r viii - volume 3... · r c. namee of personnel involved 1n the boron procurement act1v1tie&...

63
r 1- 4 ;:.. r , OE PAllTMENT OF EllERGY DECLASSIFICATION REVIEW l!t K.E.VlEW· ·: q. ,,. IJETERMft.'ATlOH !CIRCLE NIJ MBER(SIJ

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r 1- 4

;:...·

r , OE PAllTMENT OF EllERGY DECLASSIFICATION REVIEW

~ l!t K.E.VlEW· ,~ · : q. ,,. IJETERMft.'ATlOH !CIRCLE NIJMBER(SIJ

...

l. General.

...

'· MA:illiA'.fTAlil' Dl si1RICT HISTORY 300K VIII , T.iOS ALAMOS PROJECT (Y) VOLUM~ 3, AUXILIARY ACTIVITIES

CHAPT".tiR 7 • :BORON (:810)

a. marly in 1943, the Loa Alanoe Laboratory indicated a need !o~

qwuiti ties ot cryatalline boron ot normal 1aotop1o content and c17•tal-

line boron enriched in Bi.O (see Book VIII, Vol. 2). Production of the

material• waa initially reg~rded as extremely important and ver, essential

to the overall Manhattan District 9.0tivi ty. While neoeesi ty for the

materials was somewhat modified. a. t a l a ter de.te 1 nevertheless. from the

be«inn1ng the. boron project was given the highest priorit7 and every

e:tf ort was made to assure t hat production vould be as prompt and a.a

effici~nt as possible. The original requirem&nts included the utmos'

secrec7 and minimum public1t7 in all phaees ot the material production.

O<>mpliance w1 th the aecuri t,. restriction.• ca.used many of the nego\1a.tion1

to be conducted through oral discussion and thua limited correapondence

and records to bare essentials.

b. The desired materiale were obtained through1 reaearoh and

developmellt by Columbia Un1vers1t7 {SAM taboratoriet) ; developmen\ and

proceuing b7 the Norton Com:pa~; supply of raw ma terial 07 the llarehaw

Chemical Compe.?l1'l development. design, pl ant conatruotion and processing

b,y the standard 011 Company of Indianaa and development and prooeesi.ng

by the ~\mericen Cyanamid Company. ~ach of the orga.ni1~tion1 involved

and its respective performance vtlt be referred to herein under a

separate heading.

r c. Namee of personnel involved 1n the boron procurement act1v1tie&

m8¥ be found in the appendices to th1e chapter , and in other vol'Wllet ot

the .Hh tory, to which ref'erenoes '11111 be made hereinafter. Those who

were oost concerned included the following:

Dr. J . R. Oppenheimer, of Loa Alamos taborato1y;

Dr. K. c. Urey and Dr . Martin Xilpatrlck, ot Columbia

Univera1t1 (SAM Laborator1e•):

Dr. Oyr11 s. Smith, ot the Horton Co11pan7;

Mr. E. G. Seubert and Dr. E. W. Thiele , of Standard 011

Comp&nT ot Indlaiia;

M&J. Gen. L. R. Groves and Lt. Col . J . R. Ruhoff , ot the

Manhattan Dis~riot.

2. Columbia Un1Yere1tr. (Refer t o App. A-1 . )

a.. In Mal-7 1943, the request of the Loa Alamo• Laboratory, described

above, waa diaouseed between repre1entative1 of Columbi a UniTersit7 and

the Madison Square Ar ea. That disouaaion resulted in arrangementa where­

by, under Contract W- 74<>5- en&-50, Columbia 'On1Terait7 was to proceed with

the necesaar1feesearch and development for the pr oduction of 500 to 1000

powids of cryatalline boron of normal iaotopic conten' and 50 kilogr&lla

o! cryatalline boron containing no' lee• than 90~ ~o.

b. The need for thia work had been anticipated by personnel at

Columbia a.nd four months earlier (in Janua.r7 1943) , under OSRD Contrac~

O";]Msr 412, r e earch on the separation ot boron isotope• had been started.

That researoh had resulted, in April 1943, in the discovery of a promis i ng

method ot operation. Such a method ot operation waa still being investi-

gated when the Had.ison Squs..re Area arro.ngementa became effective, but

the tnformation ~hieh had already been obtained was GUCh that develop.

men1i could• d dtd, proceed "71 th a minimum ot dela.y. The separ a ttoa

procedure , which w9a proven to be suocessf'u.l by continued inveettgat1on

and. plant operaiion, was based o~ $ counter-cttrrent dlstlllatloa ot a ·

dissociable complex or pol71Der.

e. Ia add1 tion to the atud7 for separation of boron iae>topes ,

Columbia 1~1thted a research program concerned '11th trut reduction ot

ot 'boron trtohlorid.t b1' b1'drcgEm on heated rode would produce be•l re-

aulte. and developm.eut work fo~ thit !eat'UJ'e vne carried ou\ in co-

operation with the N'ortoa Co11r1Ba¥.

d. The aeparated p~oduc\ obtained b7 th• method QeTeloped a~

ColU111bla wa.• dtmetql etber-borou trifluoride complex and 1t. W'!!ll then

neaeasar1 to u;nder\ak• research oa the eonveraio of that compound to

and developmen\ work w~a carried out in ooopcratlon with the ArneriCNa

J. Tb.• lfol"toa Ooiapf!Jll.

The Nortou Comparl¥ participated ill th• boron prog,,.aa undel' two

different li~ee ot pl'ooedure•· tiret, thl"Q~ cooperation w:l. th Columbia

Unt.versit7 in developinc the method of reducing bc:ron trttluor1deJ and•

$econd• ia :produe1ng oryetallins boron. 'l'h.eae activtthe ar reterrecl to

in Appendix l for the reductio• ot boron tritluoride fllld

in look VII . Vol . 11 for the production of or1eta.lline boron. Th.a'

.. 7 •. ]~ ,. J A .... ,

, production applied to materia.l of normal isotopic content and was

!3.CCompl1shed under Contract \f- 74o5-eng•292, effective 15 Januacy- 1944.

at a cost of $53.000 (See Book VII , Vol. 1) . Government- owned rav

material , which had been obtained from the Nia&ara Smelting Company, was

supplied to tho Norton Comp8.ll¥ for their process.

Con:f'1rmill4J records and supporting data for the Norton Compan.7 parti-

oipat1on in the boron proJect are, of necessity, extr emely eketchT. ae

particular care waa exercised t o prevent general knowledge ot their

s~tivity being divulged.

4. The H&rahaw Chemical Compg.

The Rarshaw Chemical Compallf vas selected t o supply raw material

for the Standard Oil procee1 of the boron proJec t . Contract W-7~5-eng-

289, effective 15 March 19411.. called tor a suppl7 of 650 pounds of

"synthanelt per \lteek for aix montha , starting l Ma7 1944. 11 S7Jithane 11 was

the code s1Jllbol for boron trifluoride containing not leaa than 97% ot

Bl3 of a s oonetan\ pur1t7 ae possible. SUbaequ.ent supplements to the

contract increased the quantity of raw material to a total of 92, 450

pounds , a t a total contract price ot $72, 770 (see .Book VII , Vol . l) .

Rav material delivecy- wae completed l March 1946.

5. Stand.a.rd 011 Company of Indiana.

~lhen research and development a t Columbia University had progressed

to a stage which permitted design and construction ot a production plant

for the separ a tion ot boron isotopes , contact was made with the Standard

011 Company of India.na (App. A-2, 3 & 4) . That company indica t ed its

3groement to partic ip~te in the pr ojec t ~nd on 5 J anuary 1944 antered

in t o Contract .v- 7418- eng-41 . The contr ac t ·~as effective as of 2 December

1943, the con t empla ted work cons isting of the design, erec t i on a.nd

operation of a aui table pr oduction plant for the s eparation of boron

i sotopes. In addition to the above work it was understood that the

St andard Oil CompBn¥ ~ould undertake work directed tovard~ increasing

t he oer ta.inty of the aarl1 success ot t he propoaed proj ect; training

of t echnical a~d non- toohnical personnel; and1 establishin« an &.dequate

securi t y sy~tem.

A g~nera.l history ot the contractor's activity in meeting contra.ctu.al

requirements is provided in Appendix 5. That history of t he separa­

tion project describes: the work objective& selection of the production

contrnctora plant des ign fea tures; initial opera tions supple~entar;y

plant conaiderat1ona1 and the then tutu.re possibilities of t he process.

Maj or probl ems wh1oh a!:f'eoted sch eduled production r eeul t ed :f'rom

difficulti es in obtaining desired conatruction material (App. A-6) , a.rid

the i nadvertent 1ntrodua\1on ot mercury into the plant sy$tem during

the leak tes t procedure (App. A-5) . 'l'he latter d1fficult7 waa considered

to be quite aerioue in 1ta nature and lad to the erroneous conclusion

that the initial plant would be unsuitable for production and tha• re-

pla c ement would be re quired. r.a ter on during the contrac~ a corrective

measure was d i scovered and the origin.s.l plant proTed to be operable for

pr oducti on purpos a .

During the period of opera tion, a total of 736 gallons o! he~vy

golymar '"&S produced. >\p pendb: A ... 7 providea deta ils of t hat production

in regard. t o l ot quantiti e~, percent of heavy polymer for each l ot , etc.

7.5 q ·~

r a

r ~

.~~ppendix 7 tlso includes breekdo iigures f or ,.the t o tal cost , undal'

Contract 1- 7418- eng ... 41 , of 2, 309 , 546. 88 , prior t o any adjustment required

b7 ! 1nal U<ii t .

On 8 Ma.roll 1946 the Contractor was directed, e2cep t for the economical

co11iplet1ou o! Jl\8.terial then being processed , to cease operation ot the

fac111t1es , ffective 4 Febru.e.17 1946 (App. A- 8) . Supplemental Agree•

men\ No. 5. ot contrllC• f-7418~eng-41 , provided fo~ the period ot pro­

duction pe~tormance to end a \ ll r59 P. M. on }O June 1946. Alao, ill

accordance ·-11th that suppl eme.u'81 agreement, the contractor placed the

proceaa equi pmen1 1n stsnd~b7 condition and stored 1uch equip ent at

va.1 directed by the contracting officer .

6. American Cza.namid Comp!DJ.

Contract ' - 74ol- eng-91 , dated 8 February 1944, witll tM Aulerican

Cyannmid Company. required the contractor to proceea product 890 A to

the final product 891 • 2 roduc h 890 A 891 A vere the ~e&pectiY•

code s11'1bol1 tor boron t r ifluoride dimeibJl ether compl~ and for ~tal•

line boron 101 9s~ a eea7.

