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DECLASSIFIED IN FULL AufJtority: EO 13526 Chief, Records & Declass Div, WHS Date: DEC 1 0 2012

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DECLASSIFIED IN FULL Authority; EO 13526 . Chitf, RlCOI'da & Dec/ass Olv, WHS Dete: JUl 1 9 am

vJ(3 eNFI B EN'IAt

~48405

DEFENSE DOCUMENTATION CENTER FOR

'SCIENTIFIC AND TECHNICAL fNFORMA HON CAMERON STA liON. ALEXANDRIA. VIRGINIA

Office of the Secretary of Defense S' atJ'f lee. (" t"-:z Chief, RDD, ESD, WHS A.kif Date: ,,:rUt. "'/...f)I' Authority: EO 13526 /' Declassify: y., Deny in Full: __ Declassify in Part: --Reason: ---=-__ ~~ ___ _ MDR: ~-M- :J I~q

Page determined to be Unclassified Reviewed Chief, ROO, WHS lAW EO 13121, leation a.5

Oltl: JUL 1 9 •

NOtICB; Wben govenuaent or othel' 4ftv1xrp, apec1-ticatJ.ons o%' other data are used for a.ny p'.1r:pose other than j n cODllectlon vith a definJ. tely related government procurement operat.f.OD, the U. s. GovenllDl!ut thereby incurs DO responsibility" 1101' ally obllption whatsoever; 8.Ild tl:Je faet that the lJovel'!l. moDt ~ have tonaulated" tUrn.1.ahed, o%' in au;, way supplied the said drav1np, speCU'1e&t1C'DS, or o'",her dah b tIOt to be ze~d by 1m.rJ.lcat1011 or other .. ,,1e~ u in allY manner lic~nslll8 the holder or IIoIlY other person or corporation, or C!OD-feyins an.v r1sbts or pe1'lll1esioD to manuf'a.c:ture, use or eell an'.)"

patented 1.I1vention that may in IUJ;Y ~ b$ related thereto.

IlO'l'ICE:

msr £E SSi!iSii2 &21£ 22£1IiQ, '. dE UJJt££ Sl \SF mgn 75' dEdi 41. 6_ It aCE am, 21i& i6,

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DEClASSIFIED IN FULL Authority: EO 13526 Chief, Records & DeclassOlv, WHS Oate: JUL 1 9 •

DECLASSIFIED IN FULL Authority: EO 13526 Chief, Records & Dec/ass DiY, WHS

Date: JUL 1 9 • 1 . .1.

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~ O'IJF. This document consists of _Lt;;!. pages,

and is nmnbcL _'2.. 7. _ oL .4:q .. COPies. serics __ A_ .. <.itld tile following~~ attachnlents.

FOURTEENTH QUAllTERLY PRoaUSS R.EPOllT

ON DISSltMINATION OF SOLID AND LIQUJD BW AGENTS

(UncIa •• ified Title)

EoI' Period 4 September ~ 4 December 1963 Contract No. DA-18-064-CML_2745

Prepared for:

U. S ArlDY BiolOgical Laboratories Fort Detrick. Maryland

. ~.-.

Submitted by: ... ~ __ ~_"_ .... :u .... -....~ __ _ G. R. Wbitnah

Report No: %512 Project No: 82408 Date: 3 February 1964 Approved by:

AEROSPACE RESEARCH ZZ95 Walnut Street

'!U? 2PS" H R'Q Wmra. St. ·Paul 13. Minnuota ~. Fr HeWn ';a-n 1B32LZS . .5 3 Lit 6 IS

R?" •• ",iZ

Project Manaler

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Staf1 membel'l of the AeJ'08paC8 a ... uch Depadmeat aACl Eftl1Aeerifti

DepartmeJlt who have paJ1ic1patecl in dinctiDi or pufo:rmilll the work re­

porteci hereill iftclllCle 14."1'1. S. P. Jone., Jr .• Q. Whiblah ..... Sandarell.

A. klelnlOD, D. 5teDcle1', a.. Lindquilt, J. McOiUic:wicly, 1. Upton.

W. 1.. Torloloo, P. Stroam, G. UorUtt, A. T. B~. D. Hal'l'iQ.toll.

R.. Aeltroycl. D. KecU. B. Schmidt. G. LUQ/!.. R.. Dlahlberl, E. Knutlon.

J. Un, •• J. PUlley. A. J'ohluoa. G. Leiter, C. A. Morril, K. Pcmtinen. aJld G. VoU.

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Page determined to be Unclassified ReViewed Chief, ROO. WHS lAW EO 1aau, &lotion 3.5

gltt: JUL 19 •

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_CPI.I.a,. ABSTRACT

DECLASSlfI"!O IN 'ULL Authority: EO 13626 Chief, Records & 0ec:Ia8s DIv, WHS Date: JUL 1 9 2013

Th18 Fourteenth Quarterly Progres. Report pre •• at. the resulta of

work coaducted at General Mills, Inc. , under Contract No. DA-18-064-

CML-Z745. "Diaaemina.ti.on of Solid and Liquid BW AleDt." dm-lng the

period 4 September to .. December 1963.

euuant theoretical tln-utiptiona re1a.t11lJ the inte:rparticle contact

enersle. to mec:hADic:a1 properties of compacted powderl are described. Althoap an idealbed system was used, the trend. predic:ted a.re in accord

with experlmeDtal data.

!!.I.. (lot SQI-M-I09' to be used in lortheomiDgllllht teat. was found to

be more dil£lcu1t to compact than!& (lot 17) u.ed previouely. A new ap­

proach to obtain the energy of compaction from wtron data i. pre.ented.

Alent LX like othel: hi.hIyelaatiC: materiala waa fOW'ld to be difficult

to compact, has • comparatively hip compaction ahear strenjth, and a

tenaUa atreasth too low to meaaure.

An evaluatioll was made of the buoyant force conecttons for the BET adeorpdon method to measure total eunace area. Total 8UI'{ace area. and

""o.lty measurementa were made for apray-dried saccharin, agent LX,

&lld en embryo.

Our methods f"r preparing .hadow-cast sample8 for the electron mic;;ro­

BCope have peo.u1ted in obtabul1l micrographs abowing greater deta.il in

pal"tfele shapes.

A stud,. of the effect. 01 humidity (from 0 to 100 percent R. H.) upon

the formation and decay of a around powdered lugar aerosol is repol"ted.

StoralP teeU on aamplea of com~ded ~ indicate little chang. in cle-

4sslomeration efIiciencl •• and viability after 6 month" at tenlperatures of

-2 and -2]·C.

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DECLASS"'!O IN I'UU Authority: EO 13526 Chjef. Records 8. 0ecIass 0Iv WHS . Date: JUl 1 9 D'

•• - ----.-,-.... - -.I". ___ -_-.IIt,,;.._. ______ .. __ _

",r'h,1l1i

AD expe:rimeJlt conducted 1.:.ing MietrOil Vapor talc compacted in a

6-i.nch diameter tube wiped with graphite au4 UJled with polyethylene film

pla.tic ineUeated. that llicle-wall fl'iction can be materially reduced U suit.

able metbocia can b. found for prevenilnl intimate contact of the powder pal'tir:1e. with the wall .ud.ce.

lD pl'epa.ration lor the low •• peeclllight trials of the E.41 'PRY taDk on

tho Mohawk OV.IC airplane. an E-41 was filled wJth compacted talc and

,hipped to GrubUft&n Aircraft EDJineeriq Corporation. Bethpage. LOll,

bland. New York. A m&DualloacUns techDiqu.e uSiD, pal'tial charle •• a. c1eveloped in aDticipation of urina to load the E-41 with !I in th. field dunq the Ill,ht trial ••

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T ABI.E OJ' CONTENTS

Title

Page determined to be Unclassified Reviewed Chief. RO~. WHS '. I,AW EO 13526. Section 3.5

Date: Jut 192GB

Pal.

INTllODUCTtON

STUDlI:S OF THE FUNDAMENTAL BEHAVloa OF,DR.Y POWDEIlS

2.1 2.1.1

2.1.1.1 2.1.1.2 2.1.1.3

2.1.2 2.1. 2. 1 Z. 1. 2.2 2.1.3

Behavior of Powdel'l in the Compacted State Theoretic&! Iave.U,atiou of the Nec:haDlc. of Compacted. Powuu Azl&lytica1 Compactloa Thlory Cieaeral Behavi02' of Compactable Po'Miel'a Behavior of Compactable Powa.r8 at LOw Denlltie. Current Stuc:I.i •• with ~ &Dc:I. A •• at ~X Compaction Charaeteftitlc:. Shear Str.nath ancl Tln.il. Stnnath of Aslnt LX Analyel. of m.tron Comp&ction Data

PHYSICAL AND CHEMICAL CHAa.A.CTJ:lUSTICS OF Till: POWDER. PARTICLE

3.1 Total Surface Area l.I.1 Stucly of Buoyant Force Correction 3.1.2 Spray-Dri.d Saccharla. E., 2mbl'YO, and

Aleat LX 3.2 Particle Shape 3. Z. 1 Shadow-Caat1nllor lClec:tl'og Micro,zoaph. 3,2.2 EiJ lCm'bryo 3.2.3 Spray-Dried Sacchal'in 3.2. " Alent .LX 3.3 P&rticle Size Dl.trlbutioll aDd Particle Den.lty

AEROSOL STUDIES

•• 1 Oper&tin, Procedure 4. Z Esp. rimental Work &lid R.e lult. 4.3 Data AnalYlie

v

2-1

2-1 a.1

2-5 2-15 2·20

2-24 2-24 2-2.4 2-27

3-1

3·1 3-1 3-6

3-1f 3-14 3-16 3-22 3-2Z 3-32

4-1

4-1 4·Z 4-6

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Page determined to be Unclassified Reviewed Chief. RO~. WHS JAW EO 13526. Section 3.5 gill:

JUl 19 201!

TABLE OF CONTENTS (continued)

Title

. ms8EMINATION AND DEAOaLOMEllATlON STUmu OFSTOUD!!!

USE OJ' DIn Lt1BlUCANT TO REDUCE SIDE 'WALL "lUC'l'lON

PUPAaATIONS FOR. FLIGHT TESTS OF THJ: £.41 SPRAY TANK ON THE MOHAWK AIRPLANE

1. 1

7.2

Shipment of E.41 to Gl'\IDUD&D Ahc:nlt • lI:Dflineerilll COZ'pOl'atioft

lI4aDaal Teclmique for n.w LoMiQ61E-41 Spra,. T&ftlc with !8.

SUMMARy

UnR.ENCES

vi

Pase

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6~1

1~1

7-1

1-1

8-1

9-1

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Z. Z

2.3

Page determined to be Unclassified Reviewed Chief. ROO. WHS IAWE01~6,~~ Oate: lIUL I ~ ZUU

LIST OJ' ILLOSTRATIONS

Title

Kuru' Balance at Eq,QiUbrium lor a Compactable Powder

Contact EnergY' 1:1 (x) va. Compaction Panmeter x

Contact Ener." ~(x) aad Compaction EBerlY E(x) VI. Compaction l"ILrameter x

Py.

2-3

2-8

2-9

2.' Volume Coetticientl al va. the Number o£ Contacts 2-12 per Particle i

Z.5 Theoretical Compaction and Contact 1:1181'11" VI. Z-13 Dell8ity - Sphert"! Particl".

2.6 AnalyJIi. o£ Cohelive Shear StrenaCh • Dbect h&r Tut 2-11

Z.7 Theoretical Aerodynamic Breakup of 8m 342 lor: Z-19 Ca) Pre.aure-Induced Breakup, (b) ShW-Induced Breakup -Critic.al Sp •• d VI. Density (Critical Speeds Relative to Critical Speed at p~ 0.4)

Z.8 Theoretical Aerod)1I&mic Breakup of Two Sm Lou - Critical 2-21 Speed VI. Density' (Critical Speeds A.laUveto Lot 342 at

p= 0.4)

2.9 Critical Slide Angle Analydl 2-Z2

2.10 Compaction Characteristics of !i 2-25

2.11 Compaction Characteristic. of Powderl 2-26

2.12 Compaction Shear Strength 2-28

Z.13 Ener&yof CompactloD of!i Lot SCH-61-109 ~-30

3.1 Buoyant FOl'ce a8 a Function of Pres.ure for: the Quart. 3-2 Spring. BUcket. and Fibe". at Adsorption SJlItem

3.a Buoyant Force CD Quartz Sprins. Bucket. aDd I'ibel' aa 3-4 a l'unCUOD of Pre .. ure aDd Weight of Buckat

vii

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3.3

3.4

3.5

3.6

3.7

3.8

3.9

3.10

3.11

3.12

3.13

3.14

3.15

3.16

3.17

3.18

3.19

Page detennined to be Unc:/asa/fied Reviewed Chief, ROD. WHS lAW EO '352e,1Mon 3.5 Oate: JUl 1 9 D3

LIST OF ILLUSTRATIONS (colltiauecl)

Title Pale

BET Plot of NZ Adsorption on!!!!. 352 Showiq 01 Correction GIl D.:.ta

Eltace 3·5

BET Plot of HZ Adlorption on Spr.y-Dl'ied Saccharin (13l)} Shr..tng Normal Errol'

3-7

BET Plot of N:a Adsorption on Spzoay-Dzoleel Saccharill U 3C) Sbowi21, Normal El'l'ol'

3·8

BET Plot of HZ Adlorption .Data on Alent LX 3-10

Pal'tialleothenl1 of HZ Adlorption on A8aat LX at Li4luiel HZ Tempezoatul'e

3-11

BET Plot of HZ AclIOrptiOll Oft Ell Embryo Showin, No1'll1&1 Errol'

3-1Z

Acllorption Isotherm of HZ on EU Embryo at Liquid HZ Temperature,

3-13

Sketch 01. Shadow-CaIJt era .. Vieweel from the Top 3-15

Sketch of Sbac1OW-Ca,t!DI Process 3-15

Geometry of Shadow 3-15

Electron Micro.raph of Shadoweel E'I Embryo 3-18

Elecuon Micro,l'aph of Shadowed Eg. Embryo 3-19

Electron Micro,raph of Shadoweel Eg. Embryo 3-20

Li.,ht YlcrOfiraph of E,g Embryo 3-21

Litht MicrCllraph of Ell Embryo 3-23

LIFt Micro,1'&ph of Spray-Dried Saccharin 3-a.I

Electron Mi.cro,raph of Spray-Dried Saccharbl 3-25

viii

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3.20

3.21

3.22

3.23

3.24

3.25

3.26

4.1

•• 2

4.3

4.4

4.5

4.6

4.7

7.1

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p. age determined to be unclassifi~------"""·l~·:;.:~ ReviewlCl Chief, ROO. WHS I .~ lAW 110 13121. Stctlon 3.5

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LlItt: IUL 1 9 • . \J !~

'I

;1- . LIST OF ILLtlSTRAnONS (continued)

"

Title Pase

Light Micl'Olrapb of Alem: LX 3~Z6

Elect1'Oll Mf.croll'aph of Asellt LX 3-27

Electron MiCl'Olraph of Asent LX 3-Z8

Electron Micl'osrapb of Alent LX 3-29

Llsht Minosraph of Alent LX 3~30

LiSht Microsraph of Alent LX 3-31

Particle Shle Diatribntlon of ~ and A,ent LX 3-33

Ael'(Jaol HaU-LUe ve. Chamber Humidity 4-3

Initial Silnal Amplitude va. Chamber HUlQidity 4-4

Slope Index for Aeroeol Rune va. Chamber Humidity 4-5

Calculated Geometric Standard Deviation of Initial Aeroaol va. Chamber Humidity

4-11

CalCulated Ceometric Mean Diameter of Initial Aeroaol v.. Chamber Humidity

4-1Z

Calculated Initial Aerosol Concentration ve. ChlUllber Humidity 4-14

Calculated Mall 0( Powder Airbol"De ill Initial Aerosol va. Chamber HUmidity 4-16

Packaging Arrangement for HaDd Loadins Partial Charla for E-41 Spray Tank

7-~

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zawADa.& DECLASSIFIEO IN FULL. Authority: EO 13526 ct)ief. Records & 0ecIaS$ DiY. WHS _ Date:'

JUl 19 2013 FOURTEENTH QUARTERLY PROOR.ESS lUCPOllT

ON DISSJCMlNATION OF SOL.1D AND UQt1IJ) BW AGENTS

1. INTRODUCTION

The work reporwd herein ia being conducted for the U. S. Al'my Bio·

lopeal LaboJUori •• ullder Contract DA-I8-064-CML-Z74S. Th. prOfll'&Ul

ccm.tat. of experim.ntal and theoretical atud1e. r .. laIted to the Une ~ce

dh •• minatioD of loUd anclliqu.id BW alentl. 1'01' ..... ral mouth. the em­

phalb hal been pl&c:ed on the dry alents; much eHort i. bolna devQted to

the ltud.y of the proc ..... and pbenomeua involved. when dry aleut. are dil­

•• minated from a compac:ted _tate. in order to obtain a more favorable

fiWnl den.tty ill muaition.. Proce .... involved tn compacttnl a,e.e to

abtain the required den_itie. are being included in the studi •••

Work Oil the lundamental propertiea of dry fillllly-clivicled lolie! materials

il being conducted in the laboratoriel. Special Inlt1'1UUentatiOD required.

1.01' theee .t~i •• i. de_i,nee! and. fabric:ated. when I1Ice .. ary. Two full-Ical.

E·41 .pray tanka were fabdcated and lLre belq ulee! in lielcl te.te to study

the di .. em1aatlon &Dd ell.pereion of c:ompacted dry asentll under Datval c:on­

clition.. Flight te~ta at hip 8ubsonic speeds have been conducted .uc:ce88-

tully and preparatione for low.epeed til'SU are currently in pl'ocen.

ProBl'81S hi .everal areal of the program du.rin& the period 4 September

thrOUlh 4 Dec:ember 196311 pre_ented 1n thil report.

