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33 0 -m ...

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UNCLASSIFIED

1, - Eo ta, Haring 2, J, 3, Bwbage

3, .- Loa AXamos

-= Los Nrunos

-.. .

.

UNCL ASS\ FI ED

s-206-P

9

-3-

JNSTRUl6ZNTAL ANALYSIS

. Gmuph

R. E. Brocklehwst, J, Goode, Dg J, Hunt, and Do Lo Timol3

M T.. ABSTRACT

Seve.ral, bismuth cmpounds have been s u w t t e d by E, Orban for exaiili- mWm by X-ray dSfract ion, The sm6!.e of polonim in contact r.~ith p l a t inm mentioned in t he May Progress Bepord-'t.ras received anti identified tentatively from its X-ray diffraction pattern as RPo2,

Cslibration of <;he Pwkb-4Sher ixdrssed speclrophotciieter has been cornplatad and a pre-nary study of the infrared absoqkion 0% Ni(C0) , made,

spectrophotometers have been eomplated, Data slim&~g t h e spsctrd. purity obtainable on threz ultr2~5olet-vis ib f r e

Th.e emissfcn spectxm 02 a smple of volabile impurity from the operations 2rocess has been obtained,

TI , DETAIIED PZPORT . .

An X-ray Diffractibn Analysis-

A tot.4. of f i f teen different preparations of bismuth compounds have been submitted by E, Orban for anzdysis, part of vhich ms r3ported in ths Xay Progress Repcrt , l In gemral , a l l preparations of BiF3 or BLOF (rvi-bh m e exee$iton) have -yielded one of -Lwo different c rys t a l structureso ran be indexed In an orthorhoabic &ruc-ture xnich nay be the orthorhoinbic form sf BiOF which is rnent2oaed by Auri~iZlius,~ The other structure is I Q O T ~ con- plicated and 1n2y be the co,npound BiCP2HF d s o ffientioned by AwivilEuso E, Orban is gciEg to perfom chemical artalysis to establish these p o h t s ,

One s)cruo*~u~e

S a p l e s of both alpha and beta forns of BQO3 have been prepared in order t o obcain stardard patterns cf these compounds, patterns it w i l l be possible t o aetennine i f Bi93 exists as an irUpw5tiy i n the o t k r compounds

By t h e use of these

The smple of polonim on platinum was received from A, ?;5, Mafiin for The diffraction &%ern contained no l ines oZ X-rzy analysis on June l3 x949.

e i ther golonim o r p l a t b m , hut, a11 of the lines viere indexed ir a hexzgonal system with la t t ice constants of a, = 40104 a

1750 -0 . .

1450

1300

1150

1000

I

850

700

550

400

350, d

. ' t .

0 3

PERKIF

DISPERSION CURVE -

FOR

..

-ELMER INFRARED SPECTROPHOT(

I . . "t

, . ,. -. , .: .. .. . .

I i + WAVE LENGTH MICRONS J

I I

4.0 5.0 6.0 f i

7.0 8.0 * . I

METER.

I

, - I I

9v . . Data were taken for t h e Beckman 1961, mGdified %ckrmi, and the Cary recording spectrophotometer for different combinations of sources ,e. 'L - .r *,and recsivess .

desired source and receiver, Le,ngth drmn was E& a t the desired value and the slit width varied until, the galvanmeter was brought back to balance, The Cargr Instruneni; was operated by s e k c t b g - the desired 3 o ~ c . e - a n ~ ~ ~ ~ ~ e ~ e ~ ~ ~ - rmge wi%h the slit control Set a t 40 and the selector sw..kch set on A,C, How tvith t h e comp?iscn cel l cornpa&- men-& doar s3.i.ghKLy openr the output of the smple sell. compartment receiver i~ sompared t o 8 constant input into t!ie standard ce l l conpalri;ment receiver con- 2roSled by .the s l i t ccrhrolo adjusbed mnually t o cailse the recorder t o balance a6 zmo densi-ty, showing mechanical, slit widths as a function of xavelength were obtained i n .this manner, .\ Disprsion curves bdlcating the spectrun band vric€%h, in mini- rrjcmns per mi3-'b.eter of Efieap distance in the plane of the exi$ slit3 had been suppPLcci hy themznufac.tu_-srsarid m e repmdueed in Figures 2'2nd 3? spctral band x id th a t any wnpej-mg$h was obtzained by g e t t h g t h e product of Lhp-..pechanical 3?,&~wavelerq$h,

as indicated i n Table X,V The $ ~ I O Bschms were -operated bx \posi$iorxhg the ---' I a~:!'" * - -'e

. I ,_,.I. t Then-vLthJ/t;he selectoor switch at CHZCK, t h e wave- .