The procese ueed iA oonvert in« the complex to boron v&a dGvetoped

under Columbia Contra.o~ w- 7lio5-eng-50 (eee App. ~l) , bu' the en@ineerin«

and des ign work neceesa17 to put the laborato1"7 procaas on a plant scale

It has b en nentioned that the initial requir men\ v~a the continued

production of nlO u.ntil a qUlllltity ot 50 kilogr ams had been comple ted.

1"'he production schedule called for 1 ki logr of boron ae early a

poeaible, a total of 5 kilog me by 15 September 1944, c 5 .dditi onal

kil.ogrl!ma every 1onth theret..fter wl.til the t ot!"'l of 50 Y-ilogr~.ms hod

been r;btc>.ined. 'l.':-ie :.tartup of the plant '"!:l 3 , of course , :lependent upon

the production of separated complex froo the Stand'3rd Oil Company of

Indiana. The rate of production of the sep~rated complex had been estnb-

lished, by the Chicego Area sud the Stcndard 011 Company , to be 5 gallons

every three da¥B• The plant of the American Cyanamid Company was designed

to run at twice this rate if necessary, since the Chicago Area had. int!-

nl!l. ted that the¥ might be able to rrange for an i ncrease in the r a te of

separation. The American Cyanamid Comp~•ny plant had undergone test rune

and was ready to ope re te by 7 July 1941.,.. Unforturu tely, material we.a not

available at that time from the S\e.ndard 011 Compan~-. '"'bile nw111 ting

material from the Standard Oil Company, work continued at the American

Cyanamid Company. to improve their process and to prevent possible loasea

of material . Upon the start o! delivery- of the 890 A complex from the

Standard 011 Company , the American C1anamid facilities were in re~dinesa

and proceon!ng to the final product began.

In accordanoe with su:p.;?lementa.17 requirements !or contract w-74o1-

eng-91 , production a t the American Cyanamid Comp~ continued well into

1946, and 504 pounds of crystalline boron 10, 850 pounds of calcium

fluoride- boron trifluoride complex, containing a greater than normal r a tio

of the BlO isotope , and 242 pounds of calcium fluoride- boron trifluoride

complex, containing a greater t han norr.:ial ra tio of B11 , ~as obtained

(see 3ook VII , Vol . l) .

" -... ..

"

COLUMBIA UNIVERSITY, DIVISION OF WAR RESEARCH ., '!\ii.

tfti'rifd li

Copy No. _ _ 1{_ • -p) :'\. •J Xr t ' LMttr >

1•£ I lll.

"" ''\.,' t ''It,-..,. < )R '' \! \ ',' I s I () A '-

Columbia ~rial No . ..lr.•( -9M

File Index 180 ~ . - .... ,., 11. 1941

. "' Disttibudoa

Series A

DhtJ-ict ~n..r (T.-mesMe)

Area lrtgineor (Col.) Urey. Be c • . 1nytht If. De

In ge1 eraJ, a cLn~ih ed Jocurnlnt sh.ill n.v< be •op1t.d or i.lup liuru.L II .hl :, t1on.tl t• T ll' ,rt nt~C sary hey ~ou!J bcre..;ue~ted fro11~ tl.e o•1 .-111.11 ir In . Ui t ri.:~ n,,. :1c;+.,,1.i,:1no'or 111:, .l="e telegr1ph1, approval

for repoJuctions , ~pecify1ng -nics !e• er l:l ~ 1 1,:;ilx r t I T''' Il· ··~·1r:1 ' 1r ·: . .< t be noti li < I irn~:ately

of th< 1 ribution of the •trro, l t. "'< ' :\ ii'··:. , · 'l' -1 r,n ,';. ,., . ~L u i.;!d be burned.

, ...

(

, •

• ..

The Separati on of '. he '."\o C' , \ I ~o tcpe s <..:. nd he Product ion oJ . '.ctal.ltlr 3or on

100UR~J4 ri'ilu 100 1 co / • J l-1.5 P..::e 2

Fir.al Rcpo1·t Subrlttcd 1n Ac cor <func e u it. · t · e TP-r rts of Contruct fl - ? 40S1; eng-50

Hnrold c. Urey J uJ.y )1,1945

I. Histori cul }{evi ¢n

In iJ!t.:,r, 1943, t he U. S. En. j:1er.r Corps of t '. •o L'ar Depru-t.Ment r oque stod thtlt t he necessary ruacurc~ -::or != be untl erta, c:t to detdr r.i ne mot;10ds for :.he production ot crystalli ne i0r on. In ac!d itio:i t o sor:e 500 to 1 1 000 pounds of erystulli..,o Jc>ron Of nor a.l i soto!Jic ccnte:; t , a need ·. ;~ s indi<".ut .~d fo1· 50 ::ilo::=-wJS or cr:.' s tullino boron conta i !1inr, not less t an ~ of n.10. Fo~unately, 11e need f'or th s 1·.o t e.·inl had been partly ant :. c ~pat~d :i t Col.ureb a. Univei·s : <:.: / i!..'1<'.i ::- ..; scru-ch had · '08 !1 s 1. 3.r".:.cd in ~anuar7, 194J, on t'.;v si3po.ration of t ho boron lso to~s , Wll".cr 0.-i.R.D. ~ntr...ict Oml•

sr 412 . In .\!JA.•i 1- , l<)I~~ , a promia inb · r. t ror l:ac: ..-ecn (: i s cc,,,er cd at U>l u."lbia, and mis uncL r inY€J Sti.c:a t i o·· ·

A pilot plant ·as set up to (lCCm rulate c:i; i>~cer .i.r. , data nec 1.. s sury l or the design Of 3 pl.e...1t -.,h ::.c h t .Ould SC/)Cr._te JOO ffT UI :S Of rJlO pt. r ciuw' • ln addition , & research ~o ·r·eJl ·. e s iu:i.tiat od to s tuc!y w.r ir us : ·e t:. hod . of reduc :il~2 boron conpounda. !!'tt::r a surtr~r , expe··inental \. ~r,: on t he r eduction of boron tricl1l o .·i tl :J "'! }\.~:rogen and of 'Joron ': lfl uor ide 'f.r;;· sodiu::i , ' ns carried out . 'l' '. 1c i -.c t od f i_:ally ehoacn VCL• t ho r <ductb n o~ :JOro:i t i·ic!tl.oritle l'J hydrof~ r .1 on :-.t:.:ted !-o J s , a •1c. t :1e J ..; •1olo~nt \10r1~ ··.:~~ carried unt in cooµ, :1.·at. j oi1 ·.: it i t •10 :•.: rton Co·1r aflY . '! he use. or t • i s T"s t.'1od involvoo t r e produc-c i on OJ" ~ron t~· ichlor ~cc of n.:. ~ · 1 f~Jl' it~' • ": . e ITic.:;nre. ~.halting Com:-..any \11'l.iorto<;~ t M.s . or1~ a !'l<l ;h·.o ' uc c~ ::;; ::fic 1.c:i '.:, t. :- l chlor~ti. t: : or t : c.. :-rronuction or t..'1e required i:.mou.."1t o~ c r:-nUi.l.l i .1u hor (, .i. 'i' ' d s .tH! ~ .us coir. ~i ctec· by t.~o !iorton Co!lpa.tv by t h;.: end Ot : ·l!.y I 1944.

. In t :,c ac.antfre, t >e pilot IJll..:: c. · .. 1r1: on t \10 s ap:_ru~io11 : iad :-;ro$'.,rcssod to a staee ·.1hera t he comtr..ictio:i of a pk . ~ coul d ·?a un· :r t.a.! ;J;. , cfl ::l in lfov Ci 1ber, 194), tho dcsien, constr.;oti c.m and O!JerA.t .:.o .. or a )lD.~t -. ·i.l.:; . ~a th:.. ::-c:3pc;ns .'..!Ji lit:· ot the Sto..~d ~l Coi · '.lCl.~.' ot Ir.diui'J! . As t:1a <; 1.:i-r::tted !'l1"0chlc 'i:. n s t o '-0 cl i.r:tat}\yl other•boron tri!luod dc co- 9 l3X, (ai1)io•m- , it t.·as nece~t.r:,r to u..w. :: r~ : :.i r c.:acm"Ch on t j1e co llVt!rsiun or t :!.1.s ecr. ·;JOu.'¥1 to ooro~triehloride hefeir e l' '-t'.'.l.c~: c:l'l -. l t h }\Ydl"O­gon. In add i ti~, rurt ;1c;:- r csCltl.'ch \ ·o ... ·i;. . ~s ncccs~' to add t' < : f~-· ~.:. :or.ts t o t he r ::-<.luetion step. ;. pilot ;Uant 1·as set u:> a t tile ColW4bi a laoo .·a to:!'ie '> , :o.:: ~ t~.e dovolo:;r.1(.. l'!t '. ;e rk ~ :gs carri~ out :.- ith t l:c /1 !"1~·..i.can C;1anw;Ucl ~1,a.,~ . T'1i1 co · 1~~·

".>ca;an -. or k in F'3'-::-u..:.r;1, 1944.

Al."tar s . r ·e dda~' duo to oiJOl·ut lo.-1.£.l di!':'icul t ics and acc id c?1tlll introduct ion of ··t..reury il"? t c t " c r> l a:1t, ~:r~uctio:i of s eparated horon a s t :1e il ~ .. t i~:· l ct~·,: .i: •boron trif luorick co :)l c.. x be · .. an :n Jarnl.1r:' , 19A) , t~nd 1:a s "Cgtlpl cted b . · .. :· , 1945. The ,..1-c r ic;. •. :. ·..;~· :-.n~Y"id C..,, r-a.v pl nt eobµl~tsd tho yroduction o f' cr:! s W.llinc :1r o!:uet ot S!'CCifiud [Alr it~ . .i.: 1 J \mO, 19/~5 • :'xporirc::t ul SUT :) l oe Of i;ll · .. :>rO fr. ;_ ;lf.l l' ~r1 .:_, t : 0 pilo~ !J!..'.::-it .'.1":.. Col·.t.:.Y :i .

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s p-. r :c :l·-, n , f I. ,, r . ! . L -.- !" - ~Y; r :-., ·1i c -.1 ! t h d.::;.

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J. Fro.c t. iona tion fa~tor fro:-- enri chment in S +, dr.lan pa " ku l colurm

4. Fra-:;tiona+, i on ri urirL_. r o uc tion .

..•.