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Page determined to be Unclassified Reviewed Chief, ROO. WHS lAW EO 1a58. ieetlen U

JUL 19 InS

STUDIES OF THE FUNDAMENTAL BEHAVIOR. OJ' DaY POWpEaS

DlU'i. the cour.e of thil project we have been 'tudyial the bulk proper­

tie •• uCh a •• nern of compaction, e.ar .tr.ugtb, aua teuUe .treaath

which al" maBile.tatioD'of interparticle contact en8Z'lte.. Ia acld.itloa. w. have atwU.ecl particl. chal'acteriatice--auch a, -,i.e auIi ebapo--that affect

the muDber aIICl nature of the interparticle contact.,

The folluwin •• actiona d •• crib. the r.lt\Ilta of C1II'reat theoretical inve,­

tl,ation. ralatina the ir¢npart1cl. contact energlel to the meehaJl1.cal prQ­

lM'rti •• of compacted powdere. A theoretical model compo.eel at .phel'lcal

particle. of diameter d with an averale eaergy E pel' .lupe coatact is 8m-p

p10,..d to determine the energy required to produce a given chan,. ia aver-q. powder dell. tty. TId. treatment .hould. be of conaiderable value ia

addiDI to our depth of underetanding 01 the behavior 01 powders. Although

we are u8in, an idealized syetem, the trends predicted are .ub.tantially in

alreement with experimental result.. In addition to the reaults of theoretlea1

.tucliea, our current work u.ing !l and other aimulanU ia reported.

Z. 1. Behavior of Powder. in the Compacted State

2.1. 1. Theoretical Investigation. of the MechaniCS cl :eompacted Powcien

Granular material. can be divided broadly into two main classe.: dilatant

media aDd compaetable media. Oilatant materiala are 80 named because

they elUate 01' expand when .heared. Compactable materiale, on the other

hand, are found to contract when eheared. This dhtinction lead. to f1.lDda­

mental differenees in the behavior of dUatant and c:omp&etable materials.

For example, a dilatant powder ia capable of 8ustaining v.ry lar.8 .hear

.trellle. it the powder ie not permitted to expand. This phenomenon was

demonatrated in an experiment reported by Jenkinl -which _howed that a cylinder

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Page determined to be Unclassified Reviewed Chief, ROD, WHS lAW EO 13tH, 8ellltiOn a.1 tJat.1 JUl 192m3

imbecldeclln ,ancllD a caDfined apace COlaW DQt be rotatecl in it' plane.

Similar behavior hae baen reported by ZeDS aDd Othmer (See pp. "17. Refer­;lo

ence Z). TlU, type of behavior ia not o~a.rv.cl with c:ompactable powder •.

For the ma.t part, dry clilatant poweler. flow Ireely and are DOt ordin­

arily subject to bancllina difficu1tiet. By contralt, c:ompac:table powdere

do not now readily and may pruellt I.riou, hanclling difficultiee in certaIn

<:1 rcumetance ••

w. may uk: What facton determine whether a Siv.en powder will be

dilatant or compactable? Th4re i. looel reaaon to believe that the aDa".,er

tc tbi. queatioll can be found. by ex:amlDlDJ the mutual interactioD energy of

particles in contact or cloe. proximity.

Interparticle energi .. will alway. exiet in granular media a. a result

of molecular and e]eeh<J.tatic potential •• al welJ as by chemical bonds. It

is bflUeved that ahort-ranle molecular potentials are primarily reepon~~blc

for the behavior of compactable powdera. It should be Dotecl that thest', poten­

tiale .. re always pre.ent and the .. Sloclated interparticle forces are a,lw .. :.!', attractive.

The total energy per unit volume of a puwder. owin, to interparticlf'

potential. ot molecular oriiin. can be considered to be proportional tu the

number of pantcle contacts per unit volume. It is clear that the lr.tt>rpar>:ic.l""

energy per unit volume increasell rapidly with increasing powder bw.k dell­

alty (See Section Z. 1.1. 1). On the other hand. the gravitationai potent~ ... l

energy increa.ee with decreasing deneity. The eqUilibrium density of tl f'

powder eorre.ponda to the condition of minimal total eneray. This is;.nu&­

trated in FiJUre 2. 1.

r:--------------The basic di.tillCtiOD here ia that dilatult materials ca.DIlot be shear,.·d 'lnt!I the particles fracture, while compactable powders can be sheared wi!'r. Ii

small increa.e in applied load (e. g .• in the piston.cyl1ndel" test).

g ,-------~".,...' .... ...:::.;_ ........ ." """""".'.' li III

,..i~.;.~~!-...>~Jr~-::..: . .i; •.. ~ ',:";, . f II \~:t.-:::;:------- .. 11 \t

14 If ~. .. tL. '. L: It i . . :::. ! :

I I I I' I I I I I I I I I .1 f. I :L

En··8Y per Uldt Mall

.•• ---, .. --.-- ... ~-=:-~.~' ~'--.=.--- _ ..... -

Page determined to be Unclassified Reviewed Chief. ROD, WHS lAW EO 135H, Itotlon 3.5

tJatl: JUL 1 9 IRS

Total SurlY (compactabl. powcle .. ,

COIICaCC Eller" (compactable powder'

GrawUatlow Potential EnerlY

TotallCnulY (dllatallt powder)

Contact En.rgy (dUatant powder)

Fi8UI'e i. 1. Enel'lY aalance at Equilibrium for a Compactabl. Powder

A. shown ill the fill.\~.. the Ira.,hationaJ, potential 8MrlY depend. aaly

OD the powder denaity. However. the contact enerlY pel' uldt ma •• dependa

markedly upon the particle aise. 1'01' a typical dilatant powder. the number

at cODtact. per unit rna .. i. comparatively amallj thu.. the minimal total

81181'1' occur. at a clenaity approachinl the denlity of the eoUd material (for

_ph.1' •• , the maximum den.ity lor a elo.e-packed ."ray l. 0.14 ~p' where

P p I. the particle cleJ18ity). ror compactable powder •• the contact eMrlY

i. 80 ,reat that equiJib.iwn 18 !'e&ched at a much lOWer" density (note upper curve in Fipre 2. 1).

The clepeDdence 01 contact enar,y OIl particle lise can be e.en by COil­

.lderiDl a hypothetical powder conet_tina of spherical particles of diameter

"p' The DUmber of particle. per ullit mall is:

-;

n-"" w -.:~~:.'~':;-~-.::'.:~ .. ~, B

- '-!-:~.~.. t1 d Il~ I~ 1!J 14 jf :l i j l, I I [

I I I I I I I I I I I J 1 ;

J:

.• ___ " .-= ..... -.. ;.~~_-. _-7. .~-.:"-.. :..:.!--:';

Page determined to be Unclassified Reviewed Chief. RO~. WHS lAW EO 1352e. SectIon 3.5 uete: JUL _ J 9 am

The CQIlt&et eurlY pel' UDit mall can De exprellec! by tJa. nlatloubip:

I:c = (partlcl .. /UDit mau)(av. eaerlT/cOZIt&ct)(contac:tIJpartlcle)

(I)

(2)

ift wlUcb. 'I the avora •• eDe"1Y par contact and 1(,,) ,. a functlOl'1liviq 01,

Dumber of contact. per partida al • fuIlCtioD of the avera" powder c!enlity'Q':

It l. _IUy leen that the f\mCtioD f(p) .ati.liee the couGlUon.: 1/1. .. i(" I" p' .:: 6;

fl(I'I" '>0. (The condidou 1(1) = 6 correlpondl to m.xa,oaal packlDJ; I. (I, ,

P 3 .ix cont&ct. POl' particle.) Accorc!1q to Denalin aDd AbIUcolova ,the

.nez-If I 11 proportional to c!p' Thul. for Ipherical particle., the bulk con­

tact e~I"y vari •• inverlely a. dp 2.

A mathematical ~lIaly.l. of the coftlpt.ctlon fuuction I(PiPp) for the 'pecial

ca •• of 1U1.form 'ph,ncal particle. 1. liven in Section 2. 1.1.1. 1'01' parti­

cle. of rlQamdform at •• it 18 clear that the lmallel' parttcle. may contribute

Ire.ely to the total enerlY even when eonatitutinl a ama1l ma .. -traction of

the powder, The :role of particle Ihape iD the compaction proce •• is very

complexl bowever, elODJated or platelet form. c:&D be expected co reBUlt in·

reduc:ed powder dene1ty &Del a tendency to.ard compactability (e. I., conaicier

.nowtlabl or talc pgwc!el').

It h .. been tacitly &alum_elln the above clhc:u .. ioD that tbe powder is In­

itially dea"lomuat:ecl; tor ellUllple, the powder could be conaidered to settle

out froM an aerolol compo •• d of dillcrete particlea. It hal allo been anamed that U.e powc!eJ' laye!' II very thin, linea the weipt of a thick powc!u layer

cause. Pl'OIrel'iYe compaction within the layer. In actuality. moat powders

ift a natural It&te conlilt of _glome rates whJch presumably r.sult whe!! the

Z-4

" , .;.. ~',. or . .. ~'

, ' . ~: h

il t.~ ~. I ··_!:i;"'t·· r1 ........

14 ·4_' ......

~' f~ 1 ~z ' , I. ~ ~ '~ I 1 1 I I I I I I I I I I I,

t

__ -____ .: .... :'-... :8: '_"._"-'_. __ ~._

Page determined to be Unclassified Reviewed Chie', ROO, WHS lAW EO 13&ai, 8eOlion 3.5 [Jate: JUl 1 9 2013

powder 18 zoepeateclly compacted aDd hroken up duriq hudliq. Ther. are

Indication. that tile haDcWD8 properlle. of com.pactaWe powde ... an improved

by ag10aneratel of thil type. Thi. t. nat surpdliD. aiDce the _.l1ome:ratel

can be relarded ... lars' particle. for whieh the "intera •• lomerate" enarlY

il lmall relatlve to the avera .. al~lomerate mall.

2.1.1.1. AnalY!;ie&l Compaction Theoa

A very .imple theoretical model of the compaction procell haa been ad­

V&J:Ice. by Den". Tbll moclel ytelcll a C02hpactiOn .tre .. -uDIUy relatioD­ahip of the form:

(3t

and .how. furthermore that the cohelive Ihear .trensth of .. compacted powder

ia proport:icmal to the compactioa Itre... (The lalt term in the bracket. at

EquatiOD (3) iI u'U&lly _,a,ibIe compared with unity.) Both o£ the .. .::on­cl",ion' are in ,004 alr •• ment with experimenta.lrelultl.

Derr'. theory J. baled on a particWar al110merate 8trw::b&l'e. i. e •• the

.eometrical arra.emellt of the powder particle II f. IIpecified lor each deasity

It&te. A different approach, b •• ed OIl enerlY con.iderationl, ill taken in the followiDI analysil.

E2ler,y of Compaction - We a .. urne that the powder 1. composed o£

.pherical partict.. of diameter dp ' Allo, It is ."\&med that the energy of

& 111111. contact i. •. W. wlah to dete:rrn1ae the enerlY required to produce

a 11ven change in the averale powder den.Uy.

Suppo •• that a puwde:r .ample contains N particle II. lD &D Wl.tr .... d state

the total contact ener • .,. Ie cti..tributec1 amoD, the N particle I in accordance

w:l.th the number Gl contactl per particle. It i. apparent that a particle may

2-5

I' , i ~' "

" i ~

1!!I"w"­F.i ~ .. .. ,

..,. - "-. -:~~--I; t :

11 }1 11 Ii !? 1 , ~

iJ ~ ~ I

I I I I-

I 1 j

- ----......... -.~ ..... - -------.. -- .... ---Page determined to be UnclasSified Reviewed Chief. ROD. WHS lAW EO 13&26. StctIOn 3.& Uatf:

have trom 1 to 12 contact. with neipboPlna puticlu. U we ... ip half

the total contact elUlrlY to each of the particl •• in contact, the eller,y atate of a p8.J'tie1e may rani. from. ./Z to 12( ./2).

w. IlOW a.lIt: For & If,vell total C;Olltact en.rlY ICc' bow an the .MI'IY ltate. cUaeributed .moDl the N pardel •• ? Let the total .IlUI, l!:c be _x­pr •••• d bl the form:

where !1 i. the eaa.rlY du. to particle. with i contacts per particle.

It can be _bOWD from the theory of -taU.tica! m.chanic.5 CIlac the number

of partiel •• in each energy .tate can be expre ... d by the di.tributlon func­tiOIl:

where A 4lDd a ar. con.tants. Lettinl x.: _-Cle/2, the constant A b defined by:

N-

or

!-1 x

(5)

A = 12' 1 - x

(6)

2-6

, --------.--.. ~. ~.~

Ii. ; .

d \1 ..• '! q~:-:

;i-- : ~.1 _

~ ... - .". ,.,. : .. , .. " ~~;~~~::~~:~' '''~ .. "

~:-::-':::~~~- ,:

r~--

11 ~ u ~! u :: r

I

l' ..

.1 1 T

J.

Tbe total ccmtact eDerlY i.:

The enerlY 11lvelted In i th order contact. 1.:

! - 1 Ne x i

Page determined to be Unclassified Reviewed Chief. RO~. WHS lAW EO 13526. Section 3.5 !Jate:

JUL 19 •

(7)

EICx) = '-2 I x (i. 1. 2. 3, , , 12) • 1 _ xl (8)

A DUID"r of the earlY fUDction. Ei (x) are plotted in ",UN 2. Z. The

eDerlY parameter x ts small for 8mall value. 01 total earlY (I. e.. for low

powder denlity) anel increa.l. with IDcrealiDI total enerBY. Thi. parameter

can allO be related directly to the powder den.ity ... will be Ihawn later.

The eneray function, plotted in Fisure Z. 2 give a very ,oed picture of

the ellential feature. 01 the compaction proce'" At low clen.iti •• (emall xl, most ol the contact energy ia dilt.ibuted &mODI the low eaersy statel, A,

the denSity (and xl inc rea •••• the enel'lY diltribution shifts continuously toward .tate. of hipe. enerlY',

It will be ybHrved alia that each eDergy .tate (i :: 2. 3 ,', '. 11) increa.e.

from 1:1 (0) = 0 to a maximum value and then taU. off to Be ro as x becolrle.

iDfll1f.te. For any value of the parameter lI. Equation (7) IJh-•• the total con­

tact energy, A.]I; increa •• I, however. the enerlY whicb mWit be 8upplied

includes not only the incremental value o! total contact energy but allO the

enerlY needed to break down lower enerlY Itat... The latter eDerlY C02n­

PODellt evidently repre.ent. the effectl of coMlion.

Tho total energy chan,e clurilll compaction. denoted by E(x) (relative

to x II 0). la plotted v.rlUI x in Fisure 2.3. (The change in El (xl "&1

> .;~

..... 0· ... "" --.-.~~

p,~ •• '

',,:-7·-:·:-;:---:·-~·~··---

-.~ '.~ . . -

I ' j . ". , ,

~ IJ t;

J.! . .- . ...., .. ~.--~ , - :r t:oo-

I I I I I I I 1 "I

I I I I 1

1.8

1.6

.. -- .

1.4

1.2

1.0

XL ~ .. ~ .8

.6

.4

.2

x

.. __ .. - .--.~- - _. '--'-'--- --:--.--.... ~-.- .... ~------'"!'

Page determined to be Unclassified Reviewed Chief, RDO. WHS lAW EO 13626. Section 3.5 (Jatl: JUt 19 D

. ... -. :.::.'. ~

Figure 2. Z. Contact Enersy Ei (x) v.. Compaction Parameter x

Z-8

Page determined to be Unclassified RevieWed Chief, ROO, WHS lAW EO 13526, Section 3.5 Oatl: JUl 19 D3

I .,

(

I .~ 30.0 . I I I I

~ u

I rail . X

I w

I I I I

Compaction Parameter x

I I Fiaure ~. 3. Contact Ene rsy Ec/x) and Compac:tloD Eae I'll

E(x) va. Comp.ction Parameter x

I I

Z-9

I I I I I I I T

Page determined to be Unclassified Reviewed Chief, ROD, WHS lAW EO 13U8. IHUon 3.5

Ultt: JUL 1 9 2013

ilDared in the •• calculation.. .ince .ins1. Com.ctl azoe pIl,-ically impro­

bable.) The contact ener,y lCc(x) (from Equation 7) 1. al.o ahown in Figure Z.3.

Relationlhlp between Compac:tion EurlY and Powdar Denlity - The br&Ut den.ity of the powder £01' a. pven compac:tlon ltate Call b. determined la the

following way. Equation (5) Ilvel the frac:tioaal Dumb8l' of particle. in each

energy .tate in term. of th. parameter x. For the 1 th ltate:

1 - 1 - 1 I

Ni/N = x 1! x = Ax • 1 - x

(9)

Particlea in the ith

eaersy state have i contact. with nelpborina particle ••

DeDOte the volume occupied per particle in the i th enerCT .tate by at v • • 3 P

where vp '" T lip is the particle volume. The total volume for N particles i.:

.!. - 1 Vex) '" v x 1Z

PI - x 110a)

The bWk denaity iI then:

(lOb)

For the clole-packed !tate (i • lZ):

au .. -~ co. t '" 1 - tanZ f = 1.35.

Z-10

I 'I

,I I I I I I I I I I I I I I

Page determined to be Unclassified Reviewed Chief. ROO. WHS lAW EO 13526. Section 3.6 [Jete: JUl 1 9 20B

, 6 Similarly, tOI' 141"azoe pacldug (1 = 6): &6 = T' • 1. 91 and for hell-packed

1.7&1'. ltacke4 one above uoth.:r (1 = 8): ., =.;. co. t = 1. 65. The latte" arranaemeDt. are the mOlt 100le1y packed array. correapcmdUl. to 1.= 6

anel t II 8. relpectively. The denlelt pac:kiZllI for i = 6 usd i • 8 are nearly

heX&aONl arrays. aliptly eli.placed to open.1x contact. (1 • 6) or four

contactl (1 .. 8). On tbe averaie, therefore. we have:

1 1 a6 = t (1. 35 + 1.91) or 1. 63 and -a • % (1.35 + 1. 65) • 1.50.

