Manhattan District History; Book VIII, Los Alamos Project (Y); Volume 3, Auxiliary Activities; Chapter 7, Boron (B10)

Page 2

a. marly in 1943, the Loa Alanoe Laboratory indicated a need !o~ qwuiti ties ot cryatalline boron ot normal 1aotop1o content and c17•talline 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 a s possible. The original requirem&nts included the utmos' secrec7 and minimum public1t7 in all phaees ot the material production. to be conducted through oral discussion and thua limited correapondence and records to bare essentials. b. The desired materiale were obtained through1 reaearoh and proceuing b7 the Norton Com:pa~; supply of r aw 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 ~\me ricen Cyanamid Company. ~ach of the orga.ni1~tion1 involved and its respective performance vtlt be referred to herein under a

Page 3

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: 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 disouaai on resulted in arrangementa wherethe necesaar1feesearch and development for the pr oduction of 500 to 1000 powids of cryatalline boron of normal iaotopic conten' and 50 kilogr&lla b. The need for thia work had been anticipated by personnel at 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-

Page 4

gated when the Had.ison Squs..re Area arro.ngementa became effective, but the tnformation ~h ieh had already been obtained was GUCh that develop. dissociable complex or pol71Der. Columbia 1~1thted a research program concerned '11th trut reduction ot 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 $econd• ia :produe1ng oryetallins boron. 'l'h.eae activtthe ar reterrecl to in App endix l for the reductio• ot boron tritluoride fllld in look VII . Vol . 1 1 for the production of or1eta.lline boron. Th.a'

Page 5

production applied to materia.l of normal isotopic content and was 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 partiparticular 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 289 , effective 15 March 19411.. called tor a suppl7 of 650 pounds of the code s1Jllbol for boron trifluoride containing not leaa than 97% ot contract increased the quantity of raw material to a total of 92, 450 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

Page 6

3groemen t to part i c i p~ 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 ·~a s effective as of 2 Dec ember 1943, the con t empla ted work cons isting of the design, erec t i on a.nd operation of a auitable pr oduction plant for the s eparation of boron i sotopes. In addition to the above work it was understood that the t he oer ta.inty of t he aarl1 success ot t he propoaed proj ect; training A g~nera.l history ot the contractor's activity in meeting contra.ctu.al requirements is provided in Appendix 5. Tha t history of t he separation project describes: the work objective& selection of the production contrnctora plant design fea tures; initial opera tions s upp l e~entar;y plant conaiderat1ona1 and the then tutu.re possibilities of t he process. Maj or p robl ems wh 1oh a!:f'eoted sch edul ed production r eeul t ed :f'rom the i nadvertent 1ntrodua\1on ot mercury into the plant sy$tem during t o be quite aerioue in 1ta nature and lad to the erroneous conclusion t hat the initial plant would be unsuitable for production and tha• repla c ement would be re quired. r.ater on during the contr ac~ a corrective measure was d i scovered and the origin.s.l plant proTed to be operable for During the period of opera tion, a total of 736 gallons o! he~vy golymar '" &S produced. >\p pendb: A... 7 providea details of t hat production in regard. t o l ot quan titi e ~, percent of heavy pol ymer for each l ot , etc.

Page 7

Contract 1- 7418- eng... 41 , of 2, 309 , 546. 88 , prior t o any adjustment required On 8 Ma.roll 1946 the Contractor was directed, e2cep t for the economical accordance ·-11th that suppl eme.u'81 agree ment, the contractor placed the va.1 directed by the contracting officer . Cyannmid Company. re quired the contractor to proceea product 890 A to the final product 891 • 2 roduc h 890 A 891 A vere the ~e&p ectiY• 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

Page 8

the production of separated complex froo the Stand'3rd Oil Company of Indiana. The rate of production of the sep~r a ted complex had been estnblished , by the Chicego Area sud the Stcndard 011 Company , t o 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 material from the Standard Oil Company, work continued at the American Cyanamid Company. to improve their process and to prev ent 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. 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 atio of the BlO isotope , and 242 pounds of calcium fluoride- boron trifluoride complex, containing a greater t han norr.:ial r atio of B11 , ~a s obtained

Page 10

t he necessary r u a c ur c~ -::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 A pilot plant ·as set up to (lCCm rula te c:i; i > ~c er .i.r. , data nec 1.. s sury l or the

Page 12

a. Rate of f ormati on of r:iethyl fluoride b . Rate of a cumulation of methyl borate conplex a t :!1€ top of Phys i cal pr 0per t ie s l. Vapor pr essure r1 f methyl borat e , diethyl ether complex, dimethyl

Page 13

mp l ox. a c curate determinati on or the a ( the simple proc~ ~ 3 f r 1ctionat i on

Page 14

1. Conversi -: nin p'tc ko ri tubes b. Snnll sc~ l c r educti on on f ilcncnts c . Stla.11 sen lor educti on in tub e s

Page 15

c omplo t e conversion of t h0 ztnr t irlb ~ oron cor.:pound boron discl osed tnut of them all, !r or I, ·:10ul d bo e xpe c ted to wns r e duced by H2 on, or in ~h e noi chbor h ood of, c s urfo.cv ~t 1,300 to l,soo• K. 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 BBr 3 with H2 ~ ~ ~ f ound Expe rimental invost i gnti orui 5ho-~o d tho.t under propor conditions the boron leas tho.n 80 per cont) nnd t ho B c ombinud with tho hot surfaco c ould o.lHnys be r o - rlsod f or tho oonmorcinl producti 0n o f GOO grams 1)r more of ·B por 1ny. A pilot 1. Tho pr0pa.rnti 0n o f bor on by tho r oductif> n of bor 0n trifluorido with s odi un. .1\ 3. Ex t r r.cti on ofs c)dium fluvridc by \Tet e r fi'om tho r o'.lction s. Pre pul;"'.ti c n of bor on by the roducti on ~r boric a.nhydrido It 7'0..S tho object o f this r l.s.::nroh progrru:i to dovolop n oho.'llic"l nutho d tor the rroducti ,in ~ f b or on of high purity. Ini ticilly, tho objc c t 17o wn.s to pre duce boron oi thor aoorphous or ot.herwiso o f a.t lc:.st 95 a.t0a por cont purity. ta.tar this

Page 16

tom~ra. turo. (2) A singlo-stngo process whorein oryatnlling boron or conaolichted bor on t rifluoride nt high tcoperfl.turo. tha.n m tho c onprohonsivo study of tho purity of tho product• obta.inod or their where the hnncUing of tho mnt orio.ls and tho typo ot oqui?30nt uacd provod to be cul t i cs encountered with oqui pnont o.nd hnndling ot mtorinla prosontod obata.oloa III. Annlytionl Methods sults fr.or:i ~hioh n oor o sinplo sntisfnotory r cutine i:w.ohine could bo doaignod • Following the conp l etion of t his i natrut1vnt. ci. second co.chine for r outine plo.nt 4. .~nnl y s is ;; f bnr on r luori c -mothyl & thor complex