' . ~. Val e ' f - ,.; fi a ·t i -: m1.t :0r. fa . tor.

l \.x;·_v.- • ~ -.

? il f' l r Pa t;" /. ' - Jl - !.)

D. Stability of o~plexes

1. De or:ip<isition

a. Rate of f ormation of r:iethyl fluoride b . Rate of a cumulation of methyl borate conplex a t :!1€ top of

the colur.in. (' . Manometri" re thod

?. • Pe r oxid e f orr.'.a t i or.

3 . Effect of wa~r

Phys i cal pr 0per t ies

l. Vapor pr essure r1 f methyl borate , diethyl e ther complex, dimethyl e ti 1e r ,..onplex, a nd mP.thyl borate cor.:plex

') ... ~ eat o f varo rizat i r- !1 f dfr:e:l.yl et her cor.plex

3. z· .. r.si:~- '"" f ii p • r.y '.. &."". rl rii:.e hyl et r.e r comple x s

4 . V i:; ~o.- i t y 0 f -i i e ~ '.--y l and d i met! yl e her complexe s

/ . :..;- t> ·ifir r-.~:it ·, f · '.':· ·i i r..cthyl c> t ~f' r cor plex

F . O;,e:rat i on o f t ne S tt-d ·-.a:", o l 1J..r:m

I t was f o\..:.11d 7- i':at l .>'Jt ·;:.' .- , ~ r · l ·:di :, r h<, r o n , r- 011l d :)l ..; 1 parat £. d by a cour.t ~ .r ­

c'.lrren t d.b·,il l a t i on >f a -!i..,s0 ·~ i :i. · l• ~ - ::-. 1 • x r-, r po ly:- e r. T h~s novel · e t hod of ::; epara i r.g i so · .) p ., Ii _, · • .:: c f o r · :-: ... bqr on i ") ·,ope s and f ound to be s 1..- c,..essf 1 , wit!-: ar. 0•1 c: !"al l r, ·.e - .:;:~ p ·~ fL ~ i ,· n ~ :· ::; 1_. ff i d ·-· r:;:, l:,· l arge to r:iaK t he 11L' t:iori v c:: ry a : ­~, ra. ,.. : i v 1.. frr.. l'l bot ri a r. n ,- 'i r .. e r ir:r ar. pur 1.ly s c: i t>"". : i f ir po i n t of view. 'l'hi:; nev: :--1t '..o d of :;·: · ; a ·.«:: n "; qu'«· ;'f ... c :-al , 3.!".d i; :-:a t limited i n a11y way t o he bc r on ~~:,....• .. ; ; t~ S .

Th :_, ;. l \-Lod .i::; ~ c •. v 1 -r.: "S·~'' .-,. " · l.e l · r~~ s ca.l ;f)pnra t i on of t he boro n ~=- - ~, Of- s . T· :· pl r.• L ,:; > -. · • · i i.::;r · : !:: l e·.: mplex ( Oi3)20 •BFJ ' which has a s ir' plc ro ~lt; ::; frn · t: r . • ; ,.. "[r" c-r ~ f L.016_: 0 . 002. In o:-de r t o :nnkt: this r.: e t:"-:o<l of :; JAi. r · tir.r ·.!: · '.o r •. L:ct o r - s ; f J' r a.C' • i,. '..importance, it vms necessary t o find a. :r.t:: t ho·! o f n~ov -. r i nf q · nti ~ t i vc ly he ::F3 from th .ompl x, a.nd t his wus dono. The ·1" ri< ~ :-: ". bl::n ru. tn ry ri. b·~ I i . -, h•- r c po r:s, as 1ell ns th · l u r g :; cl ... I v · l '' ! : y. • <. nd app i ' ::i r :0 c. ".'r ~ ! · ·~ t::! .t ,; .. ~ 1 , •

~ ~,... ... s:; f 1l l prli l·:. : · } . . ~ .. ~ l~ • ·. · l • , 1od o f ,j . J..Lrnti o n o f h t i..:; o pc .3 to : .~rg•.

:, ~ 1 1 :·,. :· C' : ,. r. rv:r: ~ :- .rj: ~·c ri. ' '.. '1 !1 '~L ·:, · bl li t ., o f ·;n r i ous ~tmstru . · ti o n r· ".'- t: r i: ". .: ' I •,o t 1• . '. <~pi · / . · 1 0 rh ,. - · • : -i • • • ns i v c p ·oi:: r · r; •m r> rro •; i rm ·· tudi · s . '? l-- r.

! ' ' ... .U. · 3 c. :.., · . !i ·; ni 1 : ·ri ;-- : i'>:I :J f •-h• l . rn1 iq 't S us e , ::.c. r.~ · o f ·.~ hic l. c.n 1 11 · n .. , · :- _ ,.. : ~ ·~ 1 1.:Lii '. !"' tr,. r . ~'O rt : . '..!. t hods of c.nc.l ;1z in,- t " \'0mph .x f o r •• ir. o f ·:- :-.:- i · i · · 0 !., 0 ~ 3 • urly ~:'t · • ;:,_ =- ~- t ·_ of j c· r.pc ::d. t i n:., t. h .. , _i;l:s

~r- • . '. · ., , J · . · ! , 1. " • '. . . ··r · · ; r. · r ~ ·l 1 ~1"' • , 1: : c on t• . phys> 1 :·':"<,f• :· , :;

. . i L .

•· 7 l Or'Jt! R-'J ::i 1

? il c l r10 Pnge 5 7-31-45

mp l ox. a c curate determinati on or the a ( the simple proc~ ~ 3 f r 1ctionati on • ar•.1 discussed in the r epor ~ s . an ·tell n s datn nri c 0 ::; s '.l r:r ~'.)r pr oper rioaign l nnt • . '

·'

This "V'O rk wa. :s und11 r tho dirncti on of Dr::i. R. :1 . Cri 5t ·tn '1 !f . Kil pcltrick. -h t he r (; senrch was rlo no by a. ,r , up working '\ S [ l whol •: , f 0r ~ r .. nv ·_rii c nco .c of opo r 1tion, this gro1Jp wr-_3 divide d intc two s •.Jc ti0ns, ~. •: h0mi c nl

. · h section, nnd nn O "Linc - ~ riniS _,,, c t i on. Th1... C'l rly o ri r, n t i ~.; \.'1rl i r. v" :· ti r;n. ­w Jrk wa.s dono by the ch ,;m.i cnl ·.; ct:i on, but upon th ; "o m 'l l -:. :-. t :'.. '.1 l i ~hri . n t o f -:;_:; in(.; Oring section, t h t! work \r ~i; :ir · po.r ·~ tc ri ir.tn :h·~ r '" lr:h (' l "- ::;i1 ic . t i ·, r.s o f . '1d ·.; nginoc ring r c sor. rch. Aci;U!llly , mwc v._ r, :mm·~ r,f I k . -:•. ;~ lC'~ l -.n r k : .\ S

J :. by the engineering unit, -.. ·i vi e:: v c: r s1 . Tov:--. r d :- ~h ..!:d ~ :· · r._ r ::: -. r ch , thi:: ch1...m~c 'l. l ~roup 7tns diss olve d 'Lnd the ·.1vr k , r.l 'J 3tly purc. l ;r . r. 1~in . r:r i ~. 1-: , ·.1 : :; -, r. -

, tinuod by t ho e ngineering f.: r 0up 'l l 0r.c e Th,. c h,:mic ~ l r ..: -:Jvr.r r. h :.> cr: t:i L1n ·,r . ::. u11d 1, r the supc rvisi '>n o f I. Kirshor.b num, ::.nd ';he cngi 1:~c ri.n;:; :;0c t i :: 1: · .. :~ .. ~ u :--.cL r P. -::. Schutz 1nd N. S:i.bie The oxpcrimcnto. l ::o rk vm s done ·:: i th tho h r.; l p _, f h o f :: ll ·.·riny r onior r osoa.rch chom.i:;ts a.nd onginr.; e r 3 1 G. &.r-.iki ·i t c n , '!'. Cr .:;· :011. J . A. ~·uer,1 il 'ly, · ;, ·11s o.n:;ky• a.nd -:-r. C. Zmnchinsky • . 'l. i d ·Yi by a. sta 1·r c -: . n :~ i3ti ::g ri f T. Bl:·.ir , r: . Boga.:;h, A. Ctir.ir.tin, .-... Forsythe . A. Kivnic k • • Kcpr , s. Lr:vi~ , J. Sh~ dlcnky , ~ . Thornus. nnd J . Urba.n.

10 11 -:hon tho pbnt f or tho scp ,r-. ': i cn o f 3 c.r.d '.:! ri r; v r, lc p0ri J i ' f icul tLs

due t ::: tho l on.kt'l.~e o f v~.tv r i nt··. -.h 0 ~ y t c r:i . Jr . Schutz ~.:. ti ··: . ? ·,r~ythc :J.!1d D. 1'c ·~o.ulny • wo r e onpl oyod by tho '.: '; · .·vl-. rd Oi 1 Cc n p·.!·.y : f I :.<~ i r.r.·. . ··;i th t hiz i ncroo. ne i~ p.) r s . nn .: l• tho v-ri : us d iffic ·.i l : i c:; , f t ho _;:; 1 -.r:t ·::o r •J :; .il v od :.!:J tr.: pb.r~t put i r.tc pr ·.., ducti :in. i: . Sabi "l.nd - ·. ::: . Zr..n~ h.ir. :: ky :-. b r. ::p•, n t: s ·:in r; t inr. r-..t t ho -.hlting r l ::.nt .

The ne cessity f - r -.. 1· i ';i ~-1 ·..:.r. l yt i r; --.l ··· · r~ ..... ::; '; -.k._r. r;:.r r. '. f by t ho t r:i.ns f or of Uc ss r s . Jud :; .1 r. ''..nd rlyr. 1·1 t · "r. ; 3 ~·.: :- r r! i.l ': . r.jYI.j' f Ir.•! it..na..

In ndditi ::m , th ; r r · b l ·,r. r 1.C}US '.l:: .. r-:.t .:-.s •. 1 >c: r . -: r• ;!iF,. 11:-. '.!:; ne; c . ~ -

s i t "..:0 d furthe r stur)L:; ; n r: rr ·; ·: , '1 -:: ·,. : . · i :--., :: -.n·.l :rti .. . 1 c :: .r 1 , 'lnd .m ;ethr;ds f : r t ho r .".)0 '1V'1 1 -:. f·;r t !" e '!' . - ri ·;~ i. · .l:i ::-: ,; ~ - r '.' ::-. i ::; • · r: :--!l iti ·r.n l ;r up, c c n s i3ti ng ) f E. H. 11.yl r • F' . '..Jt · , .r . ;{ - · :. ,r, , •:. ~kJ-1· .... r ... z r.n-1 s . D1.t z, ; tu-Hod the pr opc rti e r. . f th ~ b r ~ "ri : l u ri. : .. h:r r · · - .