The.e valuee are plotted "1. the number of contactl 1 in l"ipre 2. 4;

lince they lie on a lineal' 101-10, cune. it il ... umed that the &1 valuel can

be read from the figure lor other valli" of i. The.e valllee are pven in the

followin, table.

i 1 Z 3 4 5 6 7 8 9 10 11 12 a

i 2.65 2.20 1. 97 1. 82 1. 71 1. 62 1. S6 1. 51 1. 41 1. 42 1. 38 1. 35

By comp1tin, the compaction eaerllY and the bulk denaity al functionl of

31:. lUi implicit relationlhip may be .Itablbb_d between compaction energy

and bulk density. The result. of thes. calculation I are .hown in npi-e Z.5. The dimen.ionle .. compaction e08rlY ZE/Nc i. plotted va. the denlity ratio

()/p p' If E II interpreted a. the enarlY per unit ma •• , the orclinate in

l'ilul'e 2. S can be expre .. ed a.:

ThUl, the eDergy Cor a given den.ity varies directlY.1 (c/dp 3,.

2-11

[i'

f. t

I

I I I I I

....

10 9 8

7

6

5

4

3

Z -~

Page detennined to be Unclassified Reviewed Chief. ROD. WHS lAW EO 13521, ItotIon 3.6 U811:

JUL 19 2013

l~ ______ ~ ____ ~ __ ~~~~~~~ ______ ~ 1 2 3 ..

Fll\1%e 2.4. Volume Coefficieuta 8i va. the Number of Contact. per Particle i

2-12

.. ~ ,"

. _ .. _--_ . . -,--- -. ---'. - --- .. - . 0 •• - ,-- . .

.0' r .. Page determined to be Unclassified Reviewed Chief. ROO. WHS

, lAW EO 13526. section 3.5 - Uate: JUl 192GB

I ) ~~ 2 ~ Maximum Compaction EarlY : I 8

Compaction ~ ~lm1UD Contact EnerlY JII 10 a 9 Eller"

I ,9 8 2E ..

R'i" u 7

I 6

I 5

1 • I :tt

3 J I

I>- Z

I III

2E H

ContAct EuerSY"'Rf '" at (-t;) ! til 10

I ... 9 u

J 8 7

I u 6 • 5 • u

1 4

I ... • 3 a fI

I s z Q

I a.

I ~

~ I FilII" 2. 5. Theoretical Compaction &Jlcl Contaet Energies

vs. Density - Spherical Particles , 2-13

I:

i

~

j

J

1.

J

I I I I I I I I f

Pag~ determined to be UnclaSSified RevIewed Chief, ROO, WHS JAW EO 13620, Section 3.5

lJate: JUl 1 9 2013

Over mo.t of tbe d.D.ity rani. the CODlpaCtiOIl eurlY i. em.el., approxi­mated by the equation:

{ P) 5. 67

!:=l!n~ - • j)p~ Pp

(11)

The dimenaloDle .. contact alleray £un~tlol\ f(-f. J .:t i. allo plotted 1.1\ ,Fil'U'e Z. 5. P

Comecti011 St1'UB &8 .. Function al Density - The compreuive Itrue

requl1'ed lor compaction can 'be found bOJr1 the compaction enaJ-IY by equatin8

the work doa.e by the compaction atrees to the chanae in enerBY between den­

.ity .tat .. PI and P2, >1»1' Conaider a unit ma .. of pawdar. contalaedlD a

Imooth-_l1~d cyUnder of crol8-.~cdonal area A. If:lt is the depth of t)'U~

powder. PAx '" 1. O. Now, if the powder ie compacted with a -maath piston. w. have;

c Adx = -dE

or

'" ::\C t :p) 6,67 (lZ)

The tbliloretical compaction relation.hips shOW1l'lnJ'taure l.5 and ex­

pres.ed by Equation. (11) aDd (12.) are very similar to experimeutally

determined compaction characteriatic8. Both the theoretical and expIiIl'imen­

tal re.ult •• how & very rapi.d increase in compaction enerlY (or applied atre .. )

2-14

·. r t

. . .j ..

1" 0-

i

I 1.

j

1

1 I I I I

J

Page determined to be Unclassitied Reviewed Chief, ROD. WHS lAW EO 131528. SectiOn 3.5 lJate: JUl 1 9 .,

with iDCrea.in, bulk denlity. Thh characteristic .troupy ImpUe. that

Ihon-range interparticle patenttab havliI a dominant influence Oft the com­

paction proceal. The theory alao indicatel 1hat the compactic:m enarlY In­

cre ... es rapidly with dec::reaaing particle dianu,ter. For particlu In the

micron lize range, the contact energy-sbe relationlhip is expected to lie

lomewhere between an invel'8e .aconO or invene third-power law. It fol­

low. from thia that the beh&vior of powd.er. i8 determined larlely by the

Im&llest particle I in the particle size di.trJbution.

2.1. '1. 2. Cieneral Behavior of Comectable Powc.t.r.

DuriD, our study of the behavior o. elry powder. several theoretical and

empiricaflaw. have been adv&Uced to describe the compaction characteriadc.

of dry powden. Theae law8 tn8y btl .tated as foUows:

1) The compre .. ive atrell required to compact a powder to a cleneity pcan be expre •• ed by an equation of the form:

a = kj)m (J 3)

where k &nc:l mare CQ1lata.nt. for a liven powder. 6

2) The sbear reabtance Tc of a powder undergoing ccmpaction is PI'Oportion&l to the applied normal (compressive) stre.s on the shear plane. IS n:

Tc - TO = Cfn tan " (14)

The angl. " is a consta.nt for a liven powder; ,. b the shear resiatanc. of the powder in an ancompactgd state.

3) The shear strength ot a compacted powder can be described by the equation:

't:: f1 tan" + b~m . n (i 5)

The firet term on the right.hand aide of this equation can be relarded a8 an effective "frictional" 1'esiatance. whU~ the •• cond describe. the effect of cohesiOD on the ahear atren(lth.

..

I 1. 1 I

I .

-

1 i , ~.

. . .," .

The COMtaDta k aDd III ma.y be fOU1l.d from the huttTOft compaet5.OIltJtllt.~ 6

the coaataDts " aDd If are obtalDed from direct Ihear teet •• 7 The ccmataAt

b is clerived from tho cODltant. A. ,and fl' bi the followiug way- Referrinl

to J1'llU1'e 2.6, the eohesive Ihear component "cob ia aeen to be:

(16)

To define b. we must exprelll CJ n in term. of the density fj. The prhu:lp&1

compaction .tr •• 1 corre.pondin. to an is cr max ~ II n 'ee; "(1 .. l'ilU". 2.6). The stre .. CJ mu 11 related to the denlity tbrouah Eq\1ation (11). Thenfu .... from Equation (16):

01'

T .. " b"m .. A COl' (tan __ tan, l)pDl COn

b : A COl If (tan" - tan,').

The COnltant b ia a mealure of the effects of cohelioD. A 1&rle value

of b implies that a powder will be difficult to deagglumerate after compac­

tion. If b fa .mall a powder will ,enerally be ea.y to deaIPomera.te. For

dilata.nt media, b'" a lince ,. .. "!.

(17)

AerodYD!miC BrqAup of 8. Compacted Powder - The dea •• lomeration of

compactecl Sm pOWder by aerCdynamic forcos has been intensively ltudied

durins thl, ;;01 ram by sublunic wind tunnel tests. 7 The a.bove analysis pro­

vielel 8. b.si. for e.timatinll the effectiveneu of aerodynamic breakup for

different loti of ~ and for other powders. Suppose that a.. small &sslomerate

of compacted powde I' ia sudclenly injected into an alutn&Dl at a relative

velocity O. This reaulte in both shear and preuure streases heiDi applied

to tbe aglomerate. The shear stressel are proportional to U3/ 2 for lamiDaI'

2·16

:1 I

~ . .

..... - .. I . ~ :.. I·,

;. ; !

!: t ,-

, 1.

I 1

!

I 1 I I I J I I I I I I.

J

CompaCtiOll Stn .. :

CJma = 1121 •• e '"

Page determined to be Unclassified Reviewed Chief, ROD, WHS IAWEO\~A26.~ Uate: tJUL 1:1 _

S&reaa R.elationahip ••• Shearinl Occur. ~

Cohellve Sear 8tl' ... th:

~eoh = .,u(tan - • tall ,I)

Figure Z.6. Analyat. of Cohe.ive Shear Strength _ Direct Shear Teat

2-17

-..

-.

~.~:~:~~;.~.~:~~;;~ t U I

I! 11

r L L 1

1

Page detennined to be Unclassified Reviewed Chief. RDO. WHS IA.W EO 13526. Section 3.5 lJete:

JUl 19 D

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

flQW while the pre .. ve .tre .... are pl'OpOnional to the dyII&mlc pr,,,ul'e

Cl = i PaUZ (PI. denotes the ail' den.ity). Th ... IU' ..... are :resi.t.d by

th. coh .. i". fhear strength of the agloroente. expre ••• d by Equ&ticm (17).

At the pcnm 01 breakup, the relationship between critical velocity and powder

densfty is:

For .hear-inciuced bl'eakup

2m T

U = C bZ

/3

" cl'h 1

For pre .. ure-induced breakup

(18/1,)

(18b)

The constants C1 and. C~ catlZlot be evaluated aD&1ytically for agglomer­

ates 01 arbitrary sha.pe. However. the above equations indicate how the criti­

cal Ipeedvaries with clen.ity for the two breakup mecham.ma. The critical

velocitiea for .he .. r and pre .. ur.-induc~ breakup are plotted VS. deDdty

in !'i,lll'e 2.7 for !m. 34~ to illustrate Equations (18a) .. nd (l8b). The criti­

cal o,elocitiea are referred to the critical velocity .. t j) .. 0.4, the primary

purpose bere being to .bow the shape 01. the curves. In eacb cale, the

rapid increase in critical .peed with illereann! del1sity closely :resembl ••

Che ezpel'imental curve for !!a 34Z (Figure 6.3. hlerenee 7).

The ~oretica1 cdtical speed. for ~ 352 .8 compared with ~ 342

have beeD eomputeci as a function of density by u.iftl J!:quatioD (l8b) (al-

8umins pressure-induced breakup) aDA! Equation (5). U8ing data from the

Thirteenth Quarterly Report. 8 the [allowing conatante are folU:ld for the two

Sm Iota:

Lot - II' m A b

34Z 40.6- 37.0- 14.5 10 9 1. 53 x 109

1.2fxlOa 352 42.5 39.2 11.6 2.04 x 10 1. 5Z x 10

m ,~.

H~ I" .,

l. I r. t

r

, ,.

(b)

pb~ 3

2

1

0.4

Page determined to be Unclassified Reviewed Chief, ROO, WHS lAW EO 13U1, I_on 3.5 [Jate:

JUL 19 2OJ3 -

0.6

Figure Z.7. Theol'etical Aerodynam.1<:: Breakup of Sm 342 for: (a~ P ..... ure­Induced Breakup. (b) Shear-Induced trreakup - Critical Speed va. Denaity (Critical Speeds Re1a~ve to Crit.lcal Speed at ~ = O. 4)

2-19

··1 ,

,

I

.~~""~."~-:,-::' -;-::. :~":."~":" !I:.; t .. I .• 4t~;.- . ...; __ . __ . __ _ -::-aa:-", .. :.f'''' - 0". . .. _- _- i4

i,

,. l.~

j

r r. }

. '. '. ----... -.-

Page determined to be Unclassified Reviewed Chief, ROO. WHS

-.-----.~

~ lAW EO 13628, S.ctlon 3.5 Uat.:

JUt 19 m The critical lpeed a. a function of den.ity for the.e ~ .ample. h

plotted in Fil'll"e Z.8. taJriDg the critical .peed tor lot 342 at P = D.4 a.

unity. At the .ame den.tty. there il a very lilniticuat dille renee in cl'iti­

cal _peed for the two !!!! lot. (thi. difference would be even lreater for

ebeal'-iDChlced breakup) at the .. me denlity. !f the two lot. are compared

at the .ame compaction .trell, however. the critical breakup veloclti~1

ar8 not IIreatly dille rent.

2.1.1.3. aellavior en Com~actable Powden at Low Denalti ••

Tbe prec:eMIlI dllcu .. ion hal been concerned primarily with the be­

ha.vior of powden that have been compacted to an appreclable de,r.e. It

il nowwortby that the phenomen& l'upou.ible for compactabUity allO exert

a etronl !nfiuence on tbe behavior 01 "uncompactedll powders, i. e .• powders

which have Dot been delibnrately or knowinlly compacted. (Conlidf'l'ablp

compaction may oceul' DY the weight 01. even a thin layer of powder.) Elec:­

tr08tatic or molecular interparticle forcea may often exceed the maa. 01

lndivichaal particles, l.&clinl to very high local aXlll •• 01. repo •••

The behavior of powder. uncleI' thel. conditione can be viaualized 1n

terms of the leneraHaeel shear etreDlth relation.hip expre lied by Equa­

tion (14). Thi. equation it plotted in Fiallre Z. 9 for emaIl valuea of an.

The key factor in tbi8 equation. as far a. uncompacted powder. ia cODcerned.

ia the iDitlal .hear atrenath 1'. This is the shnr .trenlth of the powder o In itl "natural" density state. When a. p:>wder ie compacted l' a ie ulually

ull1aible compared with the compaction .hear etAllIth 1'e. However. for

an uncompacted powcler this term may be large relative to the weight 01. the

powder itself. Thll fa illuatrated by tne followinll analysis.

Consider a UDiform layer of powder of masl m1 r.rama/cmZ restina on

a rough plane surface whtcb is lnf.t1aUy horiaontal (aee Ft,uZ'e Z. 9). Owing

to the weS,ht of tho powcler (in tbl. caee very small) the p.lWder layer will

be slightly compacted. The correspondinl shear strength charaeterlettc

z-zo

.~~ 1. ~.

:1 ... ;! -

.. :i.

f;

r r L }

-i

-- ._-'. -'- --- ,. - ---- --. --"--

0.4

8m 3062

0.5

p(,/cc:)

0.6

FiIUr. 2. 8. Theoretical Aerodynamlc Breakup of Two!!!! Lots - Critic:al Speed va. Den.lty (Crttic:al Speeds Relative to Lot 34Z at () = 0.4)

Page detennined to be UnclasSified Reviewed Chief. ROO. WHS lAW EO 1352&. SeetiQ/1 U Uate: JUL 19 •

,". '-;~-

~"""-"-" ~!".~'.-.. :-.:.;. "'-'.' -,' . ",;,,':

!.:::';-:-" .-, ..,.., .' ~'''''!''''':''''--'-...

IJ J i

; ,-

I

s,

Sz

SI

or ~/

//

----_._-- .-. "'.-.. "-------"'1-,,~

Tilling Table Powder Sample

RcmSh Surfa.c=e

m

Fipre Z. 9. Critical Slide Anale ADaIY.i.

2-Zl

Page determined to be Unclassified Reviewed Chief, ROD, WHS lAW EO 13526. Section 3.5 Llste:

JUl 19 201!

Ie ~~.~~

" 1 .. i . :

)~';: '. __ . ,--.. -- . '""'\-....,-.: ... · ... __ ,.. .. -~i •. -- -.~ .. --•..

. , ~--.

j

I 1

1 1 1 I , r J

(includinl the .aects of tompac:tion due to the powder wei.htl i. liveD by the line 51 in Fig\lre Z. 9. Now .uppo.e the .urface i. tilted throqb an

anile Ii the lheal' atrell at the Illmee i. Inl lin' wIlU. the nonnalltrell

i. m l co. S. The locu. of applied .trellea i. thaa a circle ~ in the .tre ..

plot. For the coDd1t1on ahown. the powder layer will not .lide off even at

B II 90". (Thb impli •• that the ~ ugle of repo.e can exceed 90· for

thi. layer.) It we nOW repeat this proc .. s for ma •••• ID,>m rID 1 ' a eerie.

of critical .llde &Dale' will be obtained .. I indicated in Figure 2. 9. U In is

large, the .lide &qle 1. approximately equal to the ebear anile" For de­

crea.ing ma •• dell.itt •• , however, the .lide anile pro,l'essively lacreaael.

Tbi. effect ia frequently observed with ,ranular or powdered materiaI.. In

particular, local all,le. of repole may exceed 90· for material. having an

average &Dgle of npo •• of 40 to 50·. Such behavior 11 obs.rved ia aD_­tr.me form lIIUl ... humid condition.. In a dry ~nvlrollment •• JE"ctrific,;,t!cD

01 powders caused by handlin' (i. e., by relaHve motioll 01 powder particlr.,

aDd of the powder relative to the container) markedly affects many powdf' 1'8.

Even dry dllatant mat.rial. can exhibit coheaion under cBrla..~.n conditions

(e.,., marked CUbe.iOD eflllcts have been observed for magnetized steel

Ihot, havins &Dilee ofl'epoee exceed1ftl 90').

01 cour •• , the intercept To cannot be conlfdered a con.tant fo% a gi""~

pOVtder; rather, it i. a statistical parameter which depe4Cls on the history

of a powd.el' lample. The ,enen} trend of increasing!!!!!! angle of repole

with deereaain, powder mass is Jik",ly to be found tor most powders w.I.tn.

MMD value. in the micron si~e range. If the teeh de.cribed above _".

performed many timel lor a given powder, it it probable that a Ireat d"'1l

at scatter wowd be oblerved for small value I of the powder mas. per '.'nIt

area JDj however, the scatter woold tencl to decrease with increasi.ng m.

Z-Z3

page determined to be UncIaseIlied Reviewed Chief, ROD. WHS lAW EO 13628. SIotIon a.s Ulte: JUl 19m

.. le

.. '.

I

r I

a. 1.2. Current Stuciiea with B,ancl Alent 1JC

2. 1.2. 1. Compaction ChaJ'acteriatic:a

Since !a, lot SCH.63.l091a to be uaed in forthc:omiJ18 night te.ta. a

rlprUeDt&tive .ample of thia ma.terial w&I atuctied in comparlaon with !I lot 11 uled prenaull,. 10 that reali8tlc teat parameten fol' compaction

and dtneminatioft could be pred1c:ted. The comparative atH" danalty 1'1-

lationMip. shown in Filure 2.10 indic:atea that lot SCH.63-109 h .o~ewhat

more difficult to compact than the lot 17.

