strenge,hefem' e: e ao3 - kg/cen Si {

- " 8 8 "

oemier, o

)g4 g/cin' At20* At30* At20* At130* At30* [ x j o.1 - 43 1.8 ene o.4e ns om a.o 1.s oss e.ss ss 02 0.05 2.1 f.6 4.23 0.19 2.8 f l At 20*C (room tempenture), the strength properties of expanded e.s plastic hm (FK-20) with density equal to 6.24 pcf (0.1 g/cm') are l I I i I I 'y~~~ lower than those of polystyrene fomen and rigid PVC foam but approwi-8" 8' l 'c mate those of polyurethene foam. However, in its thesmal stability. l Pem t siirinkane Cinearl d pheade f*== 10 Es/c=W Pc0 m a func-this expanded plastic esceeds all these other foam materials, retaining Ho= d', "-IHd 1) 50% of its strength after heating at 200*C for Shr with the necess of ris, s2 considered to be 150' (1). The phenolic bm 1 Ld from novolac atranspheric oxygen. Experiments at a high teenperature show that l with an increase in the temperature the strength properties diminish, rssins has low water absorption (= 0.7 kg/cm' oAer 20 hr)(1).Barodin and Corskil(I) have stu wherees with a decrease in the temperature the brittleness of the I materialincreases. tha nitrile-phenolic foams (FK-20). Their data show that the rubber-The Soviet scientists have modiGed the FK-20 foems by a diferent 5E -r modiRed phenolic foams exhibit mechanical properties that are type of expanding agent, namely, aluminum powder. He ahiminum gl common to those of rubber-modined rigid bm plastics. For example. reacts with the hardener to yield hydrogen gas that expands the an increase in density (volume fraction of resin in composite) leads tocomposite. This hydrogen-expanded phenolic-nitrile foam, which-an increase in the strength properties. Barodin's investigation ofhas been called FK-20-A-20(1),has betterheat stability than expanded h 150-200*C, the dependence of the properties of expanded plastic FK-20 on t e FK-20. For example, FK-20 darkens and deforms at temperature has shown that the brittleness of the material increases whereas expanded plastic FK-20-A-20 veteins its strength properties at sobrero temperatures, while the speciReimpact viscosity decreases at 350-400*C. The compressive strength diminishes only slightly I nnd the compressive strength increases. With an increase m tem-between 120*C and 400*C, and the specine impact viscosity decreases perature, the compressive strength, the bending strength, and the sumoothly with an increase in the temperature. The mechanical properties of expanded plastic FK-20-A-20 are given in Tables speciSc impact stren gth all decrease.Tha linear shrinkage of the expanded plastic in air sbes sharply king 4 XXVIIIandXXIX(1). i with an increase in the temperature (Fig. 53), the limiting wor W th an increase in nitrile rubber in the composition, the elastic j properties of the foam change: compared with FK-20 (20phr nit temperature in air is reported to be 120-130*C.Becently, the Soviet scientists have made nitrile rubber in 100 pts novolse resin), the speciSc impact. viscosity is i lic Isams (FK-20) at very low densities (=0.05 g/ con'). The require-doubled, the elongation is increased, and the tensile strength is i-F' ments for mnking these foams are (a) a resin viscosity less than decreased, but the compressive strength does not change, since the c$ 100 cP,(b) 5 ~1% blowing agent, and (c) special mold linings. h i-j i ~ ^r

P p MtEA.FOllMAGGFDE FOAM NI e. 3$ PotXMER STRUCTttnE AND FOAST FitOPER77EJ TABLE XXX. hineheescol Powpedies of FE 40 Feasie % d c.16-Ei TABt.EXXVIII. C. l ;FrePerties of FK-10 A40 med FE-26 Femms(Ref.1) e.Is siem") rh FK40 { P asGe.'C 'f' l T**P"'" 'II'88I*E II FK.30-A 24 g g%.C 40 'M +se +se +100 +135 +1:0