In view of tht: p·~ :n i n il.ity i..,~.~ t!-1 . -, ·ci ·L.::t 1 i: ~ · , r : 1"..t i n f :-: r. r .u ry rd t he l ~~k o fr:tc isturc inL ~h . .. l ·. ;,':1 •ich~ h·.·r r .: .J. l t) ' i'1 r.h . 1 :; :; f t; h <' 11.nt. 0. now pl'.lllt \'t'\G dc sig:ltJG r.-:·! r ::; · .. r d . . :·}:: · · · . .'> ~ r.rr i. c; .l •J"':. ~ n :-.),,_ ; :; - ibl c

iso .:· f flu ·Jr >c ri. r b n5 ~:J h 0".t 1}x r;nr.:ng 1. r c. . · · r k -.-r· .r ~.l.; ·· .rri .-: .u t . r. ::;' :bstitut i ng p lo.a~fo rl.ia.phr .-gn f -:. r tho ;:i ~c l •li r.:.-r .r ·.;7~ i n -:.h .. ['..lt•r - . :i.c: ::; -: r e:: ... r ~: r, r.!uc t c J

by L. c . Libo r o.t -. r c 1.nd It o . R ~r.b-. '..: V. ::r •. :·1 ; r: trir. t r ! 1 -.~ tic ~. "'.:l. r i·.:. l .1h i r: h l::· d ,·.n •'..'V ~ 1 0 1 c d .m th :.)r j cct (kn ·:T. l ~P-1 0 ) ·;: r :i q1d :, o' . : i :f ·. c +-. rv , · .r. l t.hr.t -. rb _, n f luoride s c ,ul -J b ::: us 0 ! 1. Z 1-__ t xrh:-.t. ,;~ :-.·::· Ii. r • • ~~·.: ~Ye r , -.:it-. ~ h . :11c c1,,3 s •'th e Jrig in..'"l. l 7l r_"lt , ';hi ::: •l , v,l , _. ~ -- v b-, i:-, '; !.

II. C , nvor si ·. n . t' ::; ...... r · ':• : ·Pr h-.:t"" :: t · lli c :' r r.

C1.r t'. ' .·~ 3 c ~:: l ux -

. ,

• •

.I .

1 oo: '2 -9 .)·t Fil e 1 '3 0 P .• p;c 6 7 - .n-~s

2. St ep II - Pr -:· 1c ri r. f .2Fs fr - r. Cr. F2, J?3 :.: r.r l cx -:rr::n ll s c r. l e

3 . Stv?S I ::-.nd I I - J:. il _ t 11-.n t

4 . rtocov c ry Jf 3

,\ n e t. ~J f : r the p r ·r '.l. r- .ti ~ · . :~ ;:.ur c r y:itc. l lin0 t r -: n .". t r '.'.t r: s f the : r -k r •f 600 gr :'.n:l p•. r 1"'.y ·:1 -i. :: :Lv . l 5·1 ir. th i s 1 -.b~ r. -:: ry. :-c . r ·~·- r t -.: .. r •> « r · puro c r yskl linc bcr . n c :-.r ich<..d i n ·:1 1 it i:; :1._ c ().; .:; ".ry t · -; :-:•: ~ r ->; t;~c f in.'\l <r ·Yluct (r,H3)20• SF3 c f thu i3 ~ t .· :-- i :; ·11r. r -. tL·r: ~ r ". -. n ~ :. - h·. :;-:-.r':i·.G ::-.-.t0 r i ::-. l

::Cl 3 : f he ::-. f ·J r on c r.t i "n -: -i i: r - ~ ; ::: s fr r '-.h _ .~r c ·~r ".ti : r: ·. f L r :1 e A :.icth :d f~ r cnr­r yin.; · u +.his c - nv or ni ; n n:; ~ 1.:-T :) l ; ·! , r.r. ~ C ':'. :- i :;-.s f ':hr c c st -: i'.':; •

1'ho -:: , rk dor.1.! in t h is l ".'..bc r". t r ry .,... t h: fi r :::t t-;1 , s t eps f t h i :; c .. :n-. .; rs i :- n pr '.)cvss ".ns un·lo r tho ii:· )~ti ':l. f .! . Ki l p~':. rick ri.:i-.! c. A. ifu tc his :n. nnd c ~rri·;d. , ut bv .\. D. Kir shonb:lun , J. : •• '-' :i rlr'. , J . 3hcd l cslcy, J. L. i'hc.nns, R. Roi der ".~l R. 3chvnrtz.

B. Conversi on c f BF3 t o BC13 ( St <,? III ) •

1. Conversi -: n i n p'tc ko ri t ube s

2 . Cc. nv c r 3 i :::. n i n stirred '".' 0 3S l s

3, CJnvc r s i -n i:. honb

4 • rtoc uv~ry .f B f r · :1 r ., 3i :lu i... s

. \ n. jJr p".rt . f th ., •)xpcr i.·T~;~ t "'. l .,.,, r k 1 thi :; third stc:, -: f tho , c ... , n ;- ,, ";'m s J. Jno by R. ~{ . Ebe r t .... ~.n'! E. R. Gl ·.:Js u.n :!o r ':.roe · i r ccti n ct

• • ,.r: s :'l r.nd 11. Kil pntr icke The F 11 ·::ing ; c r:; r m:; ('. l :; - I'' ,r"':icip:\tv i in tho wc r ".t V:-Lri JU ... st"!gosi A. J . Fl yre1, ': . 1. Juds r. , E. K.:i. lich,·:r :-. , :~. D, Kirshonbo.un• R. ~ . Sch .. n rtz. J. • Sni th , ~ . D. ~ r . or ~.nd ::; . H. ?urnr, r,

c. Producti on ; f crys to.llino b .::i r ·:m f r 1. n its hn.lid 1,; s.

1. Sunr.o.ry ,; f r ,; !11cti · ::: :;tu li .; s

n. , Srio.ll s co.l ., r e J ue t i n in ·1 hi&}i vo lt~ go 3r o.rk

b. Snnll sc~l c r educti on on f ilcncnts

c . Stla.11 sen l o r educti on in tube s

d . I.Argo nc~l e r oducti cn on r -; ds

c . Plrint r r. •b cti. n 'm r r <is

2. Re c JVury •Jf b ' r .;n

n. • Rcc cvur y r; f 0Cl3 fron cxha.us t :1 5 1.)S

b. Rec -ve ry :·f B f r · n t-mt•· lw r < s

~h- r J so'lrch :Lmc in th i s ;-h::-.sc .- f +-he W>lrk Cvnc 1.; r :t·- ·! -.:hr. le ·r, l nvnt .J f · r c ·- :>~ !' r t; ~e ~ r ::·!uct i r1n f c rys~.llinv b' r cn C; f h i gh t:ur ity ''.n .l ·nith n.:i·u-ly

~ I

lCOi,,t{-~ 31c

Fil e 180 Pncc 7 7- ;H-1i5

complo t e conversion of t h0 ztnr t irlb ~oron cor.:pound o.minati on ;f knovm r e ac: i o n~ f or ~hR Fr du c ti ~n o f tho rea c t ion SX3+ 3 :r;:+ . + 3P.X , ·::he re X i s F, Cl, 2 .

to boron mo~al. .\n initial ex­boron disclosed tnut of them all, !r or I, ·:10ul d bo e xpec ted to

~ ive the p•1rc3t pr oduct because 0:' tlw volntili t y of o.11 r onctants nnd products excepti:+, bo r on .

!'ne equili °'.) rium const'.l •1ts fo r the r o.iuction of BF3 a.nd 3C13 with H2 were computod a!Jp r oxim:i.tu l y f r Jm d:: tn 11v::.il t: 'b l c, in <:hu litcr:iturc. Tho C( mputntiona.l. r os ul ts -confinnc d our 0:x p1l rinc nt'l l -' ::u:ii c:. which showod t ho.t aF3 7IO.S not nnd BC13 wns r e duced by H2 on, or in ~he noi chbor hood of, c s urfo.cv ~t 1,300 to l,soo• K. The computo. tions gave fo r the cquilibrh.an c onstants at 1, soo• K. for BF3 nnd BC1 3, 2 4 10-ll -4 • x nnd 1.3 x 10 ro s poc tiv ly. 1'h0 r e duc t i on of BBr3 with H2 ~~~ f ound to occur nc onsily ns tho.t of ~13, bu t tho brOl'lide w~s less r eadily nvnilnblc .

Expe rimental invost i gnti orui 5ho-~od tho.t under propor conditions the boron proclucod by r educti on of BCl3 w1 th H2 is crystt-.llino nnd or grontor thnn 99 ntom per cont purity. JUso it ·.-ms shown that tho unrc<luccd BCl3 .(tho yields woro o.lwnys leas tho.n 80 per cont) nnd t ho B c ombinud with tho hot surfaco c ould o.lHnys be r o ­COTerod na a:l3 o.nd r c \U cd, r osultinr, in "rcry smnll l oss of 'n. App:u-ctus t'r.l.S dc­rlsod f or tho oonmorcinl producti0n of GOO grams 1)r more of ·B por 1ny. A pilot plant f or carrying out this pr oc os s , .. ,~. s c 0nstructcd n.nd opera.tad .

Tho oxporimcnt:i.l w_rk 'tr. :; c~rrh. d out under tho diroction of M. Kilpa.triclc a.nd c. A. Hutchison, by J. s. Jmith , R. s. Scln-~.rtz, E. K.nlic~~:ll'l. J. L. Thomo.a, a.nd R. Re ider.

D. An inv0ntigatbn of ri l t c rnnto r.10th0ds f c.; r r oducti :m of bor on C'"'mpoundG

1. Tho pr0pa.rnti 0n o f bor on by tho r oductif> n of bor 0n tri­fluorido with s odiun. .

1\

n . The ~ tch s '- i:!ii..l!il mcthL d :ind o'.lTly o:xporilllenta

b. ~th ) d:; invol Ying th:, sioul truioc us \~troducti ~n ot s.vdium -u:d b r : n t rif lu0ridc \'

'I. 28 The pr op'll"'l.tLn ·v f t .. r o.J n b ·; tho r oducti.:)1i f s odiUZ!l

fl uo b.or n t c '.7i th s _ ri i un. · ' . .