FilUl'e 2.11 lncluclea the atre .. denlity l'elationahlp for !!I lot SCH-63-

109. lot 11, and asent LX In comparilon with other powelerl stuctied. raceDtly.

Clearly. the generalization that inereaaed eaa. of compaction with lncreaaloa

particle 11&e doel not apply. The PSg embryo a.nd aaent LX have the lars.ltt

MMD but are rar more difflclllt to compact. Theae m.teriala, In contralt

to the othu powder. shown in Fi,ure a. 11, are hi&h1y elaltic aDc1 htlhly ir­

repar in lhap., (Section 3. e'1~ctrollmic:ro8raphll'. The relatlon_hlp bet.ween

ease of elasticity aDd ea .. of compaction will be atudied in detail in the comina months.

2.1. z. Z. Shear Streyth and Ten.ile Strength of Aseat LX

Like the hlghly elastic: powders tale: and egg ernbl'yo. the ten.ne .trength

01. a,ent LX 11 a.lao too low to mea.ure by the lIe,m.nted column method.

Fi,UJ" 2.12 shows the compaction _hear etrenath"of aS8m: LX ill compari'on

with ell embryo. The hiaber compaction shear strength tor a.gent LX i.

con.L.tent with the compactiou data. iDClic:atilll Increaled difficulty to com. pact.

Z-24

Page detennined to be Unclassified Reviewed Chief. RO~. WHS

~~o 11ft 'fr"ii

!r.-v""''1;".-:-J ..... -'~ .• -'~" ...... -.-.-' r 'i::~.,. "," " : -. ,.. .. -.~. [) .• ___ .~~ .•.• '-"' .• _.""' ...... ~ •••. ~ .,_.-.: I

::~; .• -.;: :.:. I: .1

t It -, n

i I J J

!J lot 17

1.0 tS

Figure 2. 10. Compac.ti<m ChilJ"&(;teristica of !!I

Z-25

Page determined to be Unclassified Reviewed Chief, ROD, WHS lAW EO 13528. SeoIion 3.6 uate:

JUt 19 •

: .-: i.

..

~ .... ~.~.:,.~:.~'~'.';~~:~ ~.;;;~;~:>~:~ .. .! •• _---.....---_.

~'::." ... U !!I!/'!'1'W'.,p'_ •• , • .-.... ,,.. ....

11 ).

t

I I 1 "'8 -• J I

• • II Ii

us ~ ... • • tI It ~

i CJ

I'

... - _ .. _--------------

---"'--- "--_._. ...... "'--"-- ----

x 107

1-----+---11--1-+------ -----.. _

O.Z

14_"-"'1'----- !!I Jot SCH-63~109 [Do 4 mic rona MMD)

1+-1---- Typical !!i (lot 17) (6." microns MMD)

Sm Jc.t 342 tr.l> microns liMD)

O. 4 O. 5 O. 6 O. 1 0.8 O. 9 1. 0 1.5 Bulk Density (g/eci

Fi,ure 2.. 11. Compactic.n Charactel'ietic.s of Powden

2-26

Page determined to be Unclassified Reviewed Chief. ROO. WHS lAW EO 13626. s.ctlon 3.5 Uat.: JUl 192m!

., ,

• 1 ,

.At pl'e.eat, mt.lch data exht 101' maay powder. en compre .. in stres.

a. a luuctioZl 01 daulty. It the data were presented in term. ol energy per

unit ma •• rather than compl'e •• ive IItl'e", oue would have more useful corr_laUo •••

'1'be -DeI'lY per IlDit ma .. C&Jl readily be obtabwd .e a function 01 clea-

8ft,. fl, for the powder in que.tfoD •• plot of the lopr1thm of compr ... ive

aU',,, veraus den.ity yield. a .tz'aiSht lin, (tbi. 1. uaually the caee for

.tr ... level. below 107 dyae./cm). Then the empirical equatioD

where "CJ '" compree!live Itl"."

k .. con.tant of the powclf,r

p ,. bulk den.ity

m .. constant of powder, _ the elope 01 the line on a plot 01 log a VI. (1 •

can accurately be fitted to the data.

Beca,," the compaction apparatu.s ehowt1 in Figure Z. 12 of the Ninth

Qla.rterly Prolr ... aeport: hal alway. been ueed with the In8tron to obtain

compactioQ data, it Ie pnlJlible to exprelJl the den.tty II') al a function of

the di.tance traveled by tha compacting platon (X) I1ling the following re­lation:

(19)

P • P o

L !;':% iZO)

where Po :: initial bulk density

L • depth of powder receptacle,

Page determined to be Unclassified Reviewed Chief, ROD, WHS lAW EO 13526, ie;tlon a,. LJate: JUl 19 •

L

~ .... ~,~; :,' •... ' .--'-. ..;... .- . i· ·. ---~ ... -. - --' -.. ---.----~.--.- -"-'~--

• .i.~-=-'.I.&,f'("...$.;...:;~' -.~.,,:" _ .,:··f~ __ '~"~-.:::'~.''''-'' . .,,~- ... ! 11 .~ ... -.~., :~ •• - •. " .....-... -•. - I; CJ r;.~.r-: .. , .. ':::' _. j,

I]

" r I j

; I.

J ..

.. 1

1 I , ..

6

5

Alent LX

Ell Embryo

1

1

O~ ____ ~ ____ ~ ____ ~ ______ ~ ____ ~ ____ ~~

234 5 6 Compaction Streae x 1 O~ dyne_/ ern 1

F18ure 2.12. Compaction Shear Strenith

2-28

Page determined to be Unclassified Reviewed Chief. ROO. WHS JAW 1013128. Seotion 3.5

UI": JUl 1 9 311

,.

I' !~: ~~-= .t ; . . J i , I

-.. ... ,- ...... - - --- 1"1 .1 ~:.:

The two .boy. equatioDa CaD be eombilUtd &lid IDte'l'atecl to yield a uaeful

expre •• ion in eMl'lY (E) pel' sraln (.). namely.

II; m-I m-I S/, = tm=IT (p ~ Po ) •

The elUtrlY of comp&ctioD of !i product lot SCH-63-109 ia shown in Figure

(21)

Z. 13 a. me •• uree! from the c1ata by a plainmeter and a. calCulated from &iua­

tion (3), ua1ns II; = 1.9 x 109 and. m = 9.01. The constant. k and m were de­

termined from i'igure 2.10.

2-Z9

Page determined to be Unclassified Reviewed Chief, ROD, WHS lAW EO 13526, Section 3.5 lJate: JUt 1 9 2DI

! t: I ; . r

20

15

N I 0 ... M

~ .... :!l

I

~ 10 :=.

~ .... >-f.G <II a

5

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

!I lot SCH.63-109

0.4 0.5

USihg F.:q. 21

o Mea.urad from eltpf"l'imental dAta by plainmeter

0.6 Bulk Den.Sty (a/cc)

0.1

Firare Z.13. EnerlY of Compaction of !JLotSCH-63.I09

2-30

Page determined to be UnclB8IifIed Reviewed Chief, ROO. WHS lAW EO 13528. Seat/on 3.6 (JIll:

JUl 19 20JS

" !~~ Ji-!i

fNj- -,- u -~--. I> ..... - - [

r t

3, PHYSICAL AND CHEMICAL CHABACTZlUSTlCS OF THE POWDER P.AR.TICU:

3. 1. Tot&l Stuface Area

Surface are •• lor eSI embryo. a,ellt LX. aDd Ipray-clJoied .a~ch.:rin

Vine mealuTed by the BET adIOrpt1OU tec:ludque. The .eaHer 01 polml

in the i,'ET plot ... weU a. in the a.d..orption ilotberm ••• s •• ted the pol.

sillility of a .y.tematic erl'or of raDdom. magDitude. Thi. pl'ohlern Vial in­

ve.tigated dur!DJ thla la8t quarter thriNah a. .tudy of buoyant forcea. It

iI of con.lderabl. impol'taDce to maximize the accuracy 01 tb1. technique

!tiDee w. hope to me. lure .mall chImi" ill .urlac. area (a.. a barometer

of particle Iracture during compaction) aDd ether maDlt •• tatiOfti of chaD8e

in IRlrlace Itrac:tut"O of particle ••

3.1.1. Study at Buoyant Force Conection

For larsel' 8urface a:real the correction due to buoyancy t. 110t ei,Dif­

lcant. However, a. the .urlace area deer .... e. (hellca, the amount adlorbed

deena ••• ) W. correction a •• um •• iDcrea.ingl.mportanc.. ID thil .twly

the buoyazacy correction haa bean only lor the qua.rta: buckat anclliber that

have bean below the l.vel 01 the liquid nitrogen bath. The additional

buoyaucy ol the spring wa. mealured experimentally with no load in the

qual'ta bucket. At the .ame time the m .. gnitude oE the experimental error.

eatlmateci aDd .ome lource. af the •• error. were located.

The experimental data of buoyant torce .. I a. function ot pre •• u:r. are

plotted in Fisure 3.1. The lin •• are .trailht lince buoyant force II a 11near

function of preuure, but the diaturbins feature i. that the linel did not pal.

through "1'0 but fell in a band O. 1 ma wide (with an averap intercept 01

O. 1 ml). No line pal.ed through zero, or below, a. mlpt be expec:ted.

from random error, indicatlDa the existence of a systematiC: errol' of raDciom

Page determined to be Unclassified Reviewed Chief, RO~. WHS lAW EO 1352','eetlon 3.1S lJate: JUl 1 9 2Ol!

-, f=-'

,. ~ .. -. "

"

f----·

f. '"1 .1

L 1

, j

o

r-----------------------------------~!

. II

i o • o II 1'1\ ..

o o N

o o

lJ 0 <]<1

-~---~---?S q, 0 ~----£!..-..Jo o 0 0 0

Pt

~ &J "=' -511) ~g 'Nt: =f' ::f 0 •• :~ .. Clo!~

'a:: !:! ... rs.

21 .. . .. IIIJ II U II =' ~cQ o • fat: 1'C ~: ~

jQ

....; ,.;

Col .. &, ...

1st

Page determined to be Unclassified Reviewed Chief. ROO, WHS

3-2 lAW EO 13526. Section 3.5 [Jate; JUL 1 9 •

"

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

i j.

malrd.tw:Ie of 0.1 mJ .0. 05 all. The source of Chi. errOJ' wa. fOUDd to be

£rom Ilftina of the apparatul .a the cover of the liquid NZ clewar was .DUlled

alaillilt the clamp boldin. the eample bulb. The clamp was u.ed al a Mler­

ence ao that the level of the liquid HZ would be the same in each run. If

we aVOided touching the clamp with the dewar cover. the pointe to cluater

were lowered w a'bout an incercept of 0.05 In, (correspondiq to Dlovement

of approximately O. 04 mm). A reference point would be de.irable but ex­

perimental diUlcultie. of placin, • reIerence point in the field of vieion are

Ireat. Theretol'e the correction starte not tram zero but from approximately

O. 05 m, (Fipre 3.2).

A. an eample. the effect of the correction and the .ffect of the errore

OIl the data for!!!!. 352 pl'ueDted laat qU&l'ter8 will be showlI. Uaint the re­

lulta £I'om the error analyatl7 the additional error in the expe:t'imental de­

termiraation of buoyant force wae adeled to the reat of the errors.

For the coneetion of the BET data collected. the buoyant force data

.howra in Fipre 3. 2 will have an additional correction for the .,..tematic

error of O. 05 mg. The error is a180 auumed to be the range of the .xperi.

mental data in Figure 3. 1 or :1:0. 05 mg. This will be added to the errou

in the maDner outlined before 7• 01' the error in the buoyant loree is:

[ ~ ~ )1/2 dW'Bf = \IVI ~: 1 + (dc)Z •

The ftret term. ill the error in the buoyant force on the sample. the I·)cond

beln, the experimental error •. 05 MI.

(22)

The new adsorption data are presented in Figure 3.3 alonl with the

normal erro'l' bar •• The area inere.lea from 3.14 *5 percent to 3.76 mZ/s

:1:3.7 percent. Althoup there is an area inCll'ea.e, the deviation cletermintid

before was actually takiD. into account the 'ys"malic error. The previoull

data on lurface area mealurements will be conected in a eimilar manner.

3-3 Page determined to be Unclassified Reviewed Chief, ROD. WHS lAW 60 13521. aeOUon 3,6 LJate.

JUL 19 Z01S

t; .

·~.;;.~ .•• , .-: ........ :\0 .•

-~:;-.~

~.- ...... U D f i

I I I

f

I

N

Q 0 .ar · 93,10.1 :aUvAOna

3-4

0 0

""

J • .. .. J ... ~i

0 1111

0 .;"8 .... -51. ': 11 .. ~ rt= j! ~'S .. 8 '-';2

~l .. rot ft." 8 ~

,.; tot

5 lID r;

o

Page determined to be Unclassified Reviewed Chief. ROD. WHS lAW EO 13526. Section 3.5 [)ate: JUl 1 9 2013

"-,. Jt

~~ !~ n; U~ ; ~ -IJ ·, •.. -,'

:: U .. I

(J

r:

-I

on o

(Od/d - UA °d/d

3-5

'" ! 0 <I E CI

i

at>

Page determined to be Unclassified Reviewed Chief, ROD. WHS

./AW EO 13528. Sectlon 3.6

LIaI,-: JUt 1 9 2D1t

),0 .....

If "

'- . .. " 11

t r t 1 1

t r j ..

1.

The chaD, .. in procedure uece ... l'Y to eliminate the aforemeDticmed

syetematte errorl &lid the experimeDtally determined buoyaDt force aD the

quart. components sbould improve the accuracy of the data. As has been

noticed belore.the data for each lndiYidual l'UD have much l.s. deviatioD

thaD deviation between duplicate l'UJ'l8. We hope to have conected this

.now'toeftable u. to better evaluate smaller chanpa in lurlac. mOl'. reliably.

However. it mu.at be mentioned that the ,ravim.tric Byltem ia belt .uiteel

for particla. UDder 5 to 7 microns because. In thh raAJ". lNoyaDt force.

are .a la~lJe .a the weight adlorbed. Over this raDl •• what ia actually m.ea.­ureel i. the elifference between the calculateel buoyant force anel the obaerved

buoyant force; if the buoyant forc .. CaD be accurately preclicted thi. should

pose !lO problem. The measurement of the total 8Urface &1'8.S of the la1'l.r

particle ,ize powder, or small change I in surface area 1. be. au1tec1 to a

volumetric sy.tem. the only aclv&Dtale bei.n. that the Inaoyant force i. elimin­

ated aDd replaced by the dead space determination in the aample bulb. The

calculation ia a bit more reliable for Imall surface are ....

3. 1. Z. Spray-D:ried Saccharin. Ell' Embryo.aDd A,ent LX

To determine the uppe:r limite oi the BET il:av1meter adsorption method.

the total Burface areaa a£ two loti of spray-drieel saccbal'ln. 13C and 13D.

ware m ... ured. Th ••• puwd.n had a lar •• Whitby MMD (13C wae 8.85

mic:rona and 130 W&I 11 microDs) which made mealu:remeDt of the area dif­

ficult and the UDce&'taiDU •• Ireat. Tha meaaurec1 total IUJ'tace for 13C was

0.78 rr/',.*40 percent and for 13D was 1.06 m 2'S*n percent. aUlo.iuee

were Z. 0 for UC and. 2. Z fur 130.

Figures 3.4 and 3.5 .bow the BE'l' plot of the d&ta. AIJ Is obvioua the

error bare are extremely 1a1'1I8. but in !'igul'e 3.5 the e1'rol' bar. are shown

to be not unl'ealiltlc alnce they lipan the :range of point.. In the previous .ec­

tion (3. 1. 1) it was pointed out that: the mAjor error il the error in the ex­

perimental determination of the buoyant force.

3-6 Page determined to be Un A,vlewed Chlet ROO classified lAW EO 1_ • .ca.......:_WHS Oate: • --.3.5

JUt 19 2Dl3

;; .

,. J1 r I r .

-n ,U

/-

~ 41 \,I .. l

COlI /II

8~ $oN

'g! 1:1 ... ... ...

II II Q II

~~

"'NIfI "''''til J!J 0<10

o ..

s ('t\ .... -0 --a '5: ... '5 u .a 11\

COlI '0 CD 1: Q ... • 0 ~k ...... ",101

gl a" .2~

if ~6J i 'a .. 0 a:

E-4 ~ r:Q .. ..;

t e. ... r..

o ( dId - IlA

°d/d

3 - 7 Page determined to be Unclassified Reviewed Chief, ROO, WHS lAW EO 13526, Section 3.5

Uate: JUl 1 9 •

t .

--...,;.

"" , 01

C-lJ" !!1.~~~ ~ miD'lIl

O:li:a. CD 111 c:.. .... a. CD

c:::: ~ 0 § r- ~=-=r - !!I. CD

- f~~ c.o 9,0 0

g g'Pg ""sc: . ::f:l UtUJi

I l

. -,;

o Po

l.O

1.5

~o

.... , Il. 1.0

a.s

o

b Run 5S

[) Run S6

...

MMD .. 8. 85 ml.crcml Area :c 0.78 rn7./, 01: 40 percent

FiiW'e 3. 5. BET Plot of NZ Adsorption on Spray-Drled Sacchal'w (l3e) SbawiDs Nol'TRAl Error

0;35

~"r:-;l

'.

- -_ ~ -..._--1

:r: T: ":;-:-'-:=-¥~U';"': I , ~ . d I :.i:;;~ If;"1.-,. ~ :'

;,-.~ ....... , ___ 4_ ~ •• _

... :- ,! -I U , I I [;

[

I

i.

This metbocl CaD thu. be uaecl lor approximating the surface area. lor

powder. DOrmally. conlidered beyoncl the upper limite (5 to 7 micron.) lor the method.