';:a~el@n&h values were selected and t h e s l i t Data

nid3h ad. the dispersion in the plane of the exkc slit a t These data for t h e dizferent inst-wenix are shxyn in Figwes

\ . c 0 E&ss$on SPectrosc'op~

Four sealed tubes contcii,njiig samp7,es were prepared by A, \Yo HarLir-, The first tube contahed o-dy he l imo the second was a &me of helium md mercury1 the third tube obtained f r o m V, F, ?esold, contained sone of the volat i le impurity f r o m the 0perzi;ions Process under about one m, pressuse of eo.iiercia1 helium and the f o w th 'cube contained abouk f o w cur5es of pwif ied

Instrument

Caw

I b n ~ e Covered Source

Gary

Optimum Range

Lfodified B3clunan

Receiver or Region I

Modified Beclanan

- Cmu > k$&.l-,, I

Modiffed Beckman

€I2 Disc.

Beckman 1961 (Standard)

Beckman 1961 (Standard)

Beckman 1961 (Standard)

Bechan 2969. AS$ nd:drd) Y-

Photomul-biplier (V,V, Reg, ) 210400 200-335

H2 Disc, Phohmil . t ipl ier ( V i s Reg, )

incand es c en% Photomultiplier ( V i s Reg )

H2 D i m , Photomultiplier

Incanda seen% Photoataltiplier

7

2904-620

290-725 335-7'35 (800)

ZO+G5 200-320

300-&15 320'"6140 ___I_.,.

H2 Disc,. Blue-Sensitive PhotootubQ ' I 2lO-420: I 20@-=325 I 630-105 0 I Tncandescenf; I Red-Sensitive Phot, ot ube I 340-ZO50

7' I 380.2630

Incandescent I Blue-Sensitive Phototube . 1 300-645

1 P Incandescent I Blue-Sensitive Phototube I 305-tt.oo I 325-380

. . . . . . , , - . . . . . . . .

' 8 9 1 2.5 3

........... . . . . . . . . . . . . ?-- . . . . . . . . . . . . . I : . : . . . . . . .. . - . . I . . . . . . _ . . _ . . . . . . . . - . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . _ I .... . . .

. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .- . , . . . . . . - . . . . . . . . : . . -

. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

::.;I; ... yj.; .... . . . . . . . . . . . . . . . . . . -... . . . . . . . . . . . . . . . .

. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . - . . . . . . . . .

. . L , . . . . . . . . . . - . . . .

1; --!f?#;;

. I . . . . . . . . . . e _ - . . . . . . . . . . . . . . . . . . - . . . L . . . . . . . . . . . - . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . _ . . . . _

. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

.*.. . . . . . . . . . . . . - . - ... :: :- 1::;. :::ilZp?Y; . . . . . . . . - * .

. . . . . . . . . . .

. . . . . . . . . . . . . . . . i . . . . . . .....,....... . . . . .... .! .. ... . - . . : . : : : I . . - .............. '71

................... , . - . - .a .-. f . r . . . . . . . . . .I-. ..... ,,. ................... ,....-_ 1 . . . . . . . .

. . . "3

1

. ' . < C . -

SPECTRAL PURITY

. . < -., :

0 . .

9

re51t I ML! -313

P U R I T Y I

7 0 F I M O D I F I E D BECKMAN I +

I

UNC

I

f

INCANDESCENT SOURCE

4

1

C

I+ U.V.

SPECTRAL PURITY OF

CARY SPECTROPHOTOMETER I!

IO 600 800

C .

colonium under abotik one me presswe of comercial helim, The sample tubes Lave a pbne qmrtz wjll~low in one enci ~~~owr in t i ; observation of the KIA,- Faviolet spectra, 2200 A t o 9080 A have been obtaiaed and iire being interpreted, source used xas an R,F. generator PSI Serial No, 1 built by the ZLectrolllics Seekion, EJ.eci;ronics Section so t h a t more k-bense enission can be obtahed. pans of the polonium sample are in the process of being taken.

Spectrogram of t he vol.zixile inpurity sample covering %he Yange from The zxcitation

A more powerful It,??, geneyator i s nmi king constructed by the Spectro-

PSFERENCES

1, liound L2bozoatory; Iiiamisburg, 0M.o @ay l-%L3 1949)

hfikiv f o r KemiJ ZinerologL, och Geologi Bd 26, No, 2,

Timma, D, Lo, Instsuneatal Analysis Progress Bepore, IGI-357,

2, A ~ ~ V ~ J ~ . U S , Sere, X-yay &westigation on Bimu-Lh Owfluoride,

3,, ldellon Insti tute, A.r) , Io , Project U s No, 14.4.

. , . P . 1 . - .