3. Ex t r r.cti on of s c)dium fluvridc by \Tet e r fi'om tho r o'.lction pr e ducts

1 . Prepnr~ti )n c f bor on by the . r~duction 0£ boron t rifluoride '\nd S'.) diur.i fluob Jra.to with o.lumim&:l

s. Prepul;"'. tic n of bor on by the roducti on ~r boric a.nhydrido with CUJtivo ~o ~'l.ls

6. Tho high torapor~ti trc purit1cati 1.-n a.nd oonlrnlidc..ti on of 'lr.lOrphoun bor m

It 7'0..S tho object o f this r l.s.::nroh progrru:i to dovolop n oho.'llic"l nuthod tor the rroducti ,in ~ f bor on of high purity. Ini ticilly, tho objcc t 17o wn.s to pre duce boron oi thor aoorphous or ot.herwiso of a.t lc:.st 95 a.t0a por cont purity. ta.tar this ..to.a rovised to consolidatod or crysto.llino b cr <.in .J f 99 por c ont purity. ·:i. rk vrns directed t owa.rd achieving this gcnl by trio motho<l3 1 (1) A trro-stcgo pr r..; 00ss

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' I

1000R•9M File 180 P\ge a 7•31-45

v1hornin nnorphous boron ·.ms first propa.rod by some simple, diroot choi:donl method thnt wns t hen f ollowo1 by n purificntion nnd/or conaolida.tion. troo.tccnt o.t n higJi tom~ra.turo. (2) A singlo-stngo process whorein oryatnlling boron or conaolichted boron of high purity wa.a pre pa.red directly by tho lntora.ction ot troo-.aodiw:a wi tJi bor on t rifluoride nt high tcoperfl.turo.

Pril:lnry cnphnsis wns pla.cod on tho toohniquo ot propa.ri~ boron ro.thar tha.n m tho c onprohonsivo study of tho purity of tho product• obta.inod or their r oc 0vory. This Wfl.s pa.rticula.rly ovidont in co.sea imOlrlng tho use ot aodbn, where the hnncUing of tho mnt orio.ls and tho typo ot oqui?30nt uacd provod to be tho Gr 0~tost pr oblco.

This invos tig;ntbn did n0 t yie ld suitnblo positi<ro r esult•• The dittt• cul t i cs encountered with oquipnont o.nd hnndling ot mtorinla prosontod obata.oloa th~t w~ul1 ha.vo nocessita. tod ~ l ong•torr.i r osoa.rch.

This work wns do ne u.'ldor tho gonornl direction ot • lllp~trict, J. Se S~evack end A. Kur~•• a.ssistod by H. H. Stnrko, T. Cla.rke1 Ge Cohen, S. Fode~ M. Hruiig, M. TetenbnUr.l ruid R. UlL"XUle

III. Annlytionl Methods ' '

Spoctrooetric .\nalysia ; '

., .\. honvy meto.l CC..83 11 poc tronotcr wna usod f or tho first "1ork on tho isotoiio o.no.lysis. This instl"uno!"lt w~~ uaod to get the nocessnry .t\mdm:liOnto.1 ro• sults fr.or:i ~hioh n oor o sinplo sntisfnotory r cutine i:w.ohine could bo doaignod •

:.ttcr tho ba.s io -mr.lysis nc th0d h-i.rl boon f ound, o. speoi~ inatruccnt we.a constructed which lmS then u~cd f or r 'utinc ~lysis of slO nnd all compoaitiona. Following the conpl e tion of t his i natrut1vnt. ci. second co.chine for r outine plo.nt C ~ntr o l WO.S f ound neCCSS'l.ry r._nd C)n s truc tcd ~C C O Tdingly. <

This nork Ytns unrlcr the ,.cncn.l 1 ir ·..:c tion cf M. G. Inghrru:i nnd J. s. Soi th , ('.Ssistod by ..... a. Sch-:r .b. • Y. Bc-.r t h.:- l T CW '.Ultl H. Groonborg.

B. Chccic". l .\nn.lysi3

Invcs tignti ·Jns ·:ro ro 0Clrric1 cut .. m the f' ul bwing subjocts 1

11. .\n..'l.lysis ;f pure cryat n. llinu bo r on

"I De orninr. ~i • n ;:; f' silic; n :".nd irL' n in bor on .... . 3·. ,-_n'.'l lysis of b ·r .·n triQhlori do

4. .~nnl ys is ;; f bnr on r luori c -mothyl & thor complex

s. C n ::; tituont 'i.mlysis Jf bor on fluori~e-nothyl ethor C<Dplo:

6 . · .'.n.'.l.lyn i s J f ox i t c;a.s os fr on bor on trichlorido roduction ·

7 . .'Ul!'.lysis ;;,f cu!"l::: ti tuonts a.nd inpuri tios in boron tl"ichlorid

a. c ~np lcte n.nnlysis of bor on

Tho g1..: ncra.l o.no.lytic 'i. l t-·nblc.:ns o f this project T10ro invostigo.tod by n gr ur c _op ::>s od ,. f • !J • • Judson, c. D. Turner• r; . H. Tumor, .\. J. Flynn, J. Ae V')nn, :~. D. lir sh·.mbcun -:.ml :i . Kurp~ . ,'

t

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~. Liat ot leporta

lOOUR-934 Filo 100 7-31-15 P:.;e 9

I. Reporta C!! Separation of lbron Isotopes

A. REPORTS

nrshenba\la, I. " "

Monthly Report, 5-15-43 Bibliogi-aphy, The Chemistry of BP'3, 6•19-43 Chemical &nd Physical Properties, 7-2-43

A•,705 A• 734 •• 742 A•l278 !&plan, I., Cohen,l.P. The Approach to F.quilibrium of a Countercurrent

Cohan or a Square Cascade with Material .fho!e Mole Fraction Ia Not Small, G-1-44

A•2120 11.rshenbaua, I., Sabi, 1., Schutz, P.:!'. The Separation of the Boron Isotopes, 9•30-14

.\•2192 Taylor, E.H. Chanrlstry o f !P3 •2H2o, 9-1-45

K RIPORTS • BI-ft'EEXLY

2a-229 lirshenbe.tua, I. 6•21-43 l-l-422 So.bi, N. 3- 1-44 21-659 Sohuts, P.i:T. 8-19-43 lf-424 II 3-20-44 21-705 Schuts, P., ;f-426 II 4- 7-41

Kirshenbawa, I. 9- 4-43 !4-428 " 4-19-44 2R•'7Sl Schutz, P .w. 9•15-43 U-130 II s- 1-14 11- 400 lirshenbaum, I., ll-901 " 5•19-11

Gilbertson, L.I., M-905 " 6• 3-41 Sehut1, P."J • 9-24-·t3 J-907 " 6•20- ·~4

!f• 401 Sohutz, P.i:r., ~{-~09 II 7- 8-l4

Iirshenbll.Ul!1 , r. 10- -1-43 ~-'.1 17 II u.nd

K• 403 Schutz, P .rr., .Kirshonbo.um, I. 9- 7-14 Iirshenbaum, I. 10-20- 43

M- 408 Schutz, P .rr.' Iirshenbaum, r. 11- 9-43

)(- 400 Schutz, P,"!., Iirshenbaum, r. 11-26- ~3

K• 410 Schutz, P.'"'., Iir shenbo.wn , I. 12-20- 43

K• 414 Schutz, P.~!.,

Iirshenbawn, I. 1- 8 - 44 K• 416 Schutz, P,'.f.,

Kirshenbaum, r. 1-22 - -14 K• 418 Schut1, P.'1'.,

lirshenbaum, I. 2- 7-44 K• 420 Schutz, P •. :.,

lirshenb.1um, I. 2-21-H

\

..

. (

2R· 2 rarsher.hnu..,, I.

2R· G2 Crist, ·· .• 11., ~

. 1• 412 Kirs~en'XllL~, I.

r.i- 427 ~11.bi, :~ .

lOOlr~ - <; )4 :·nc i : .. o 1- 3:.- 4 :) ?c. rre 10

rr~· ct to L \.i.o l F ... ctor ;'o:-- "[:')' 1- · -4.J

Proercss - ~ A -:; r ':. , J-1,-4)

Corrosion of Sted::a..., Pnc}~ing, 1,-ll-l..4

i'.• 90) ~c: · utz, P •• , Zoo.chinS: .:1 1 Liq '. id Dbtr:iJJUtio"l ~ ~terl an PLC: fr ,· , 5•19-44 ' .c.

/.-"t-174 :<:aplan, I. The Design of t he VitAu ... in J Caacaoe, 6• . ...,•L:4

io- 910 Sc)'lu~z , P .' • , · •t".Cci·insJc./ ~ . • L.

:;. 911 !:.abi, ;· .

d• 91J Sabi, P•

: i• 914 ~:.ia<.: .·ins , I . ...,.

;J- 915 Sabi, : ·•

/iil-190 LetkO't11 tz, J' •

:J-llBJ Zmch.1.ns .• ' , • "" •

i.;.:-192 l(aplan, I.

. 1-11£5 Theort;tica l Group

. .-l.1L7 Lib<".rtito··n, L.c., 1css0C.ch, ~..: .~ •

. -UU, Libc.""atorc: , L.c;.

. :- U.OJ Zn:.chins1 ~, r . c; .

-U.04 H·itc: i~o~, ~.A., ·r~o: as,

J .L. i-ll,05 Kirs:.e11:"au; ·, I.

L.1.c uid Distrihution throua1 : ~tecir ·an Pt-c ' ~ - [ ;.ro. ), 7-10-LJ. Test of ~:·a ~in :~ "':ff i cicnc:•, , -'?..-1.4

Conductivit~ · of Pol:1;·,c.?"- · at~r . iY' ... ..ir s. Dotcr. .1.1:t1011 or · nt .. r ~., Pol: 1 er, f. -10-IJA

Conputo.tio.,,s, 10-1"!-44

TL a of' , 'PJ"O- cl\ to F.quilibrium in a Coluan, 10-2)-1.4 Liquid i> i s ~r 5 ·T. ti v11 "':. : U'OU._3.~ ~te\!J-a:~ P:- c i · .,; , 10·23-44 F.quilibrilll'l Tir ~e ··::;r Vi tuni. '. 9 CA>.sc;. ~u s, 10-24-44

Effect ilf r.~r ot1 t .:a Co; ,ilcx, 10-Zl -/J+

Equili' r~_u;n T .. c , lC-JO·/~

~tatill:ltion Curroa to: Samples of C-714 and c-sir., u-22-LJ+

Corrosion of . :o!'".ol Sera 1n i.n Jar1pi.es u_" J.ant Co1 ~ :-.:i.ex , 12-.J>-.l:4

Conv :::r 3io~1 o :.~ l 3003 to mi' J' 1·5·1~5

A ~ c.ud:• c' Sor:ie o ~ t:1c p ;"trsicr.l ?.nC (. ~ c1>1ico.l Pr o;..>trties of Con~lox, l•Jl-45 ...., ,

...