In addition to the '!nooth .pheric:&l pal'ticlee at apray-dried aaecb&rlD,

two material. 01 radically diltennt particle Ihape were .tudied. The IU1'­

race &l'oa. 01 the aleDt LX, Fiaure. 3. (, and 3,7, ancl en embryo, Fillures

3.8 aDd 3. 9. were found to be quite wle al were their rulolltie.. Sur­

lace area. of the alent LX were 4,40 ma, ••• percent and for ega embryo, 2-

14. Z m 11:i1 p81'cent. Their ruaolitiel were 6.8 and Z6.8. re.pectively.

The lar,8 ru,o.ity of el' embryo ia in the •• me ranle .. talc 9 • The

difference between the two 18 that talc hal a .mall particle liae, appl'OJd­

mateIy)' 75 to 3.5 micron., wbUI ell' embryo ia larle. approximately 8

micron.. The hip nl,oaity of talc relult. from ita being a very irresular

platelet Itl'tlCture IUtd pollibly having some ma('1'opore Itructure. EI.

embryo. on the otheJ' hand. ie a mixture of ~I'ticle. of widely varyins size,

.ope, and conatitutiODj here, al.o there 18 the poasibility of sOlDe macro­

pore Itl'ucture because of the Iteep ri.e of the <:urve aa PIP _1. There a

i. netliaible hYlterelis in the adaorption-deao1'ptioD isotberm (F11U1'e 3. 9).

However, if the lilica in ell embryo ia of the porous type. a few pores

coulcl be left open which would Bve little volumetric: effect but aUlLment the

lurface area. The extent of IUch .tructure is Ima.lllndeed( jf the stracture

eXist. at all) Since the Burlace area II still quite small aa compared to a

truly porous materW.

A charac:lertBtic .bareel "., both talc: and eSI embryo i. sreater ell.8ticity

at low bulk den,ity- -a characteristic .hared &1.0 by ageDt LX. whoae rUloe­

ity i. much lower than either talc: or ell embryo. In all three cUea the

particle shape. are veryl:rresulal', iNiicatiDi that particle .bape mayu­

termine the extent of e!alticity. A lsl.e rugoaity (greater than 6) with the

absence of Ixten.ive pore structure, .eems to indicate that there will be

much elasticity. The relation, hip between rugosIty and elutiCity- -~rti~\llarly

for hi,bly elaltic materiala--will continue to be investiaated.

3-9

Page determined to be UnclaSSified Reviewed Chief, ROD. WHS

lAW EO 13526, Section 3.5

Date: JUl 1 9 201S

;

r· ... " !', j,

~""'.r .....

J. ~, .. ' r .!. ,. I: "''' ,j ~

" !. I

"

It [!

~~ }

1

. 1.

'" o

t did - tlA °d/d

l-IO

.. -.- ... ~-.... _ .. -

t

.... 11\

! 0

... Q

• II" III III

! ! <] 0

.., .

'" 0 Pt° .... II.

0

~ ... C II

~ s:: Q

~ t! CI 0

~ 0 III

~ '" ~

'a

~ ... ~ .D ,.oj

~ .... . ,. SzI

Page determined to be Unclassified Reviewed Chief, ROD, WHS lAW EO 13526, Section 3.15 Uate:

JUL 19 •

,; !~

Ii '.

J

.1

;t-", ..... . c .•

~~;,: .

:". :C-9-._

_.

-

n IJ

J: , ~ .. f

l

I T

1 I 1 1 I

6: E-I !! -" .., B .

'1:1

~ Q

• ~

J 0 >

1.5~ ______________________________________ -,

O.S

o 0.2 PIP

o

O.l 0.4

.. I lure 3.7. Partial Isotherm of HZ Adsorption on Agent LX at Uquid HZ Temperature

Page determined to be Unclassified Reviewed Chief, ROO. WHS lAW EO 13626. Section 3.5

Date: JUt 1 9 •

\

C­c: r-

--" CD

I

0-:;0

~~~l •• m iir (I)

~l~ foJo1l! ~:!" 2. _ !!I.:::l (D- 8. .::u_ n 00 02:ou ~. CD

!>J~§= OI cn 5!.

III

t

w

~t I ... N

0.12

0.10

0.08

0.06

0.04

o

.... ~ ,

MWD = 8. Z micron. Area = 14. Z na2 lIJ

0.1 D.Z PlPo

O.Run 46 6 Run 47 V aun 48

o Run 49 • Run 50

0.3

Figure 3. ft. BET Plot of NZ Ad.orptiOD on Egg Embryo Showing N01'1Dal Error

'"

~

~

0.4

":ri'~" " , i i

, I

.";1- ~~':""'':'~':

1::=

.~~:I:;:"':".~:

;. - .. -,---,

t '.·1." f I I'

) :

t

j ,

1:

" ..... - ._---_. __ .. - ~ .. -- .. ---- .--~--

~~--------------------------------------~

20

5

o O.Z

o Adsorption -¢- Delol'ption

I.D

P'ip!'e 3.9. AdlorptiOil Jsotherm of NZ on. Egg Embryo at Liquid N&J. Temperatures

Page determined to be Unclassified Reviewed Chief, RO~. WHS lAW EO 13620. Section 3.6

Date: JUl 19 •

---._-- ....

~~ I~~ II"'" "' il

~:'::"" -- ', .. '., , "','

r r f

i

:1: ..

EI. embryo and apnt LX 'both exhibit the adlorption phenomenon first

oblervec1 with the other fl'e .. e-drled material, !!!!8. I •••• that the surlac:.

I.ema quite inacUve. The re1&tive pl'e.lure .. t which the monolayer 11 com­

pleted b approx1ma.tely 0.2. Allo the value of C· In both c:aae. ia appl'oxi­

mately 10. 11 b lntol'o.tlnslha.I thil characteristic holcla for 'both material.:

ell em'bI'VO 18 fl'eue-cll'!ed, but it i. DOt known whether or not a"Bnt LX 1I~

this lIeema to iDellcate that freeze -dryina produeu an inaodve IUl'f&co.

3.2. PartiCle Shape

3.2.1. Shadow-CaaUDC for Eleetl'OD Micro,rae-

Dl\l'iD& the paet quarter we have lpent a conlW8ra.ble amOWlt of time in­

velti,atiDI the techniques neceea.ry for shaclow-caatin, samplea tha.t are to

be observed in the electron microlt:ope. In the I'roc8111 we fOWld it necea­

aary to modify our vacuum aystem in order to [uUlll the requirementl for

Ihadow-caatins witb chromium. The methodl used are almilar to tho.e dts­

CluI.ed by HaUIO and 'by Flacherll •

--_.--.-

In senaral. Ihadow-calting wW ald in determinilll the structure of a

pa1't:i.cle in that the height of the parti~l. can b. obtail\8d fl'Gm the shaclow

l.alth. and the particle atructure in the third dimenlion i. liven by the .hadow

Itructure. Th. u.efulnes. of shadow -casUnl in d'3termiDinJ t:rue particle

shape i. shown by the simple example lD Figure 3. 10 where a ahadowed

cr088 il viewed from the top. It b allo found that .hadow-caltinl can be

uI.lul in 80me C .. lel for eohaneins the detaUs of the lurtace structure.

* C fa related to the average heat of adsorption of the li:rlt layer by

C = exp (Enet/RT] (23)

where C = conltant of the BET equation R. = lIal constant T .. ablolute temperature.

(Equation Z3 corrects the one appearins in the Thirteentb Quarterly Report. p. 3-14.)

3-14

Page determined to be Unclassified Reviewed Chief, ROO, WHS lAW EO 13526, SeGtiOn 3.5

Date: JUl 1 9 2013

~ lI-It: I;,

~--~-- -_.- - .... -":'! ".;' .......... ~ ••..

'---'" .

.. " -. -. - .- '. -- .. ' - ..... - .~., . H

11

I : I )

t -

I

r

Fiaure ). 10. Sketch of Shadow-ca..t Cro .. Viewed from the Top

--- TUDII'ea Filament

FilUa-e 3. 11. Sketch of Shadow-Casting Proce ..

Fipre 3. lZ. Geometry of Shadow

Page determined to be Unclassified Reviewed Chief, ROO. WHS lAW EO 13526. Section 3.S Datt:

JUl 19 2Ot!

.,

: ~ ..... -............... .

~"_--So'l ~,:'. _-:".: ".': .--

- I • "':"'. ___ 0 • _ -_::: .. --_ ..... _- .- ...... "- -......

i 1

r f r I

1 l ... -. j! .. ' l'

t ii l!

:1-1

. -:. - .~'. ----:...~ ..... _-: .' _. ' ___ '. ":.=-c ........ .

Ba.ically. ehadow-ca.UD, i. the .vapoll .. doa 01 a mltal '~om a 'eIl.taDt

.ouc. located at a Ihal10w •• le with I' •• pect to the nl'fac:e 01 tM .ample !IUb.t:r .. te. S.ftl'al metale a .. e .wtable for lbadow-ealtlDt--iac1wiiDl aoltl. ch~um. uUllium, aDd a.l'maDlulft. 11.1111'1 3. 11 FVII a dialram iUa­trat1na tb8 .hadow-castina proc ... (locatact. ill a ftCUIllD .yetem). Metal

i. evaporated frolft .. t"ltea Illalneat that il wO\aftd In the aha,. of .. wi!'t

balket. If tlae pl'e .. un to tbe V&C\1\Un 'yatllm 11 low .noup (a1:Knat la-5 mill

H,) tIse evaporated metal travel. La .tralpt line_ uc1 it depollite. OIl all

.u"fac" facllli tIw Alama.. .alou behind a panicle .W aot Ilcel". ..

Ift.tal liepoeit &all thu8 will be detectecl .. s a "lhadOW" ift the electro. micro -

.cope. The helpt of the pe.didl (1'1.1"1'1 S. 12) ie linn by tha 1'8latloa

h:. 1 tall I. where 1 and • are deteradD64 ,ecnutricaU,.

The .badow-aa.ti .. JWaGe .. r • .,.tr •• a vaC1lWll eyetelll aDd a low volta .. • hlp eUl'l'ent power .upply. The only .... ulnment of the pow .... upply I. that

it .upply luffleielSt power to the filament 1ft order to I'eacb tbe evapol'a&ioD

tllftperature 01 the metal. The V&CUDIIl Iystem mu.t have vacuum pampi

tbat are capable of maiDtainlna .. 1004 V&CU1llll thl'INpout the .vapor.liOll

pl'oc.... It i.limperative that a ,004 vacwam be maintalnecl at all tinle. ,iDee. a. the pre .ft ... inaide the vacuum .y.tem inc "a •• I. the metal :raye

are scattered mora ItI"Onily by the re.tdual .... molecule.. The "IUltlq

.hadowl become eliffu .. (iD aD. extreme ca ••• tJw ahadowe may di.appea&').

Thl tbi"II". of the sba40w f11m 1. detel'ml .. 4 ,"ctrical1, lIy m ••• • uriq the n.lItanee 01 the 81m clepo.lted on. pa ... Ucie. Tbl. e.ble. UI

to p:roduc. fUm. of 4ellrecl thickae •• in allY pvell escperimlat. In ,Iural • .. thick ehadow 81m i. uled to cletenmM Ira ••• t1'Ucture whill thlftJl8l' film' an ••• d to Utel'miM flMI" detail.

3. Z. 2. Ell Embm

The value of Ihadow -castlnl ill dete'l'mimn. the 3-D laNctlU'. of pant­ellil ia IU.drated by the electron miCl'oll'apb. of .u ImbrYD panicle. Ihown

3-16 Page determined to be Unclassified Reviewed Chief, ROD, WHS lAW EO 13628, S~Ii~ Date: JUt 1 ~ _

.-.='.' .. ;

.,::.:..... . ,

" .' .-: ":' - ;~.~~~:.~.~ . . ~.,...~ ..... ..,.'''I,·I .': ..... t:~·~~_ .. !,.:l~~.....J.--.. ~ : n.'I'"..:r~ .• 7-~":~ :0;. ... ,-•..• f.lll't",:~':';;,;;",;· •. t .

. ~~.' ...... ~.' ~ ................. *~:~.~,;~.:i!."~:~·:: ~..:..:'~< ~.:~ .. ' .. , ~!Ft'":'," .•• -,.ot.--.:.,;. ... _ .. ..:.-- I

I I I I I I I I 1 I 1 I I

- -.- - ... ·.7::.-.- :"":"-_7 .-.... -.--.

til npn. 3. n. 3. It. an.cl 3. lS, J'ip," S.U i. of "particWaI' late ... , fol'

it allow. how the fIDe pal'tlcle. of ... embl')'O can have a vel', 100 ••• t:nc­

tuN. Oae can ••• how lINch lDfo~matloD .badow-Claetbaa ~ U one ft .. ,

thl •• pbotOll'apb. whUe lmap-w. that the .badow. aN BOt the:..

Th ••• photo,rap allo point ou.t a poI.lble pl'oblem that ma., aril' 111 the oba,,,vatioD of, filii part;lc1e. with light 01' .1eegon micro.cop": The

lDflueDCIe that the eliepe"llDI FOCI .. may have on \:be appanm: pu1Id.

at7uctlue.

In the photOll'apb. of el' embryo. two eliaper'tlll proce .... aN ... 4. III 0IDe rnethoa the powdel' II ultra.onleally eIi'peu.d in butyl alc:obo1 aacl

theD ,p,..,.d OIl the pld with aD ail' pn (Ihnllal' to a paint 'p ... ,-r). In the ,ecODClmlthoc1. a lmall amount of powder I. placed on a 'I .... ,llele and

thea .'p •••• d (d • .,) by dlecha1'lPnl a 'park throqh the pawM' wltll a tella coU (Ref. 11 J p. 127). The photolraph. of elll .mbryo Wu.tl'&U our ,IHI'&I

ob •• rvaU.a. The dl'Y (Ipark) eli.p.r.ed particl., ar. compo •• d 01 nb­particle. tha~ al'l app"eclably amallu than tU .ubpa,Ucl .. of tile Wyl

alcohol dllp'l'Ied particle. (which tend to lay flat 011 the eurfac:.). Thi.

aUflI-.t. tbat the lubpal'tiC1e. in the •• photo,raph' an actaall., aaloln_tatel

o! vezoy _mall paftic1e.. If till. it the e .... the laz-I.r •• paI'Ue", ObMI'Y.a

with the htyL alcahol diaper.inl method could. be 101'lD.d durilll the .. apot'­

ation of the Ipra., droplete f1'om the ,rid. Thi. prOC •• I wovlcl aLlo tend to

caUl the II1lbpartlc1e. to lie fl&~ on the ,rid surface. al il oba.l'ved. The ultl'a.onlc proc ... could break up the part;lC1e1 of ... embryo &llowina them

to refol'lft lome.hat clurift. t!a. naporatlOD of the alcohoL. We believe that the ~:b, ('park) eIi.panllll method la bettel' for obs.l'viq fiDe partida.,

It appeal" a. tho. the fine pazttc1 .. of e .. embI'YO. IhCN/1l in FilUM.

3. U. S.14. &lid. 3. 15, are eUlea. The •• part:icl •• (iDClwliBI the aubparticl •• )

azo •• imila .. in appearanco to pbotolraph' of Ce.b-O-SU (Illiea lo1'lDecl by a

vapor pbue p1'oce .. ) appeariDl 1.11 ReI. lZ. Tho larler particle. allow. in

np .. 3.16 (alia shown in Ilef. 8 ae Yip" 3. 13. p. 3 .. 24) an probably

Page determined to be Unclassified Reviewed Chief, ROO, WHS lAW EO 13528, alation 3.5 Date: JUL 1 9 20IS

~ ... -- ..... ,~

J; .... 4-.:--· ._ .. - , -.--- -

.. ,

1

I 1.

1 1 1 1 ..

I I 1 1 1

Powder Zg Embryo MMD (Whitby, 8. a mlcroa.

Method of IX.per.lon _ ... S;;.IP!=I'.::;k;..;Dl=._cha=r""e. ..... ________ _

(Bhaelow-can with chromium at .. 1 to , heill~~to-1ensth ratio)

Mapiftca.tiOll 28.000 x (microaeope) 2.5 x (ealarpm.allt) 10.000 x total

Micro,raph No. _' .. 3;.,.-_10 .. -..:2:;;:;3 _____________ _

Flaure 3. 13. Electroa M;icl'alrapb of Shadowed Ell Embryo

3-18

Page determined to be Unclassified Reviewed Chief, ROD, WHS lAW EO 13526. Section 3,5

Dete: JUl 1 9 20IS

~.~ ...... .. -... - ~. . . I

l'

~ ,

~. ,. L

I[ ,

r 'j I ....

1 ]

1 I I I 1 'I 1 I I I ."

" ·1 I

----_.- --.-~ - ._----_._- -~--

Powder Ell Embryo 1040 (Whitby) 8. Z miC!l',,1

Method of. DisperaioD Pre ... d OIl arid and Blown off with Air

'Ihadow-calt with chromium at .. 1 to " heipt-to-leD,th ratio)

Malftilicatlon za, 000 x (mlc:ro8cope) ~. 5 x (enlargement) TO, 000:11 total

NacrolrapbNo. __ 6~3~-~1~O~-2~'~ __________________________ _

Ftl'lre 3. 14. ElectroD Micrograph of Shadowed E.I Embryo

3-19

Pa9~ determined to be UnClassified ReVlewecl ChIef, ROO, WHS lAW EO 135.iG, Stet/on 3 5 (Jete: '

JUl 19 •

i I , I I

:i: ,

Powdu En I:m'b~ MMD (Whitby) 8. 2 DllCl'OU

Method of Dllpereion Ulua.oaic nsaperlecl in Butyl

alcolaoli "1'a,.d Oil with air sua

MapttlcatlO1l 28,000 lit (micro.cope) Z. 5 lit ( ........ Dt) 10.000 & total

MicJ'ol:rapia No. __ 6.;.;3;... • ...;,'_.3;..6 ____ ~-__ - __ - ..... _.~-(.haclow-caet with chromiUlb at • 1 to" helaht.to.leulth ratio)

"pn 3. 15. Elecn-on Micrograph of Shadowed EU Embryo

3-20

Page determined to be Unclassified Reviewed Chief, RO~. WHS lAW EO 13526, Section 3.5

Oate: JUl 1 9 D

r~-'-"·~-··· , .. • . -f~ '''''~''.~::~:.::. \: U ,_. '. • .•••• ~_ •• w •. "

r U

t r [

i

1 i

1 -1

T

.-. ____ ._ .• "_.o...-______ . _____ .• _ ...... _~.

Powder Ell Embryo MMD (Whitby' 8.2 mlercma

Method of Dl.p.nion. ..-;;s,.~.:;,;rk;;..;;Dl;,.=.c:,;;;h&=r.iii.,;;.e _________ _

Malnificati01l 100 x (m1crotlcopell x (eftlargement) ZOO z total

Micl'o • .,aph No. _::.:63:,.-;",,:1:,;:0:.;,-=.5 ______________ _

FiJUM 1. 16. Light Microll'aph of Ell Embryo

3-21

Page determined to be Unclassified Rel/iewed Chief, ROO. WHS lAW EO 13121, IlKtIcm 3.5

JUl 19 20B

II

~"'."" .. -~.~­It;r;:-. :.~ :"0

~~~. "":7- •.• -.--- _. -'

..--

i[

I 1:

1 1 1 I I

, 1

compoleel oI1acto •• (innlparent partiel .. , 'I&l'1'OUDdlDl .man .i1f.ea pani­cle.. ne •• la1'I'l" lacto •• particl •• may bav. el. ~m.bl'YO Oft eM lVIac. (thi. appear. a. opaque ponion.).