,,4 so soo uso 300 350' se n00 Property w

] speci5e tseyect O serength,ks emlem' OJO 04 6.45 1.16 12 L5B TAB 23 gu l ,y,j s 13 0 10 3 30 2 10.0 gA 30 s 62 c.,,,,,,,,s. Compreestve sweesth, strength.hg eseleve' O.74 05 02 0.58 0.33 oJO o.3D kafem' 23A NA 17.3 13 ru l ,q,,,,gth isfem Tenede steweath, gene,g,1.g,g, gt spectacimpact 7A 4.7 3.0 ksfese' Se.5 Shriebene eher34 ter,% RA 2.5 15 32 .a 4 (e.pe,lemenes ts eer) indter 1br) struc'ture, and density than on resia composition, we would predict l that the FF (novolac phenol-formaldehyde foam), FK40 (tophr I material to elastic (see Table XXX). At subzero tesaperatures, the nitrile rubber added), and FK-40 (40 phe nitrile rubber added) foams would have similar K values and that with a rise in temperature brittleness of the expanded plastic increases and its properties sp-and an increase in density the thermal conductivity would rise some-pr:xircate those of expanded plastic FK-30. At normal temperature,FK 40 foam has higher impec what. predict since the concentration of nitrile rubber in the matrix is i VI. UREA-FORMALDEHYDE FOAM doubled. Since heat-insulating properties depend more on the gas, cell! Although several detailed monographs have been written on the chemistry and mechanism of wren-formaldehyde condensation reac-i tions(1,1), little information is available on the subject of condensa-htechenseel Freportler er Espeeded Plastie FK.so. tion reactions and the expansion procese. ne only information that n relates foam povformance with polysmer structure can be found in the R. TABLE XXIX. 3.,e patent literature. Tampente** of die Melsmine may be used elther in place of urea or with it to prDduce

f Density.

= I structures contair.ing slightly diferent aminotriazine resins. Mels-PP'"Y mine formaldehyde condensates form stable solutions between pH 8 and 10.5. Sulfomate salts have been used in this system to ensure the c.,ep,,,,i..e,,eg i, kg/ce,= 10.14 83 5.3 g required degree of condensation (3). Primary triots have been em-l lo.no ssJ 11.9 318 N3 played to modify these types of resins and are reported to improve Covereesolvemoduhs eteisenchy. {e.it W 383 8 i 8[, the resistance of the foam to heat distortion and cesching during cure karem* 78 Temalle strenstk.hefe=' 3 and after cure (4). The use of primary polyols and triaRtylolamines i (!.e., triethanolesnine) is also described as producing heat-cursbie dos 33, T*" 1,ned.hisierelesacky* (c.10 J o.se 7ss st7 foams based upon the aminotrinaine restas(5). These resins can 3 neleuw eleenietes,% 10.11 1JU accept high concentrations of Sllers without cottapse. 10m 22 In our discussion concerning the foam formation of uree-format-s.rr 1 21 shear stemisih.hafem' ha.34 T is (see Chapter 6, Volume I), we noted several variations 8 h dehyde re ~" in the basic urea-formaldehyde condensation reaction that were used o'.13 231 M t S1,eer meduhes efehseefty,hafem ru [ f j

. ~. - Director i Office of Nuclear Material Safety & Safeguards February 10,1999 i (? Page1of1 j i I l Phenolic Chemistry: A Brief Overview Schenectady Chemicals, Inc., John Sullivan,1987. 1 l l i f-I l.

JAN-2F99 WED 08:52 M FAX N0. P. 01/21 'I I2 SCHENECTADY INTERNATIONAL,INC. FAX COVER SHEET DATE: January 20,1999 Tsae 8:53 A.M. To: Charles Vaughan PHONE GE Nuclear Energy fax: (910)675-6350 Pnou: D. F. McLaughlin PHONE: (518)347-4422 fax: (518)382-8129 Number of pages including cover shest: 21 f b 33090 l Information you requested is attached. k t I i .}}

ML20207E066

Contents

Text

Subject:

References:

Subject:

Dear Mr. Vaughan:

Dear Heather,

Navigation menu

ML20207E066

Text

Subject:

References:

Subject:

Dear Mr. Vaughan:

Dear Heather,

Navigation menu

Search