.. ·'

. (

W-1406 Libera to:-c. , L. C..

'3-UD7 Sabi, r..

Li-ll.08 lachin~. ' .• c.

Supplericnt to U-1407 Sabi, '•

lOOUR-')JI~ File 1(-0 'l•)l-45 Page 11

Diaphrn:~1 Punp l nvestic:ation, 1·2'-45

:-:t'tect or i·!atcr on Fractionation and Decui::. ;v... ~ ition

ot r.90, 1·)1•45 Salt•. ettine !>tedmn Pecking, 2-11~·45

Fractionation at LcJt, Reflux Rate•, 2·24 •1.5

II. Reper'.;,:! on Conetoion oi ~ewat!d Prodµct t.o :lct.allic r3oron

4•1246 S~clc, J.s., lurta, ,"...N.An Investication of the P.ropnnation of 1oron b)­P.eaction of :1oron C~JOUnda :it~ i:et&l•, 5•25-44

•-1247 St&l"ke, H.li.

4-1268 Hutchiaon, c.J..., Ssaith, J .~.

•-1298 llutc!l!SOTI 1 (.;•"•I Saith, J.it..

A•2lD8 Hutchiaon, C. il ., Saith, J.~.

A-2121 Xirahcn ')au-1, j, • i) •I liu~ls:m, r; .1 ....

1-2122 Huto i so;,, <: .: .• , i.:=t.a, ~ '.J .

A-212.3 Hutc.:dson, .... ""·ft.

a-658 Gilbc.rtson, L.I. a-691 GU '>ort90n, L.I. a-743 Gilbertaor. , . .: .I. ~ Gil~tao. 1. L.I. lW04 Gil" iartson, L. I. ~ Hutcr.i~o;i , C.A.,

~pavaclc, J .s. JJ-1111 Hntct.iRor., c.A..,

Spevac!<, J .!J.,

!~ i3t:~•, a. H.

tchi3011• :.:. .J.. •I Xurts, A e f! • .

star:ce, E.ll. :.J-411 llutc!iiaon, C.A ••

Spowack, J .s., Stcir?cu, H.H.

~) llutchiaon, C.A., &pnack, J .:>. Starke, H.H.

Attempt• to Con8011date J.oorp~• Boron, .3•10-44

Thcr..'10d~·Nni.ca ot Product~ on or '!Joron i ·et.al b:' f1e­duction Of ;]Oron f\EAli,1oa1 5•29-l.4

Reseurcl ~ on ~ · et.hod:• or P...oouct~O 'l o ~~ t,;J,:·stallino Boron o! i!i?h rurit:· frOT· ·00r<>"u .~H~.os, C•lD-44

~uwlenent to A-1266, T" ::. .--:··odynai.; .. ica of t.ho T',e• duction ot CertaL, Hal!.dea, ~-10-44

Conversion of (afJ)20•il'J to 11'3

, ::itcps I t.nd II) ll-JJ-44

Cr.nv~~sion of ~J to BCl) (Stop III), 1·25-1~5

Pilot Pla:1t <.;onvcrsion of (Q!3)20•W .3 to Cr,,rstal• line Joron, ll•l0-44

~-19-4) J-41.5 t:utchison, G.A., 9- 1-43 Spew.ck, J .s. 1-229'4 9-20-1.,3 ?J-417 l~Ltchi80n1 C.A. 2- 7-44

10- 5-43 rw.i9 flutchison, ~.A. 2-21-44 10-21-43 1.t-421 Hutchison, c.A. 3- 4-44

lloo.42l Hutohimn, c.A.,~abi,lf. 3·20-44 u- 9-43 iJ-425 Butchiaon, c.A.,!)abi,N. 4- 7-44

iJ.429 Hutch18on, C.A. 4-19-·'J• !l-900

ll-26-4J U-902 Hutchaon, C.A. s-.~4 llutchi.on, C.A. 5-19-44

· ~-904 u Butchllon, c.~ 6- '.J-U.. :J-9()6 Hutchiaon, ~.A. 6-20-44

12- 9-43 lJ-900 1:utchiaon, t;.A. 7· S•IJ. 1~912 IJ-916

Hutchison, C.A., n..M a- 2-44 Hutchiso.,, c.1 •• 9- '7-44

12-20-43

1- 8-'4

I

•' ,,

(

il-1400 llutchiaon, .;.A., lt4-rshcnbAun, .a. .o.

il-1409 llutchison, ;;.A.

100lr.{-9J4 File 14:;c. 7·)1.-45 Pa~ 12

Pr~t1on or ~] ~J_. _ (CJt3)2'>·m', to uhich r.at.er Hu ~- J.ddod, 12-2S-44

Doten· inatJ.on or I110topic J.bundanco Ratio in !Uomental D

III. Report• OD ArpbtiaJ. t4ythpda

4 RJJ>O:£Ii

A-121.0 Jud so, , c. :1.

A-1266 Judso~, c.1 ;.

A•l.2!>7 Judaon, l; . ; •

A-1299 Judoon , • 1 · '"• ···•,

c.n.

A-2155 J udso:i, ' v. •

.'1 -2156 Judeon, c •. •

A•::'lS7 Judson, c ...•

A-2150 J udson; ... . ...,, • 1 . •

;..-)257 Ingt:ra; I .• G., R. ; '•' Hester, Scin~u~ , · . • G.

W R.:}>Qjg'S

T1U-l"er,

i t:.Stud 1

c.11.,

I>eterriination o! ~1ilicon <:incl Iron in :Joron, S•l-44

Ana~vsia ot ;oron Tr).chlol•ide, 5-1•44

;.na~aia ot ~ !1.uorido-Ucteyl '"'the•· Goi i!>lux, 7-21-44

Consti tuAnt J..li.al:·sta or 'Wren l'luorido-: {et!~l ~t~r Counlox, ll-15•44

11110.l.ysis of .:dt Guoca -"'rota Boro!1 T:!chlori<!e Rcductio11, ll-"1-44

f..na.lysis o~· Co~titl1cnts Md lT'lpUl'iti1..o ln 1oron ~richlor:!.dc , 11-JO-J.4

llO ~ :L: ~s .>pcctronetei; 3•21-45

.~- 918 Sraith, J • ., ., forstat,H. Analysis of <.ic:s .1aoplc, T0\1 ::ir 8, 9•18-M

INl'l' l.\L ~7P01~T • CO?fJ}AC'f NO, \' • 741!!-eng• 41 Dccnmber 2, 191~.3

b

On l!ovorr.ber b i, 1C/1}3, t ho Standa.1.d Oil Company (IntUnna) i .,::3 '\";as approached by Brig . G ~n • !Jt "R. , Grov s of t he 0. S. ~rrrry Gorps of F.ngineer s ae to its willingness to undertako the manufacture of a small ll!nount of a critical chemical . On November 22 , 1943 :;;r. E . ' . ThielG of he f tandard tiil Ccmpany visi tod the r .. ~dlaon Square Area Office of the ~nhattan District to diHcuss the tech-nical aspects of t e proposed p oj ect . By letter of Nov·~ u:b ; r 24, 1943 fro~ Ur . E. G. Seuber t to Gen . Groves, Standard il Company indicated its~reemcnt to proceed with the design , const~.1ction and operat1on of the necessary f acilities, provitled a auitabla contract were developed to provide for the reimbursement of t~• e cost of construct ion and opara tion or the f acilities . On Dec<'wb~:ir 2, 1943, the u. s. F.nzineers Office issued a l_tt~= of intent covering the propt1sed projeot and on December 6 , 1943 this letter of intent 1'.'SS acceptod by Standard . Subsequently , on Januar-y 5, 1944 the parties entered into Contract No . 7418- eri g-41 dated Deconber 2, 1943, covering the proj ect .

The objective of t.~e project is the erection and operation of facilitfoo to produce "B" units per day of "X" pro Juct (letters "B" and 1'X11 are defined in the nsecret l etter" anted December 2, 191+.3) , Hereina.fte" and in subsoquent reports "B" will be considered to be 1. 7 gallons (U . S ,) and nxtt will be callod "Uoavy Polymer , " Hea·vy polymer is to be fractionated from "Polymer " v:hich is produced by tha reaction of "Synthans" vJith 11!.Ionomer . tt

The sto;.1s contempllkd £or the execution of the contract obligations and the originally o:xpectod completion dates for each step are indicated in t . e following t abula t ions

1 .

2.

4.

5.

Descri(?tion

Deaicm of Pilot Flant Facilities

Preparation of Pilot ?l ant ~ itc a.nd Installation of Of fices and Laboratory

Erection of Pilot Plant Facilities

Start up 0£ >ilot Plnnt, :. sta~lish.~2nt of F.qnilihrium, and Pr0(1uction of Initial Product

OpQra t ion of : aoiliti~s

Scheduled Completion f)a te

Feb. 1 , 1944

April 30, 1941~

June 2, 1944

,

It is to be undorstood that the a1'ove schedule is contingent upon Standard 's obtaining deliv~ry at the nocesoary times of 1raterials and suppli3,, . It is also to bo understood that 2 tanda ... d does not zu,erantee tht:-.t pl.1 or:uction of hoavy polymer can he started by the indicated ' date (June 2, 1944) J howev::ir , c fondal'd \.ill use its best efforts to do so .

In addition to the above <;ork n0ccssary to tha oxoc:..:.tlon of tha Contract, Standard expects to und3rtake vrork directed towards incraasing the certainty or the early success of t~c proposed projBot . It~ris of major iJ!lpor t.ance in this categorJ follov::

1 . Investigati on of performance of high .efficiency fractiona t ion colur:ms, particularly Stedman columns .

2 . Investigation of the properties of polymer. includingt

a . Helative volatility of light and heavy pol.imer

b . Corrosion c . Decompositi on d . Infl ammability e . Toxicity

.3 . Training o.f technical personnel

4. Training of non- technical personnel

5. L.stablishm:c.mt of an adequate 3ec11,:•ity system from the standpoints of fire protection, espionage , and sabotage .