To celt the above bypothe,", en elftb~ wa. <<It..pened 011 a l1a .. IUde

&Ild theD photol1'aped with the ule of a11Jbt m1cro.cope. The ,llde _.1 chea

carelully placed iD dlltW.d _.ter for 40 hOl&r.. remcwed, and a,dD photo­

,raphad (th •• am. ar8. belq phot0l:rapbed eacb lime). The two photoll'apb'

aa-e .bown in n",1'" :So 15 and :So 11. We .e. that all the tl'aD8pa1'ent pGl'liOft'

of the pal'tlc1 .. are d1 .. olved iD the water; thia .upport. out luppollitloD that

the.e ue compo.ed lal',ely of acto... In the plae. of tIlea. uaDa,.1'eDt

pol'ticml. an left .mall partiel .. (pruumably Imca) and a:rlll' o~ :repon. (po.aibly e,. embryo). We .ee that tbe rernaiDinI .mall particlea

.howo la "1'11" 3. 11 form pa&terne whlch c10.e1y corre.pond to the olipul

pa1'tl.elea CFiaun 1. IS). nu, indicates that the trulp&l'ent pa:rliclu are

dillolved b\l1 not waehad .way. Another experiment dewl'mlaed that approx­

imately 45 perc:ent of the ell embryo powder i.1 water .o1uble ..

3.2.3. Spray-Dried Sacch&l'1n

Some work baa allO been done on Ipray-dried I&cchal'in. Photo,raphl of

thil powder are Ihown in n,UrU 3. 18 and 3. 19. Thi. powder appea1"l to

have ave., lmooth lurfac. and il very epbe:rical. The ,oad epherical llba.pe

i.oI s,.clal intereet since the properCie. of .pheres are ,eMrally much

ealler to .nalyse than the p1'opIII'ttee of powdel'l with i:rreaular .hap.I.

3. 2.4. Asent LX

F1aur.1 3.20 throqh 3.25 now the structure of asent LX. FilUre 3.20 show I the lelleral powder Itructure a. obl.rved in the 111M microlcope.

1'11\&".' 3.21. 3.2Z. and 3.23 sbow lome of the Imaller parUcl •• ob'lI've4

1n the electron microlcope.

3-22 Pag~ determined to be UnclaSSified ReVIewed Chief, ROD, WHS lAW EO 13526, Slction 3.5

Oate: JUt 1 9 20D

-.---

t \1 I~ i: " ,

t!:: - ,.. ... ~ ..... ~ ,. , :- .

i <-

--. _ ....... ,- . -' --.'~' --- ... _---- - ...... _ ... -

Powder EO lCmJnoyo MMD (Whlt~) a. 2 microne

Methad of Dlepenion _.-;;"SpaL;;;;;r;.;.k;...Di....;.; • ..;.dI...;.a;;;.r-lI~. ________ _

(F1QI'. 3. 16 po1l'der di .. olv.clln H 2 0 and cll'lecl)

MapiflcatlOft 100 11: [micro. cope) l x (amug.ment) aDO x total

Mlcwoal'aph No. 61_10_!§1

--~~-------------------------Ftl\l" 3. 17. Lipt Mie1'olraph of Ell Embl'YO

3·23

Page determined to be Unclassified Reviewed Chief, ROO, WHS lAW eo 135a1. Seotlon a.5 Oate: JUl 1 9 ..

u U I :

Meth04 of :D1.' .... ion _....:.Sp'c;:,;Z';,;;k ... Dl_._ .... c .. h;;;;U' .. la• _________ _

Mapilic:atlOft 400 , Cmist'o,cop!} 2 x (.,,In •• meat, 800 x total

Mlcrolraph No. -...;6;,;:' .. - .... 1;:.,1-..:1;,.:;0 _____________ _

3-14

Page determined to be Unclassified Reviewed Chief, ROD, WHS lAW eo 13526, Section 3.5

Oate: JUl 1 9 D

.~;~.-I ~1 1'-I·.·.

II .~

i; .. It !t

~~T·~.~~:.·· . '.'..:.~ .... J.-.' :

: .,..' ... ' . - I' I~ .:. ! , .

... If .;

L r t

L

L

. i

- - -... -.'----~ ~- -------_. - ------

POWde'l' '!pray-Dried Saccharin_ lIOlO (Whitby) lZ nUCt"OIUJ

Method of 018persion Spark Dl.C~!.~I.:..-________ _

MaflDillcatton 11,000 (mieroscope, 2.5 x (.Dlar,emellt) 27,500 " total

WicI'0 8J'&ph No. -.,;6:.;:3:..~.:.1.:.1 • ...;6~ _____________ _

Fi,ure 3. 19. Elel.:trcm Micro,l'aph of Spray-Dried Saccharin

3-Z5

Page determined to be Unclassified Reviewed Chief. RDD. WHS lAW EO 13526. SeotIon 3.5

Date: JUl 1 9 •

ft' .......... ·_· -. - ....;~:-: . .:._'":'_* ___ •

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

I.l

II .'

r J t

J

I

-- ------_ .. ---.

... ., ,:~,'···k~:'·: ~ ".... '1:.#"

.' '. .,,\ '.' .; ,y' ...... , \~ ... ~~..,. ~. • :t~ .. ;.. -a.j

... • • ' • .., \1 .~" \ " .f. _ • ". ' •• '''n . e,. '

~. ~ .. i~i'~I- .;;~ I~-:~'

, :w.., .,',~:....., ~'. . '~~ .. : .~. ~~. ~ .... ~ ".,- t .' ' , , '.... '. '.,' :v6. '~

;,. -:t:' ... '~~ ~.~".' '~}f:"" ~' '...:, . . , " ... ,.. ""

.,. ~ · .'JI.. ' ,,~ -. ,

.,J' , " II ""' t '"'' t" .... . . . ,. ."', , .. ~. ~ ... . • • : - "'\ I ..,. "!II'" ~ -,

~. I?!ti~"'. '.:'" I ... :~~ .... (' ~ .. ~ •.• !. ~" ..;., .~~ .. ~ •. ~ '.-- , '. ,.. . ... . .', .

" ". . I • •• \~ ~ ~ .. ~ :-",' f:,' \ ,-:~ ~,~! -- ........i... •. : • .' ,'. , ~\... .... ~ r r---y."r~.

" It,' : .. ~ ... ~ .... ,.t .• ~-..... . ... Powdel' ",Int LX WMD (WhttbJt • mianu

"' .. &hod 01 Dl',el'atOQ _~Sp&r;:;::;l'k;;;:..:;;DI.;;;';;;dI;;;;.::;:I'~r:::... ______ _

Mapiltcatloa 100 II (mJel'~cop) Z " ( • .a..,.m •• ) 200 x tatal

Micl'o, .. aph No. _6;,;:3;...-..:.;11:..-..;,15:-. __________ _

l-26

Page determined to be Unclassified Reviewed Chief. ROD. WHS lAW eo 13526. Section 3,5

Date: JUt 1 9 •

.,.".'t-l« .... _"'" '. '. ' .•• ~,~' ," " .• f'·:':-·"

-'.' --~ .. -' .. -'

r L.

1 I

i

I I 1.

I

.. _--------- -. __ . -, -'-

Powder Au. LX MMD (Whitby) _..;:;a..::mi=c~rona=o.-_

Method of DiaperliOil ~Spa:cJCIL::~:k..:Di:::.:..=cb&=*,~lo:.' ________ _

Maplfication 47g9 x (pdsro,cop.l Z.5 .IS (aNnumeut) 11,700. total

Wic:zoo.l'&ph No. ~6 .. 3~-~1 .. 1..,-1 ... 1 _______________ _

FilUN 1.:n. J:1eCt1'OIl MierOIf'aph of Ase. LX

3-27 Page determined to be Unclassified Reviewed Chief, ROD, WHS lAW EO 13526. Section 3.5 bI~: JUL 1 9 201

, . .

i: t. I _

1

Powdel' AI. LX MMD (Whitby' _"",I ... mllll&l' .. ' ... cm;;:a,' __

Methocl of m.,.uiOft __ 8 .. plO;&;.;';,;;k;..;D1.,..'_C._h&._f.., •• e _________ _

WaaDlllcatiOD 4700" (mic,o.cope) i. , x CeDlaqemeDt) 11,700 x total

Microll'&ph No ...... 6;,;;' .... .-,1-.,1.,..;Z;;.,;;O _____________ _

1'1",,,8 3. ZZ. Electron Micrograph 01 A •• at LX

}-Z8

Page determined to be Unclassified Reviewed Chief. ROD. WHS lAW EO 13526. Section 3.5 LJate: JUl 1 9 2DI

1"-

'\

r L

Powder AleutLX MMD (Whitby) _..;;8;..;m:.;;;;;.i~;;;r;..;on;.::,:;. __

Method of Dilpel'lion _-=5:,c:p:::&:.:,zok::.,:D:;:i::,8;:Cha.:.:::.;1';,s1t,;;8;..... _______ _

Ma.,Difica.ttOD 9,100 x {micro. cope) Z. 5 x (enlarlement) 24, ZOO x total

~crolrapbNo. __ 63~.~1~1~-_Z~1 ___________________________ __

Fl,ure 3. 23. Electron Micrograph DC Agent LX

3-l9

Page determined to be Unclassified Reviewed Chief. RDD. WHS lAW EO 13628. ieollon 3.6 lJate: JUl 1 9 311

Pawder MeDt LX MIlD (Whitby) 8 micron.

Method of Dlapenion _...;Sp&~;;,;;r.:;lt;..;Di= • .;;cb;;;;.:;;I';"E!lI,;. ________ _

Mqnif1catiQIl 100 x (micro.cope) 1 x (eDlarrmeDt) 200 x to~

Microlraph No. 64-1-2 ~~~--------------------------

3-30

Page determined to be Unclassified Reviewed Chief, ROO, WHS lAW EO 13528, Seotion 3.5 (Jate: JUl 1 9 201S

I 1.

1

1 .,

I .

a.o.m (Whitb" • 1liiie"",

Wetbocl til IX.,.rll _ _ .;!P&c.;:: .. :.:k~IX;;.:;._eh::::a::I' .. ,_e ________ _

(., ........ it f!!!!n •• -at ... )

...... caeaoa 100, (mlcroleop) 2 x (ctDlar.eD!!!!!) ZOO. t.aIal

Wicl'OIra", No. _";;;.;;;..-... 1-... 1 ______________ _

Page determined to be Unclassified Reviewed Chief. RO~. WHS lAW EO 13526. Section 3.5 Uata:

JUL 19 3)1

..L

L

The .. photograph. Ihow that apnt LX ia another powder with hlPly

irHplar lhape. Thia ineplarity i. mainly due to the lUle amount of

debri. contained in the powder. Th. cella are not •• ally recogni.ed iD the

dry atate. When the powder ie submersed in water, however, thea. celli

aI's hrunediately ob.nvahie beeaa.le the,. chan,e to a Ulliform liae and. ehaps

that a1'e quite dille rent from the debrie. Upon clryin,. the- .eeUe .,ain blend

ill with the 'back,rO\\Dd. d8bri8; but lcnowlq of their a:ld.tence and appearance.

they can 'be I"eadily ob.erved. The difference in the cell Ii •• and shape W1Cler

wet and dry cond1dcmA is Ihowl!. in Figurea 3, Z4 and 3.25. This challie ~k ..

place npidly upon imrnerlioD in water or dryias (widlLD :& or 3 8ecOllCla).

3,3. Particle Size DietributioD and Particle Denaity

Particle alse diltrtbutillna of !.alut 17. ~ lot SCH-61-109. and alent LX,

a8 c18t81'mined by the Whitby technique, ar., pl' .. entcd in Figure 3.26.

We employed our u.ual Ichedule for Bise aDAlyllil of the ~ lampl.a. For

a.ent LX, compatible liquida and the truo particle delliity were cletennbled

betor. a Ichedule could be calculated. Bensena waa uaed ae the .attlinK liquid

and an 85 to 15 volUMe ratio of benzeu.e to naptha was the diapersins liquid.

SolabiUty of the alent LX in the •• liquid. wa.s negligible u determined by an

analyate of the radiation tl'anamluion at varioul wave lengtha. A true parti­<:1. clfln8ity of 1.34 ,I em3 waa determined by a liquid dbpla.cemeDt technique

u8ing a va.cuum-insulated volumetric flask.

Page determined to be Unclassified Reviewed Chief, ROD. WHS lAW EO 13526, Section 3.5 Uata:

JUt 19 3)13

:.] j

99.9~ ____________ ~~~~ ________ ~~ __ ~~~~ 99.8

1

!i lot 17 " = 1.61

MND .. 6. 4 micron.

Agent LX CJ -= 1. 75

MMD I: 8. 0 micron.

!Llot SCH-63-109 a :: 1.45

MMD :: 6." l11icrolUl

F1sure 3. 26. P&rtitle Siz8 DlBtributioft of !a aDd Agent LX

3-33

Page determined to be Unclassified Reviewed Chief, ~OO, WHS lAW EO 13526, Section 3.5 lJate: JUl 1 9 2Ol!

I I I I 1 I I

- - -- --- ---------------

t. AEaOSOL STUDIES

The prevtou work OD the effects 01 receptacle atlnosphere h\lln1c1ity

upon formation and decay of a8zo0801. ha. been limited to three cas •• : low

humicUty (S percent or Ie .. ), room humidity, ann bilh htlDl1cU.ty C95 perce.

or lreatar). l)Qriq1he fourteenth q,uanet' prOVilions were made fol' the lB­

It1a1 aerol01 ohamber humidity to be s.t to any prescribed level. A .. ri ..

01 ~8. ulin, powdered ausar, was then conduced at !Ditia! chambe,. bumiditie.

coveriD. the full ranae of 0 to 100 perc:ellt. The re.ulU of the •• n.na are

discua •• d in the present report.

4. I. Op!rat1y Procedure

The operating procedure w .. discu,led rather fully LD the 'Ihi:rteeJith

Quarterly Report. In the present quarter the powder .ample handling. standal"cl­

iaation of the optical sy.tem, and data reduction were exactly a. de.cribed ill

l.eCion. 4. 1. I, 4. 1.3, and -t. 1. S. respectively, of that report. Further-

mOl'e, the powder-diapening procedure wa. the lam. aa that deacribed in

the paralJraph on ''humidity runa" in eeetion 4.1.4. The HZOOI01 chamber

humldtty control &nd mealurement, howevel' •• el'e different.

Chambel' humidity wal controlled in the pre.ent work by connecttna; a

fluBbinS a1'1'ansement to the chamber. In tIlla IYltem. air waa either bubbled

throulh a water flaak or pa. ... d throllp a deliccant bed Mlore being uled to

fluah the aeroaol chamber. The changinl chamber hurnlcl1ty WIU then contin­

uously monitored by one of two methocb; when the de.ired humidity wa. reac:hed.

the coadltioniq .yaqm wal _hut down and the run initiated.

Chamber humidities low ... than 70 percent were meaaurl" by an iJlfI'&l'ed

hYlrometer which aample" air from the chamber tIlroup a lonl Copper tube.

Thia method wae not applicable to hiahel' humiditi ••• probably becau .. of

water conden •• tion at c:old apotl in the lampliq tube. ror the higher bwnicli­

Lie ... rne.aurement. were made by me.ne o£ a p.yc:hrometer inltalled in the

4-1 Page determined to be Unclassified Reviewed Chief, ROD. WHS lAW EO 13526. Section 3.5 [Jete: JUL 19m

chambe ~ ne.~ the fan. The p.yc:hrometric method ia bettel' '\\tted to the

meaBUr.ment of hilh humiditl .. ainc. eno .. , it any, will be ID the direc­

tion of too hip nacU.n •••

4. Z. E!perimental Wo~k aDd aeaulta

A .eri •• of r\lll. at varioue chamber humidities was cOhducted lor pow_ dered ,ullIor .ero.o1.. I'h6 aia. analyaia at the powdered IUIAI' Jiv ..

MMD • 5. 8 micron.

Os. 1.74.

The numbelt mediaD diametez(NMD • d~ of the lample may be computed from

(24)

we obtain

NMD ;: l. 3 micl'on •.

Figure. 4. I, 4. Z, and 4. 3 ehow the aerclol "half-lile", initial ampUtucle,

and "slope index", reepectively, of the v&rioua runs plotted alainst relative humielityof the chamber at the inception of the run.

It ie a.en iD Fipre 4. 1 that th. aeroao1 half-lU. incl' ••••• UDilonnly

with humidity from 5 min a.t low humidity to 7 min at the hllh end. The In­

ereaee 1. thua 40 percent ove" the raDS.. The ec:atter of the data. la quite

IImall for thi. type of experiment. Thus, half-lite ia an aeroao1 parameter

that can be detel'mined expe rimentaUy with acceptable pnclaSon. We ,hall

attempt to delve into the lIilnificanc:e of thia pa~amet.1' in section 4. Z.

4-Z Page determined to be Unclassified Reviewed Chief, ROO. WHS lAW EO 13528, S8ClIIon 3.5 Llate: JUl 1 9 2Ol3

I ,

"IW 'aJrI-nVH

g ..

a-

1 :II

101

k l .I

:d .-• r::I

~ ... .. .. .;.1 - I '0 ~ ~'B :!

:I: -a oi • 2 .... :! ~ II ~

...: .. 0

i Cf'I

... It.

2

Page determined 10 be UnclaSSified Reviewed Chief, ROD. WHS lAW EO 13526. Section 3.5

lJate: JUt 1 9 •

C) 0- GO I' ~ .r. ,. ~ . 0 c:i c:i 0 0 0 0 ... aplUltdwv IvnlUI

4-4

i ) ..

.. l sl Ii >

a i ... ~ :=

~] t 1 VI

1 ;i N .. II .. j IIf

0 -0

0

0 0

Page determined to be Unclassified Reviewed Chief. ROD. WHS lAW EO 13526, Section 3.5 LJate: JUt 1 9 2DB

• •

•

4-5

f .. i

... 8

sJ Ii tt-

I ., ... GIl

r: '0

=) • 0 .. < ..

= oS s1 j ~ • IS

..; .. " ! i;

0 -

,Jage determined to be Unclassified Reviewed Chief, ROD, WHS lAW EO 13526. Seclion3.6 LJate:

JUt 19 20IS

'( J..

The aero,ol initial amplitude i •• hown in J'il1U" •• 2, Tbi. pa~amete~.

too. exhibits &ccoptabiy .man .catter.. It iaerea'.' .~ac1ua1l, &lid .uol'ftlly

bOlD law humWty to about 70 percent. theft drop. 1'&ther .ha~y at 85 per·

Cflnt. The cu~ve.c:ou14 have been draWl!. to iDdicatil I. pS'eclpltcN. drop fum

0.45 to O. 15 at 85 percent. The fact that it i. drawa to iDclleate & .. amootb

rell-aff reOects tbe belle! dlat powder properUu (aDCi, theNfpr.~ aero.ol

parameter.) chanae l1'adually··not d1,c:oD'tba~l,.--wltb hurnicl"y.

FlguN. 4. I and 4. Z m., be cOtnpare.-J wlth Fl,"NS 4. I pel •• a of the

Tbbote.ntb Quart ... l, aeport. (For compal'l.on P"l'po .... Will may take

12 I HzO/m3 • 50 percent s:elative humicl1ty.) . Half-Uve. CompaN q1Iite

[I.vorably, bu.t there i. a .ipificaDt diUeNnce in the initial amplitude. The data on Udtial ampl1tw1e .ecured during tho Chi~.Dth q_rtel' reveal va1ae. &bout: Z-11Z times tho.e .ecured dUl'iDi the fOUI't'.4nth lllIartel'. Thi. till· fer6nce 1. po .. lbly attributed to the fad that tile "lAI! ua,d , .. the preYi ...

pel'iod _a. ,ro1lDCl in the winter (10 percent laboratory I.. H. t. wheNa. the

,ular uaeel durin, the current quarter waS ,round. durih, tile .umm~r (50 pelt­

ceDt a. H.) l'esultill. in the poaalble formation ot & few bard a"loMeratei.

Thi. would " •• ult in lowerl111 the initial AznpUtll4e. To overcome tbt. pro­

blem. a facUity iI beln. conetnc:ted to pennlt ,rincl1nl of the powclen 1ft • eompletel,L controlled almo.pilere.

The aerosol paraaneter "a10pe index" is IhOWllln Fl,ure 06.3. This par­

am_tel' eeamed to be well behaved in the rauF of 30 to 80 perceDt. de­

eNa.illl ovel' that ran,.. A 8bar, "pwaN 8wlD1l. indlcated at about 85 pel'­

ceat.

In this .eetlon.". sball Attempt to look more deeply into the 81.Ullcance

of the val'tou. aerosol parameters. The analy.is is ba .. d CD the tlaeoretlcal

model for the opti.cal pI'GJHlJ'tie. at a ~bu1eIlC-decayin •• nODalpomeratiq

aerolol fir" discus ... in sectioD 3. Z of the EilhtbQu.rterlya.port~3 Senne

4-6 Page determined to be Unclassified Reviewed Chief, ROD, WHS lAW EO 13526. Section 3.5 /Jete:

JUl 19 201S

air-ct. 01 the madel were fIlrthu dilculaed 1ft the Nladl Quarterly RepoJ't ,1'CtioD 3. 3) &All the wbole copic •••• uinmari.,d ill !non coac:l.e 10l'1li f.a Appendix A 01 the Eleventh Qua~terl,. .epol't.

The model fol' the optio:al propel't1e. of aD &81'0101 al.\UIl', that at .ome

bdtlal Um. til. a"olo1 patti.cl .. are wdfol'mly (within eu UmitatioDi of

Itati.Ue.) 4iiatrilnahcJ thl'Ot1pout tbo c:bamber an4 .that the ,i •• c1lltrilNtiOll

at th. abbol'llI paJ"tlc1 •• CaD be '''lIlde1,. repre.eDCed by a los-aoz-mal cUI. bllnatton. Pr •• wnably tid, diltributiOD i. elo .. 1y related to aae aemal .la, di,tribution ot the powder.

lot a

SQl1.

c

LOI Diamet ...

SUppolinl, ill the dialrUD. that the line "an il .. actllal liM •• trilNtloa of the powder l&rnple. theD 10 .. ollar,e II$ntc:lea to chambel' waUe clul'i,.

thl diaperalq pIIa.o would yield the Ua. "b" a. tb. hdUe1 airborne .l ••

di.tribution. If Incomplete lepal'alloa 01' .. apiel "oalllamoratioll preclude.

the appell'ance of filiI particle. In the lnitialu .. o.ol. Uu "c" .ouW reMt. Othel' comb1slatloDe a .. 1 pOI,iMe.

4-7

Page determined to be Unclassified Reviewed Chief, ROD. WHS lAW EO 13526. Section 3.5 [)ate:

JUl 19 2.013

.~

",

The model for ftODalllolllel'&tI.,. tu.bu1ent a.tUlna furihel' a ..... . that the ccmc4uatrat10ti of· &no.o1 particl .. of ., •• el& •• "d" dec ..... " .x-pouentl&1ly with Ume:

wh.re "d) = tuminal •• tWal velocity of a paz'tlClle 01 dla.te~ d

H = chambe r helpt.

(15)

Th. allw due to the acatterllll of lipt by a .iDlle particle in the .catterlq .0 .. Ie

S (eiDlle,.rth:le) = raG !J(d)

I. lilht beam lnten.ity in photometer unlts/em!

~Q = IB.nn.tric factor

CI(cI) .. crlMla a.ction of particle 01 "lametel' d fol' 90-acateeri ••

a.au1te quoted in Appendix A of the Eleventh Quarterly Report ahow that

(d) may be approxUnated by

dm ate!) = T: 1ft, K = coutant •.

In the analyaia to follow. we took

M = 1.6

,OJ K = 20

(~i. in Iquar. micron. if d ia in microns).

(26)

Page determined to be Unclassified Reviewed Chief. RO~. WHS lAW EO 13526. Section 3.5 (Jate:

JUL 19 20JS

Who thea ••• aumptiOll8 are eamblaed ... th. neenaa,", 1fttelntt.oa pulormed, it ia found that the initial a1aul amplitude So 1a "laW to the initial auoH! p&l'ameteu d. aM If I Or

where Cia concentratioA of the initial "I'oaolla pal'tielea/ec aDd So h tha

volume of the aeatteriAl .OM. n. time clep.lldanee 01 the eipa1 S II PI'8-cUetecl to be loa.normal:

I I :i 52~. ___ : _____ _

:s I J

J l'~ --L _____ 1 ______ I ... I I I

I I I

til

The alop. l'Ddex 1= ttl/t') ia a fwlcCioft of 0, aloll., •• ebown in F1Jlll'e A.]

of the Eleventh Quanel'ly ltepol't. The hall-Ufe til & ia related to the lnIClal •• ro.ol pa",ameter. by

(28)

Page determined to be UncIaaeIfIecI Reviewed Chief, ROD, WHs lAW EO 13526, Section 3.5

LIlli: JUl 1 9 201S

1

I ....

0. 01 the limltadolla of the aeroao1 .ettUDJ ezpaoeliiOD ia that it clo .. not

take luto accoUDt the unknown 10 .. of aeroaol pal'tic1 .. by lmplnpan .... OIl

vertical wall.. COl'l'ectioll fol' thi. wo\Ucl ftOt di.turb the nlaClCID fol' the .10pa i_x INt cO\llcl chaD,_ the ball-We n~ttDil by •• mllch a. 40 por­

cent. The eli calcul&tiDD. by that relation .1'8 therefore .pt to 1M too btJb by 10 percent.

The lboat ltep in the reductioll of data .... to detel'miM the ,eometric

.t&ndard deYiatfon tI, of the initial &e 1'oaol.. Th .. e ",e re lound tram ch.

me.8'Qftci .lopo huH c •• by meana of the .rapbtc relation between the two

quaAtitl... The l'uwte, plotteclalun va. chamber hwnlc1lty, are ehown

ill riprs 4.4. The .catter in tid. plot. which of eoa"ae r.flect. the acatter in the mea"'l'ed .lope tZldic •• , ia unfoftu1l&te bee.la. 01 the key role pI.,.cI .

by a I tn latel' ealculatiolll. We cominue. how.ver, aDd .... au JudlDlent

on the credlbtllty of let ... I"aph.. I'DI' CODlparillODo in Ftlal'e 4.4, it wlll

be :reeallecl that tbe OSD of tb. aUlu umple ita.U wa. 1. 74.

Onee the IZ ,'a are kDowsa we ma, proceed to tbe inlUal ael'o.ol d , ' From

the relation

(19)

The half-Uve. &ad f1~'e determine the .ettllq velocl". Stoke'. relaCion then

.peeWu the ell'.. 'fhe •• a" .hown in FilUl'II 4.5. We IlOte fb.t dlat the

d l ', 81'8 somewhat above the count median diametel' 01 the powUl'. This I.

110 doubt •• ift part to the bd'latioft of d l value. by virtue o! lmpiftlement oa

wall.. 'but ~11. faetol' should be con.tant aero .. the hwnWty ran.e.

The change of diameter with bumidity o~aht, therefore. be real--a~p

the .eal. may be too high.

Page determined to be =ssIfIed Reviewed ChIef, ROD. lAW EO 13526, SectIOn 3.5

uate: JUL 1 9 2D1S

-'

;,.

I • -." .. - --• -- ...... , ...

I ' / \ -,/

I r

I

-4 I • I'

/1 ! I

,.' f 1 •

•

8

4-11

•

D 0 ...

... i ~t 'D! ~I C! ..

CI U ... (,I •

~f li:

J 11 c!J1

~j 'O~

i 3 0 ... .. ..

0 5 fOI • -fie

0 ...

_0

Page determined to be Unclassified Reviewed Chief. ROO, WHS lAW EO 13526. Section 3.5 Uate: JUl 1 9 2013

." I:'

, ,

.~ .

. 1

j )(

f,

,,-- -.;

~

I

• I

.;

I I

,/

x x XX

4-12

8 ...

j ~f

J~ U Sf .. i= 0'" o ~ c!0

"'J -u! $d ~.t

u

~ aft .. :: , ... r..

o -

Page determined to be Unclassified Reviewed Chief. ROD. WHS lAW EO 13526. Section 3.5

Uate; JUL 1 9 •

1

J'tpl'8 t. IJ b .ua-pri,lll1, Oa the ba,'a of I'I"",e -t. 1 &lODe,. one I.

tempUd to m&b tJI •• tat8mellt that tIM "typical panicl •• i •• " (Jiot cl.arly

daRned) elec:n& ••• with lftcNa'lDa hwm.41tr. J'llU~. ".5 ladlcate. a more complicated behavto~. In fact, J'tlure t. 5 allow. that cia (which 1. a Ie ..

amblauoua mea.u.re o£ .tae) iDC~ea ... with lnc~aa.lDl hu.mldlt, over much of the nul". thea drop •• ha~l, at 85 pes-cent.

The lDleD.ity of. the vel'tiea1 Upt beam ha. been mea.UNd '_eUon 3.1. Z. Tenth Quarterly lleport,lfnd fcJUDd to be

and the loUd antle .u'btended by the detector i.

'" -3 1lu = 5.88 x 10 •

The volu.me of the Ic&tterm, aOlle 1.

Th ... data. topthe .. with d, ' CJ I &IICl the initial al,lI&1 amplitude. elatel'_

mine the initial auolol concentration C. C la plotteclln I'1P'" ... 6. Thl. quantity t. rather conataDt at 1000 paniclel/c:m3 over she humtdity I'&np

of 30 to 70 perc.at but falls off at elthel' aDd. of that n.... 1'11\1" t. 6

beau a clo .. I'ea.mblance to the inlt1a1 .lanal amplitude (FtlaN t.2). Tbi. justifiea the 100 •• ic1entification between the two ,1IUlUteI a. made in the paat.

A final calculation determiJIIB. the rna •• M of powdel' airborne in. the la­llial aerOlo1. M II alve. by

4-13

Page determined to be ~;SSlfied Reviewed Chief, ROO, 35 lAW EO 13526, Section •

LJate: JUL 19 •

~

\:

•

•

•

• •

\ • •

0 0 g g Q g " • r-... ...

tu,uodslQ .I.~J. uyw t :J3/ •• 13",,-d 'ON

4-14

I ...

f ! ...

J ~ 8 11

S >- = .. 1! ,

'i .. ~

0= ~ 1ft .. '0

i l I .. ~

i J

I 3 ... .. z r-. ..

!we

e 0

Page detennined to be Unclassified Reviewed ChlSf, ROO, WHS lAW EO 13526. Sect/on 3,5

Uate: JUL 19 2m!

I

i .1

I

I I

(30'

where V .. 106

em3

Is the chamb.,. volume .ad PI • 1. 59./em3 i. Che puti.

eIe den.ity. M 11 plott.d in 1'1,"1'11 4.7. Over Dluch ~ tJq humidity ranp

(up to 10 percent) thl calculated ma .. I. In the nelpbol'hoocI gf 180 ....

Thil i. impo •• i.ble alne. cmly 100 l'hl of powder were eli.pened tn each 1'Uft.

The fact that MI. too 1ar •• by at least a factor 011.9 prob4aWy me .... thai the calculatld "I" aN too lar,_ by a factor of

1 I (1.9) !""="'m • (1.9) r.t • (1. 9,0. 712 • 1.58.

It Is lnat •• stl .. to Dote 1ft Ji'illlN <to 7 that the lcatter of palms is no

worse (better at low bumldltlu) than in F11ul''' 4.4. ".5. aDd 4. 6. This

II remarkable in that M is proportional to d cubed aDd to &II exponential

function 01 fl.. The scatter tn cr,' cia. and C 1. mad. more acceptable by the lact that W 1, lett more or Ie .. undi.turbed.

Thl curve whiCh belt fit. the data in Flpre 4. 7 II perhaps the .001d

CUl'VI shawn. Thi. CUl've llUlicat •• that above 60 porellm relative humidity, ther. I, incr.aNI dlffic:ulty in ,ettina tho full powder IaI'IlpIe cU.peued and

all'bo",e. It might be noted, however, that--except for the 1a.t fOUl' po~ •••

the cune milhe be drawn on the l.v.l aa Ihown by the dalheclllne.

4-15

Page determined to be Unclassified Reviewed Chief. ROl? WHS IA.W EO 13526, SectiOn 3.5 IJate: JUL 1 9 IRS

•

,

• ••

•

1 ~

J .!I ..

J h I) -j U ,i j =

! I ..: .. I

Page determined to be UnclasSified Reviewed ChlElf. ROD. WHS lAW EO 13526. Section 3.5 uate:

JUL 19 2DI

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1 I I I I I I I I I I I I I I J

•• 111 •••• "

5. DI88ICNINATION AND DZAOGLOMEaATION STUDIES OF STOlUS) !!!

DIll'ilil the fourteellth quarter. teUI were completed to determiDe the

eUeete of ltonl' on the vlabtllty ami c1e ••• lomuatioD of compacted~.

Sample. of the IWUerial",e .. 1 .toNd at temperatur .. at -2 aDd ·23C for

periodl IIp to eix monUl.. The data aM bel .... Wysecl 011. •• taUetical

ba.il at the pre.ent tbne W. therltore. only prellmln&ry r •• u1tl will be

prel.nted ift tid. report.

In "ftual, windl-tunlMl taat. have abawn that Ito"cl .ample. can be eM·

•• Ilo&nll'atecl aa efficiently a. tho •• that aN DOt atoted in \he compacted atate. Mlcrolcaple aWY8e1 of lUtes- aample. at the .tx-month peI'loci

Ihowed that apprmdmately 1.8 pel'c.nt 01 all paz-tiel .. ob ...... d wel'e al-

alo .... nte. INatar thaD "mieron.. The ael'O.ob had pal'tlcl •• Il •• df.­

trUnaUona chazoacterlJlled. by a 0.8 microft MMD aDd a 3.2 OSD. Approxi­

matelya perceftt of all pal'tlc1 •• oba.rved. ."el'l .reate:r than" micron ••

YrQlft the.e data it can be concluded that abcnJC 20 p."cent of all particle.

Ireater than "micron. can.i.ted ol aJllomerate •• & value wbich ia in a.ree­

meat with pNyiouI data o1ltained dvlJW thll proaram. and. ia con.tder~d to be aman.15

VlabUUy •••• ,.. 0« the atorlld. material.lzadica&e that tbe cleeay !'&te

over the .lx-month period to~ each of the tl'eabDeatl •• 'Illite .hnUal' to the

Datlll:'al decay Pate 101' uncompacted!!!!. .tared at -Z3C. It appear. that the

decay rate I. hither clarilll the Eil·.t 15 da,. or .tara._ than durin, the fo1-

lowinll68 day.. ...altl from the .taU.ticalanely .. ' ."W be pre.ented In the next report.