·. or1: on the above items is of a continuine nature and no schedule fa

being established in advance .

lf-9- 23-47

/ s / J. K • . iobo ts J. K. non;;: ,rs

I.D;i CG 1

- .. -2--

lHJI'fT-'I) STAT1'S ;~ j(;nr 7 H OI<'FICE MANITATTi\11 Dl~>'l'FICT

Chica ,.o .\reo. Of'fice ?. o. nox 6140-A

mnc \GO so, ILLnr: IS

4 Jo.nuar'/ 1944

Uemorandum To: The Piles .

Subjects Contract No . ~."•7418 eng-41 v;ith the .Ctandard Oil Company of Indiana .

1 . The work being undertaken is the separation c)f isotope Boron 10 from Doron J.l . The light component is desired at 95% purity. Boron tri-fluorid will be the basic material . Thie ce.n be procured as a com-ponent . Doron tri-fluori e and nethyl other 1'1ill i'orn.1 a complex 1 hioh boils at ahout 200oC . It bas been determined thut the lleht complex haa a dif.f erAnt vapor pressure than the heavy complex and will boi l off at a sliehtly lower temperature . It is believed that the sepa:itatlon can be obtained by distillation. The Job is var; difficult , howevor; ecause

..... ~ ' : . .,J ~J

the difference of volatility is hout one pa r t i L a thousand. It is con­tar:1plated that fractionating quipment consisting of al.~out a thousand theoretical plates l'7ill e used and that the equipment \70Uld oporate at about a thou­sand to one reflux ratio,,-. Boron tri• fluoride and , t.hyl othor a:re both !~ases but the complex is liquid . 'l'he .uipmAnt. as contemplated will con­sist of nine columns 35 feet high . The first three will cons~ of thi rteen (}• triangles, the second three of five 6" triangles , and third' three of 6n dirunetGr tubes . The chemical engineering job concerned is to get the holtlup aa low as possible and slso prevent c.ecomposi t.ion of the com-plex . This latter will not only ruin production but also oause corrotiion of the diatillating columns . To decrease corrosion, monel packing will be used . The components uill be deL~v red as eases and it is e..xpccted that these will be formed in the complex at the oita . This acheme has been t1orkod out at Columbia and no difficulty is xpeoted in effecting the for-mation ofthe complex •

. 2 . The basic r.or k for this method of aaparatlng boron isotopes has presumably been done at Columbia . Drs . Urey and Kilpatrick re the con­tacts or the Si..ttndard Oil people . Technical in£or1!lr"ltion f or thA start of desi .,n has been obtainod in llew York by Dr . Thiele and !r. Conn from Ruhoff, Kilpat1·1ck, and Urey .

J . Sp ,cifications call for the production of l . ? ,,,allons per r ay ot complex 95% pure . This will prod.llce in the order of 600 grams per tay of the desi red componont .. It ia planned that the plant will be completed biJ 30 pr11 and t' at the start up of operations Jill be 2 June 1941H

4. Standard Oil will operate under a prir.io contract callinC'> or the design construction and operation of t , ~ pilr.Jt plant 1U11 t to aff' ct t'1is

Subject : Contrnct No . · - 7/,.111 ong- 1+1 •:;i t h the Standard tl i.l CoL"lpany of Indiana.

separation. Standard Oil is in +.he process o subcontracting th purchase or fabricat ion of t; e e tnipmcmt and erection of the entiro plant to the Foster-~ heele:r ,ompany. This Company has had exp ~irience in the l'sbri­cation of Stedr.an columns t1hioh will be usod in the pilot plant .

5. At the present moment , tha work is orGtinized along the ollmring linos:

! • G. f oubert - President - Standard Oil Company ( Ind . )

J . K. ~toberts , Director of Research

R. c. Gunnes , Project fnpervisor

Ar thur H, Conn - Operat5.ons ' Supervis2r

I Toehnical !.!en (about 7)

Operators, etc (about 25)

James i.1ather - Job Enzinear

E. ~ . Thi l e - Project Consul tant

Vm . L . ;'c:>b - . <lminlstrative Assistant

thfo line

M. G. ?aulus - Vice Pr·1sidont - t!anu.facturing

S. A. .'.!ontgor-.ecy ' tanagor · hi ting :lef'inery

--- ' .

Subject: Con7,ra,~t No . ·-741 ~- 8n,,-/~l ·dth Standard •Jil Company of Indfa!'a

4th '.· rapper Inrl .

U.S. ·•ngineer Off ic ,, Chicn1Jo Ar,.,a, Chlc·t~;o, Illiiv· is . 26 Octobet' 1945 . To: The nistrict ~ngineer, "tanhatto.n 11.ls ' rict, ('ak f. i rler• , 'l'enn ··:rneg Att t

Captain ·= . '.". Teeter

l . The informo tion transmi. ttnd hqrewi th ts .f·trnished in compliance ;··i th Jrd r rapper Ind . Thia inform, tion has hoen obtained through personal contact v1 ith parties interested in tho early history of the contrar't , prin­cipal ly Drs . H. C. Urey and Martin Kil patrick , and is not substant iat ed by docuoenta in the filos of the Chicago 'rea Office . I t is suggested that informati on be rAquestod of the Col UI!'lbia Area F.ngineer .

2 . Dr . H. C. Urey, of Col umbis UnivPrai ty , 1as aware of the pot ential val uo of the separation of the boron isotopos and undert ook a res ·~arch pr o­~ral'l to offoct such a separation. Dr . 1.1artin Kil patrick supervised t he <level opr:tent program for Dr . Urey . ' hen sufficient data had beon socumulat.ed to indicate the feasibi lity of such tt proeram, and · hen a requirement for one of the isotop9s had boen submitted from Los Alamos , the Fast~8n Kodak Company of Rochest ··,r , New York , a firm •"3ngaged in the pr e!Jaration of fine cher.ii cnls , was anproached '9ith a r n uest to design , construct, and operate a plant capable of produci ng the desired fractionation . Thia concern declined to ont er into a contract with tho _, overnment for this purpose .

J . On 19 llov0mber l 'J43 , i.1aj or General L. '.{. Groves and Dr • . ~. R. Compton proposed to Mr . • G. Subert , Pr9 ident of the Standard Oil Company (Ind . ), that his firm undert~ke an undisc losed project or ereat importano •

4 . The standar d Oil Company is a firm with a reputati on for compe­tency and effic iency in r efinery operations , principal of ~ ich is that of precise distil lation . Certnin members of the research staff , particularly noberts , Qunness , and Thi ele , were Y•ell- knoT+"ll to the research org{\niza tion at Col umbia Univarsi ty and wore comiidered by th ts staf f to be par ticularly capabl e to engage in tmoh \~ork . Ur . Thi.al e had been proviousl y employed on the DfM Project on a 1 ave of abeene granted by The Str~nnard 011 Company . On 22 November 1943 , Ur . Thiolo ~as Gent to New York o ~onfor ~ith Messrs .

~ray and Kilpatrick , and the nature of t'e proposed activity was disclosed ~ he desired.. separation , and on 24 Nov .,!!lb ,r 1')4.J , Mr. Subert informed Genera im . He reported to Mr . Subert t hat the 8tandard Oil Company could accompli

~roves thnt the Stand rd Oil Company (Ind . ) was willing to enter into a con tract for such services .

5. On 4 Doc 'mber 194.3, Hajor Harold Grnenstein presented to the Stand­ard Oil Company (Ind . ) a letter- contract datod 2 D c mber 1943 . The Chicago \rna Off :tee ms asked to r ,,ndar administrative t:i ~rvioes such ss priori t.y assistRnco and certification or 1 f ,nm nt r quo<Jts, fer the ftandard Oil Com­pany . On 19 January 191'4 , the Ar ,a Bngineor, :mdison Square .\rea , transferred

;; . ,,

T~-O/ho/1£-9•23·47 Subjec t : Contract No . - '7/,,1' Ol''!j-/~l with 0tandsrd 1,il Comp'.lny of Inri iana

26 Octob r 1945

to the Chicago 1il'ea Office, the entire rospc·nsibility i'or t he admini tration of the contract. The orieinal stimata of' the cost of the contract was 3901 0001 rihioh estimate waa raised to ~600,000 prior to the execution of the in­s t rument . The contract was later supplomented to provide additional .funds so that the total value of t.he oontraot is now ."'2,soo,000 . The contract was negotiatod on tha baais of cost. The cost is determined as the actual expen­diture for this facility , plua opera+ing costs , labor anrl overhead . The over• h(',ad is calculated as 10(),l ot labor, labor being construed to include only operating personnel and not oervioe and maintenance . This calculation is based on the precedent established y previou contract bet~een the OSRD and the Standard Oil Company (Ind , )o The principal item of cost wae the design and conatruction of the faoili ty . This l:as p0rl'ormed nder a subcontract by the Foster \';healer Corporation of New York, Ucw York . 'l'he construction cost is estimated to be ~1,225,CX>O .

For the ~rea Engineers

1 Incl . a M/C

T. S. CHAPMAN , Cl\ptain, Corpse£ Engineers,

Assistant

\

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<. •

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Thi ::; ~OC!J:OOr. t •_•r;:<,' ''.

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1'53

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l.i.:: :: ted.1ian co.i.Ulirta- .tor lh:i.~ project .

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Jn tLe event · i • ·•

that. therQ .. is a re:~'iire~1mt cmly tor a .:?pecific quantity of" t.nis t!K~el'i~i,. _

1t..s u.r:d.que. nuclea:t p.roporti~ :nak~ it. useful for ot.tel' µ··rpos•~ ~'.1.i.cli r:Jti.1

jw;t1.fy th.e cper&.tio.n of tlv~ . plzmt ·. tor ~dd.itional '{uant.ltl6$ • . OM· of t.he .

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d-atecting i nstr uml!t.nts . ,,1r1)ady', U..!.o.n:.tories wn:t.ch have learned of t he

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tor: suoh u pllrp,~ee . A· relatt~ly tJ.U;,ill po:·tion of th~ production i~

stif.f1.c:1en.t to sat!~fy; t..'leue ~s ~ l · litr· ' ' •, ."·: ~

is" axtreiLely corro•4.~1 : it is· I;• r~obz~ble . ' . . .

no w,evor J 3ioce t.he proc41.;i~ . ~l'c.tertai ,"' . ~ : .

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th& t; a. prolonged period &t ·idleoae3.'' I ·,, :~ .(

It is doubtful ·t ha t. it. 'i'fill "Ver tie · · .! ' ).~' "''.· . . . ) .\_;~" · ~ ·,__... .. .

economicully feasible to · o~rfa.te . this !~lant or a.not.her f or t.bfi ~ol:& purpose • . ' . . . ',,· 'J

· ot oper a t tone . '

in ~ddition to potantial oiler~tions util.iz.ing the

~thic.h it -W6.S de.signed,, . tlie pl.ant.. re_pf-e 3en t.1S a .e9mplete1.y a;tt(}\J..~ing·;· . .. ' ...