DEClASSIFIED IN FULL Authority: EO 13526 ctlief, Records & Oectass DIY, WHS

Date: JUl 1 9 •

f

L 6. USE OF Day LUBRICANT TO llEDUCE SJDI: WALL nuCTION

IiI the Twelfth aDd Thi1'teenth Quarterly Prolre .. aeporta, work b

:reponed on the ua. of dl'Y lubricantl to reduce powder-to-metal friction

fo~ pl",1 of c:~pacted powdol' Ilielin. luide • tube. Molt of the experi­

menta were conducted with Mhtl'OIl Vapol' talc packed lllt~ 6.lnch diameter

alumilmln ","I. aelw.te with very lItBooth luriace. llldlca&eel that ttu.re

were JU) IltaUlcant dillereacel between the lubricated aDd unlubl'ic&tod ludace.. A ncluc::tloa til lrictloual force, how.vet' , wal oNerved if

,I'&pbite wal applied to the tube wall when nriou. lurfaC8 roulhlut •• con­

dition. e.t Iteel. A pollible explanatioll i. that Iraphite tend. to fill up Im&l1

.cntc:he. UI4 to .mooth the IUlaC., tIlue allowlnll the plUi of compactecl

talc to aUcIe OYer the lurlace with little or no ehearina 01 powder at the In.

tnlace.

In aD eUon to 1e.1"n more about die .lidina phenomenon, an experiment

wa. collduccea in which the talc-aluminum interface wa. eliminated by limu,

tbe tube with polyethylene film plutic before packinK it with talc. Dry

graphlte wal uled between the metallUld tbe pluttc film to provldo lubrica­

tion at thil point. Whell the pluK of powuZ' .... puahed out of tb. tube it .. a. ob .. l'vecl that the plaltiC liJlllr llid over the Iraphitl-lubdcated ndac.

aDd thare .. al no eUeling of powele .. relative to the plalti.c.

The 1eftlth of the plul of talc wa. 13. 5 iKhe. IiviDI a !.enlth-to-dlamet.1'

raUo of z. as. A forc. of 150 Ib (3. 5:J pli) was " •• d. to compact the talc. 'l'he force .. equired to puh the p1ua of powder out of the tube wal only 18 Ib

(0." p.l). In prior teltl, whe .. e • Idpblt.-l~bricat.d t\J~ wtthOllt the

plaltlc liner waa filled with talc IUId compacted at 150 Ib (3.53 p.1), the eJec­

tion force for. lellith-to-dlameter _tlo 01 ~. Z5 wa. 150 lb--equal to the

compaction force. U it ie ."1Im81i that the .id. wall unit pre"""8 il Che .ame in botb in.lancel (with and without pla.tic liner), then it appea .... that

the prea.nee of the pla.tic film allow, the lZ'aphite to act al a lubricant,

wherea. the ablance of the pl.ltic film allow I th. powder particle. to aome­

how •• &inu.ly clelrade the ability of Ia-aphi'a to act a. a lubricant.

6-1 DECLASSIFieD IN FULL Authority: EO 13526 Chief. Records & Daclass Dlv, WHS Date: JUl 1 9 2DI

I I I I I I I I I I I I I ,

.. ,. The lurpria1ns1y low aide wall fric:tiOD obtain.1i with th4I .raph1u.

lubricated film plalti~ li_~ demoutratea that, by pnventiftl intimate

conta~ ot powder p&l'ticla. with .urlaca. wbeN relative eUdinl mu.t take

place, it it pollibl. to obtaiD a11Dlficant reductions in the 8tde wall 11-10-

Uon.lsoell1ltaace. The pol,ethyleDe {"um plaBtic with Iraphit. lubrication

bn b.en employed in .. tacluUque tor manual loacllDg oi the £."1 8pZ'ay

taDk with JOocl lucce .. (Section 1. a).

It i. conceivable that u iuteriace other tban plaltiC film can be eN­

veloped. to be M1,. efll,::-tive In loweriDi aide wall friction. Such treatment

woWe! b. duirabl, COl' Iyatema where a conti1Noue plaetic: film II objac­

tio_We, aDd thil mat"r will b. livea cODaicieration in plannilll OQI' future work.

DECLASSIFIED IN FULL Authority: EO 13526 Chief. Records & Declass Div. WHS Date: JUL 1 9 201

7. PRl!:PARATIONS FOR. FLIGHT TESTS OJ'" THE E-41 SPRAY TANK ON THE MOHAWK AIRPLANE

PrOIN ... dlll the Hpo1'tina period in the plawn, aDd preparation

for the low-Ip.ed fiiJht triah oC the E-41 Itpny tank 1. l\U1'\Dlariaed below.

L~te til NOYember the Qr\Unm&D Abplaae EnaiD •• riDi Corporation N­

c.incl a.uthorisation to prQceed with modifi9ation. of a Mohawk OV-IC

&1%plafte to permit lly1DJ two E-·11 .pray tank. on tbil airplane. The per­

tinent eDline,rinl data for th' £-41 we .... ent from (Jenera! MiU., lnc.

to Grumman for u •• in maklnl the modification. an. E .. ,U Ipray taDk.

with a .. oelated .quipment lor around checkout ancl operation of the Uft",

.. as shipped to Orummap at Betbpa"e. Lonl bland, New York, early in

December. 'I'bil unit wal filled with approximately 300 Ib of WltrOD Vapol'

talc which 11 to b. di. ... miAa.ted duriftllround checkout at Cil'umman a_

durin. the fiisht trial. at tbe Naval Ai .. Telt Center, Pumeeftc River. Maryland.

7. Z. Manual Techn1,ue for Fleld Loadlnl 1:-.&1 S2-ray Tank with 8,

In connection with the nipt triab of the 1:-41 Ipray caNt on the Mohawk

airplane, th.re w •• a period when it: appear.d that only ODe of the E-41 unu.

would b. available for th.,. triala. The other wit bad be.n Ullt to EI11Il

Air Force Ba_e aDd the time for completion of the Eilln trW. wal indefimte

UIltll late in Novemb.r. With only one unit avaUable for the Mohawk trial.

it would have been nec •• aary to reload the unit In the field. A parUal ehal'"

of 80 Ib of !I would constitute the load. The exposure of !L durin. loadin.

would have to be minimized to pr ..... nt absorption or mol.ture ancl to p",#eat

contaminating the area with!&:

The experiment_ with a graphite-lubricated polyethylene liner in a f.-hach

cylinder with cOMplLcted talc (Section 6) demon,ttated that it Mould b. pOI,IW.

7-l

DeCLASSII'IEO IN FULL Authority: EO 13526 Chief. Records & 0ecIaIs Div. WHS

Date: Jut 1 9 •

1

1

to davelop a packagilll arranpment wbueby a relatively ImaU force woulcl

IIIKftCO to Pllh lbe compacted cMr •• out of the tube ~t bacl beell " •• d to

cOZll!_ it durina c:ompactlOD. A eu1table manual IYltem wa. developed and

demon.trated b the laboratory before it became known tllat acbedul1na would

pennit uling both E··11 Ipra, tank. and that !l1oacliDi in the field would not

be required.

The anUllement which wal developed foZ' lodin, compacted !iii

aketebed in J'i11ll'e 1-1. The wtch Ibowe the eartriqe of powder inaide the di ... minator prior to remcwal of the polyethylene liner aad the alumiINftl

II.eve. The lle ... ia approximately 16.25 inche. in dJ.ametel' 80 t'bat it

aUde, fl"ely lnto the cl1 ... ml .. toZ'. Tlw cegtral tube ia 1IIod to pZ'olvic!e a

hole fol' the dill.minator driw .crew ancl to pide tb. Icrew thl'oup the

polyethylaD8 Ileeve ia the center.

The polyethylene liner h plac.d in the oaluminum clecve prior to 61Ulll

wUh powder. The film pl.etic tube in the c,ntlr ia doubled back on itlelf

10 that the free end i. adjacent to the central tube at the bottom. A!~r the

.,oweler ie compacted in place. the pwyethyleno ia lathered to the center a:ad

tied arOUDci the cenCral tube 1IIi"l •• peelal IUp-knot. By pull.ina 0Jl thi. line

thelmoe can be rele.aed to b •• the polyethylene. The polyathyle_ lillu ia

.xtra lOll, 10 that it can be draped back over the tie cord and the out.ide of

the aluminum a1.",,,,,,. The bottom eliacs are needed to pulb the cartridge

into the dial.minator and Co hold the powder in pOlitlon .. the aluminum

sleeve &lid the polyethylene Uner are wl.tbdl'awfl.

For the loacliq operation the diu.millator i. ~ppol'ted on a rack with

the open end eUted about 30 d..,Ne. below horizontal. The powder c&rtrid.e

il inserted and heW in place 'lihUe the rol •• se line on the knot.~ 11 pulled to

rele ••• the polyethylene. The polyethyJflne il pulled .wa, from the race of

the powder by tu"ir11 at the skirt ol matel'ial extE'ndhll bel."., the bottom eli.c. Next. the tnatel' bot.~om diae 11 remoyecl 80 that th. aluminum aleev.

can be withdrawn whIle holding the powder in place with the inner bouom

dilc.

7-2

DECLAsalFlro IN FULL Auttlorlty: EO 13526 ct)ief. Records & DecJass 0/\1 WHS Date: •

JUl 19 ZOIS

DI".minator Screw Drive

Polyethylene

Grapblte Oil Surfac •• between Polyethylene anc1 AlwninUlft

- Tie Cord with 81lp Itftdt

Powder

Knot Releaae Line

I'lsure 7-1. Packa,in, Arranaemen~ for Hand Lpacliul Partial Charle lor E-41 Spray Tank

DEOLAIIIII'II!f) IN FULL Authorlty: EO 13526 Chief, Records & Dec/ass Div, WHS Date:

JUL 1 9 2013

QI't"U,'i&L c

Before I'emmn, the inner bottom dilc the dl ... millatol' t. tilted to

bl't.ftI the loadlnl end approximately 30 delre .. above honaontal. Tht.

maneuvel' coo a ••• the poweler to .tay La place while the bottom clilc i. 1'8-

pl&eed with the eli".minatol' pilton and hu.b ... embl.,.

The tecJudque delcrllMtd above hal been found to be entil'el., aati.fal'tOry

for loadlft1 pal'tial char •• where the weilht of the cartrici.e doee not ex­

cee' that which can be conveDiently handled by one man: aDd. when the powder

ia Umlted to nonpachopnlc .imu.lant.. The procedure 11 eaay aDd DO epe­

cialloadinsequ.lpment other thaD the compaction pn .. 18 required. The

polyethylene mbdmiaee the expo.un of the powder dUl'iDJ the loadiDloper­

atiOil. The 10a.&Uas cartnd,e is inexpensive 10 that it cCNl.d b. deltroyed

atter lD&dinl to .bnpllly the decontamiutioD operation wheD !!J i. uled.

Th. louin, cartdd,. can allO aerve .1 a .hippinl container if packed in

a sturdy wooden crate.

7-4 ama.a,m oaOLASSI"'!O IN FUU Authority: eo 13526 Chief. Records & Oec/ase Div WHS Date: •

JUt 19!D

SQM"'IDlE P £ Ai

8. Stn04AllY

ThIll "ol'k completed dUI'iDI the fourteeDtb quarter i •• ummarlaed ill the followillJ par&,raphl.

Durin, the courte of tht. project we haye been Itudying t1u. bulk pow-

der p2'opel'ti.1 .ucb al enerlY of compaction, Ihear Itrenltb, and tenlne

abeuath wh1eh are maDifelitationli of interparticle contact eneI'll... In

addiHon .... han I'udiecl powder particle characterilttci auch at sbse and

ahape that affect the number lind. Datura of thet. inte:rpartScle contacta.

Current theol'8Uca11nveatllatlofta relatin, the .. interparticle contact .~rJi.1

~ mechanical pl'operUu of compacted. powder. are delcribed ISection Z).

A theoretical znoclel compo.ed of .ph.rica! particl .. o! diameter dp with an

ayeft.ge oner" • per cODtact la employed to determine the enuI' required to produce a,iveD dIaDIC in average powder denaity. Although an idealized

Iyatem wal us.a. the treDds predicted a,7e in accord with experim.,ntal

claia (Secti.oD Z).

!!I. (lot SCH-63-! 09) to be ueed in forthcomin, flisht teste was 10"'00 to

be more cIlUlcalt to compact than !.I. (lot 17) u •• d previously. A new approach

to obtain the ener" of compaction from Inetron data 18 presented (Section Z).

Alent LX Uk. other hiShly elastic m .. terial. was found to be difficult to compact, has a comparatively high com~ction ahear .trenlth, and. tellSile

Itren,th too low to meuure (Section Zl.

An eva1\&11Uon wal made of tbe bUOyaDt force corrections {or the BET

adaol"ption method to rDealure total aurface area. Spray-dried saccharin

13C and 131), a,.pt LX, and e,. embryo wore found to bave total lurlace

are .. at O. 7&, 1. 06. 4.4, a.nd 14. Z with correspondins rugo.iti .. of Z. O.

Z. Z, 6.8. aDd 26.8. Spray-dried eacc:barin it compo.ed of amooth .ph.,r .. ,

whereat the es. embryo and agent LX ia iii. hilhly irregular'ly .hapeel elaatic

particle aa shown in me microll'l.phe (Section 3). Our method. for preparinl

ahadow-cast lamples for me electron micrt.)IIr.:vpe are deacri.bed (Section 3}.

8·1

..iO,,"1 L'".I OECLASS/PI!O IN FULL Authority: EO 13526 Chief, Records & Dec/ass Dlv WHS D~: '

JUl 19 2m3

(

-A 'Cud, of the eii.ct. or humidity (frQm 0 to 100 percent ]t. H. ) UpQ!I

the (ormation aDd decay 01 a ,round powdeud. ,ulal' a.rolol ia reported

in Se:tiOD.. The data were tbor01Ji hlyanalyzed, conailtent with the teet

parameter. cleellAated h. the method of mealurina aerolol elecay by lipt-

. eet.tterins technique.. The nau1u indiQ.te that pronQW1C:ed c:haq" pro­

bably do DOt occur until the rel.l.t.lve hluJddity ia greaeer than 65 perc:ent.

VlalriUty a.n4 d .... llomeratlon studl.a were cc.nduc:tecl. on aamplel of

compact6d !!!l that hacl beeD etored in the ccnnpacted atate for a period 01.

6 manth. at temperature .. o£ .l and -Z3 ·C. Wind-tunnel t •• u eho-c:l that

th •••• ample. were deaglomerated •• efficiently a. c:ompacted !!!!. that had

not beea .t.ored. Viability a .. aya have not been c:ampletely analysed but

bJcUc:ationa are that eIfIeay rate. for aix monch. of atoras" are .imilal' for

compacted and uncompacted!!!!. (Section 5).

All. expe:rirnent 'Wal conduc:ted uaiag M1stron VapoT talc compacted in A

6-im:h 4lunetel' tube wiped with graphite aJlcll1ned with polyethylene film

pta.tic. The force required. to pUfih tho plug 01 tale out of the ~ube waf ap·

pl'eciably Ie •• than baa been obaerved for Similar plug. without t.he poly.

ethylene, iDdicatinl that aide-wall frictiDn can be materially redw:ed U nit­

able method. CaD be !0I121d for preventing intimate contact of the powder

particle. with the wall aurtace (Section 6).

In preparation for the low."peed llight t:!'ials of tile E-41 apray tank on

the Mohawk OV-IC airplane, an It-41 wal filled with compacted talc ancl

Ihipped to Grumman Ail'craft Engineering Corporation, Bethpage, LonS IelaDd,

New York. A m.anual1oadiftg teChnique using partiAl cha:rges was developed

in antiCipation of having to load the E-41 with ~ in the field durin. the flight

trlal. (Section 7).

8-2

,sg"IIISZA iilL

DECLASS/PlleO IN FULL AuthoritY: EO 13526 Cttief, Records & DecIass Div WHS

Date: JUl 1 9 an!

9. UJ'EllENCES

1. J'etllUn, C. F. Proc. Roy. Soc. (London). ~: 53-89 (1931).

3. Zenz, r. A. and D. F. Othmer. Fluidization and fluid particle .,.teme. N. Y., Reitlhold. 1960.

3. Dari,.,ln, B. V. and I. I. Abdkolova. Soviet PhYI. JETP 3:819 (1956).

4. U. S. Army Chemical Corps. Biological W&riare Laboratories. Technical Memo. 9-ZZ. Mathematical model for eMI'IY of. compaction of a bed 01 powder. by 1. S. Den (November 1960).

5. Lindaay, 1\..:e. Concepta aDd. method_ of. theoretical physic.. Princeton, New Jereey, Van No_trand, 1951.

6. General Milla. Inc:. Electronic. Division. Report no. l~44. Din.min­atian of lolid and ltClnld BW Agent. (Ul. by G. R. Whitnah. Contract DA-18.064-CML-374S. Ninth Quarterly Progre88 B.eport (October 19. 1962. Conflclendal.

7. ---- Report no. 2411 •.. Twelfth Quart"rly 'Progress llepurt (July 10, 1963). Confidential.

8. ---- Report no. Z451 ••• Thirteenth Quarterly Progl'esa Report (October 17. 1963). Confidential.

9. ---- Report no. 1,395 ••• Eleventh Quarterly Progress B.eport (May 4. 1963). Conficlential.

10. Hall, C. E. Introduction to electron microscopy. N. Y., McGraw­Hill, 1953. p. 329.

11. Fileber, R. B. Applied electroli microscopy. Bloominlton. IndiaD~ Umvenity Pre .. , 1954. p. 109.

lZ. White. L. J. and G. J. Duffy. Vapor-phase production of colloidal fmca. Ind.. Eng. Chem. ll: Z~a-38 (1959).

13. General MiU., Inc. Electronics Divilion. R(;purt no. ZlZZ. Diaaemin­ation of _olid and liqUid BW Agents (U), by Q. R. WhitJUlh. Cnntl'~r.t DA-18-064-CML-n45. Eighth Quarterly Prolres. Report (August ZZ. 196Z). Confidential.

14. ---- Report no. Z373 ..• Tenth Quarterly Progrea. Report (February'. 1963) • Confidential.

15. ---- Report no. ZZ64 ... Sixth Quarterly Progre .. Report (February Zl. 1962). Confidential.

9-1 Pag. determined to be Unclassified ReViewed Chief. RDD, WHS lAW EO 13528, StctIon U

Oate: JUt 18m