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l ent for practicu prod.uction J)urpo~ea, it is a ~er.v vai~.u.bl~ ln.a,,.rmx:e.n\' • ! ,' . ~ • ' I .,_; . • '

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TfC/ VF/ lf-9-22-47

I 29 April 1944

Subj ect ; Vitamin.

Tos Dr . J . -a . 0ppcnheimar, P . o. Dex 1663, Santa Fe, New Mexico .

1 . Confirrd.ng telepho~ conversat ion between Dr . Oppenheimer and Captain Chapman of t his office of 2j April 1944 and t eletype of 29 April 1944, the immediate status of t he vitamin proj ect i s submitted tor your information.

2 . · Tho vitamin facility under construction and to be operated by the Standard Oil Company (Indiana) consists ot lS r:lonal metal towers filled with Steadman Packing . In detail, th re ar e J - 6" cylindrical tOW9f'S and J - 12" hexagonal tower s and J .. 18" hexagonal towers . The design capacity of t he equipr.ont i such as to provide 600 grams or Boron par day in the for m of tho t ri- f'luoride dim.ethyl ether complex ano:.1 of 95% nlO isotopic concent ration . Initial dclive17 data a.a apeciried b;r t he contract was 2 Juna 1944 but due t o diffioulties in obtaining monal metal, this initial delivery date had been changed to 3 July 191+4.

3. Del ivery of LJonel metal mlD later t han in accordance with the established schedule . 'i'hen it was received, it was f owid t o be in an un­suitable form due t o oale and irregular surf oes s nd !urthar delay waa incurred in prepar ing the plate for fabrication . As a resul t of t hese de­lays , the completion dates of t he f abricated sections or the hexagonal tol1ers have been placed t around 60 days :Crom 8 ?.!ay 1944. There ar e tT10 authentic but conflicting otat ern nts with r egard t o the dat e on which the sections can be completed. 'l'!le exact delay cnn not be determined at this t ime . Efforts are being nade t o plac part of the t ov1er machining in other shops in order t o expedi te f inal complet i on date ,.,f the nt i ro f acili ty .

4 . t he cylindrical columns , due to dosign and ize offer smal ler iiaohining problellllJ nd are oxpoctf)d t o be complete not much later than schedul e . By roschadul ing the hoxagonal colut111s , it .s anticipat ed t ha t at l east 2 of the 12" columns can ha completed . rior t o the completion of the 3 -6" columns . Preli M ry ngineering studies have 1.ndic :.:ted that wi t h t hese 5 colw:ms a production ta approximat ely 7lJI, of th'3 contr acted ra t e _nd of specif i cati on concont~ation can be atta ined . The contractor has been instructed t o proceed with t ho fabrica ion and er ection on a schedule '11hieh 1'111 allow t he ini tial production date to be ".la.l ized at this reduced r nt e . ·:ixpoditing and compl ion of tho ~ntire aci l lty will be oontinucd with no di rnunition of i.ntcns1ty.

I I::·

£ubject : Vitamin

5. The Chicago Office has '1e n lnfor':"1ed inforrxllly an 1 unofficially that a redetermination of alpha sllovrs the µred· ction that t' ·· is facility 111 ba able to produce the BlO complex t a rate · re~tly in oxcees of

that specified in the contract. It is, therefore , Alieved that any loss in aeoumula+.ive production sustained by t his reduced operation can be re­ca:lned in a short period of time aft .... ,r the en ti-re f a.cili ty ie compl eted and in operv tion .

6. It i s contemplated t hat dolivery of the complex wil l be initiated t a rate of lt50 ~rams a day Jased u on alO content on J July . This ma­

terial 'vill be delivered to the Madison Sriuare Area for r educti on t o the crystal line material 1n a ncil ity under the supervision c· f that oftice .

For the Area Engi neer:

\

T . S . CHA.Pf.!A!l , Captain, Corps of 'Engineers ,

Assistant •

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Speoif1o llol" wt. % ;, r."t. " \'fatsr ' Raaiatanoe

1.4+; ?Jo. Gala. Httavy Po {llft" Iron .!z..!arl Pia ohor at 25°c.

1 8 63.2 0.01 0.12 Z60 ohms 246 oo• 68.S .. -

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' 6 aa.e o.04 o.l• · 270 8 6 81.8 0.03 0.32 · 210 9 15 ez.s c.oa 0.30 210

10 6 83.7 0.(16 0.22 280 11 6 82.6 o.os o.1e 280 12 r; s2.o - 0.02 o.2a '°° 13 6 si-.a 0.03 0.16 21':> 14 5., 4 84.6 0.03 0...13' ZfJO lfi tr-·- -- " -·-- .. - IK~i · - . ·o:.-c» - ----- 0~17 soo 18 b 83.~ 0.03 o.32 166 17 r> 81.8 . 0.12 0.22 4'1t> 18 ~ ~.()< 0.02 1 Ool4 . 115 19 f> 81.4 o.04 0.24 • 160 00 6 90~7 o.o3 0.10 280 21 6 92-~ o.oa "' ;

0.24 - 200 za 6 .. 92.2 0.02 o.2s 200 28 l 98.9 o.o~ o., 110 24 6 9S.9 0.1~ 260 2~ 6 ~~1 0.04 o.i. 260 26 5 96.o 0.02 0.04 810 2'1 6 9,.9 o.o3 o.os 2$0 28 5 96.8 0.02 0.1• 2fl() 29 6 9&.o 0.01 0.14 280 30 6 96.o 0.01 o.i1 ~o 31 6 9'.9 0•03 c>-o7 280 32 · 5 94.·a. 0.01 o.o9 32o S3 6 94.9 0.01 o.oa 2VO S4 6 &i~3 0.01 o.os 090 35 6 . 93t.IS 0.02 0 .. 04 ·'10 36 6 9'.4 - ·0.02 0.0& 400 87 6 94•1 - 0.03 0.09 :WO 38 &v~ - · .. , .. , • 9~L __ ____ Q..,QL _ _____ 0•1'- · 411 -----·- --- ----- .. S9 6 $S,6 . 0.01 o.06 416 40 6 93.1 o•o• 0.11 2bQ '1 6 i2.9 ·o.oa Oel6 = - 42 6 93.1 1 0:04 •0.11 43 6 81.e· o.z o.oe ~o 44 15 94.~ o.p1 ~-- ~ , _o.oa •601 46 6 94'.3 0.01 Oo09 310

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-Stam.lard Oil Company of Inlliana . 8 t~rch 1946 0

and for HA.cvice in coru10ction · ith the closo- ou.t of operations , all as requirod Oi' a. proved by the Contra0tintY, Of.ffoor . In conformity with current neJotiations, it is proposed that you m:i.nta:ln procoss equipm'1nt in ~ro . {. Procoss Y.ahorat.ory in stanrl- )y conriltion and ;'ltore Governm1.mt proparty on a mu tually agreeable fixed- :1rice basis to be covered by a r.uI'plom~ntal !li!."'"'·~:"11'1nt to thla contrnct .

Receipt is acknowledged of ycur hreak- down of proposed fixed• price for stand- by and storage . It is requested that you .furnish for approval of the Contractlng Officer an ontimat~ of all cnsts, 0xc(!)pt for storai;e anLl st. nd-by, that may bo inm11·rod L.--i comrnction with the above d ir'ections.

- 2-

Ve!"/ trnly yours,

/s/ A. Tainmaro A. TA~Jli-JARO ,

Lt . Col . , Corps of ,nginears, Contracting Officer .

." tnnda rd Oil c 11; ~r; ct l'.V r, r r;y~ ~a.n ·1,

.110 R. ~.ic~1,;. 't.J.l~ ;~v ,31J·1 ·, ; c· . Caf~C, HJ.in" i '1 .

/

Att,nt,i m ·rr • . T. K. •loh~rts .

i..:i'or>11t:t;e Js .tle t.o JOUl' Colltmct do . -7/~l·1•eng-1~1 , d:.t .. d 2 Tl~cr:r:b,")r 1 . .:~J , f01· the der1i1~n, cunstr'l.1ctinn, .tnst:-:1lation and npF:}ra­' ion of fac-1lit:.i--1 ;,'or t.'l., ::r(v,11ct-ion of X Pro 'tct.

Cont' L'JlinrJ tol~g--:·nm d, 1t"ld 1 1'' hri:tary Ulh , Y"'U arn d.tr ,, !tr>t"l to c~Jase op rr~·: , ion ~f the faciliti~s ':.lff0ct.ive S a . n . , /~ Fo'irumy i · 1+6, e:>.cept for final p.::·ocossin'-' of' such rr.aterial then in p:rricess "'Thich in your judgnent :1.; economical . You are i'urthe-r cUrectod as i'ollO"."::a

1 . I t'Oinptly 1:a.1h vtt t~1;~ nl..'1.nt ancJ ~)l.1c, it :b :itand· o:,- conJl tlon .

2 . , .1~r1p · •' ~ f pro 'net ~ 3 .Ji ·ricted by c,·;ntmctinc: Officer .

J . l<'-i!·.ni<}h r! 1·o~iort .au .mrizinz yr in· ::ictivi-t.ioc , findin~ r,; , and concJ.1Hdons m1 "IUch othor repo.rts e.::: dirocto'~ '>y the Contractlng Officer .

4 . 1n conformit.y r ith rgicle XII of the contract dispose oi' !lll Governmnnt property detrn•r i!i.od by th , Con­t.racting l)ff'icor to be surpl •ts .

5. Place all other Gov0rnrnont f'l'Opcrty in your 1fo . .3 13oiler HrnrA :3.nd ·~ec:lu·"'lY locl{ rPrn nreMises ll~' rJ.ii'ect~d 1.Jy Cont ... act.int~ )f.ficer .

Ti , :l.d~urnernont ' ill not ~e •"adq t0 your l'or )Xp0nsAs incurred aft.-.r B i . :1 . , 4- . 'ob.:-ilSI"J 1'~·1,.6, unl,,si; s1 b:scquently directed t·-- r~surne production, nxcet)t fc'r t~o r.ork a..,.,ovo- mentioned and except 1.or 811ch

··'lp~n~HW ns E:iy ,.,_, n<"Jces m.r;.· f o:r:• t.1 '.) protAction nf .lOVe rnment proporly