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UNCLASSIFIfED
AD 2 6 4 841
ARMED SERVICES TECHNICAL INFORMAT!ON AGENCYARLINGTON HALL STATIONARLINGTON 12, VIRGINIA
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UNCLASSIFIED
Best Available Copy
NOTE a oc'~rnor othaer &rarin-gs, speci-:!=atic= or ctber date ar-o iusiPi fcr=- .jny q-oeothUer thaqn in v:,r! + % deflijdte]7 re3AtAed
go~e~ezi pr~~st exaticm, tbhe ii- -:.G--e-oLeret there-by- Incars no respomisib;L:ty, nar anyobligatimn~to~r amd the fact tlhet the 9--rer-=en- may hz-.e fo~m]atted, ftrnisbea, z-- in any va~ysurpjlle-d the said dravings, specfinmttims, or- o-tbhed-stsa is nct to lbe regarded by I-,%Lication or o~ther-
.ieas I.- any7 mm=r l-icens!=g the hole oar anyat-her per-so orm 00! oztim.a ouyray --ri&tor pe==issio to =a~faetmre, =se or swef azpattented invei-aian that =ay In amy uwy be related
i -c T!--- Acce1lt-.%tci Cc rrsof Metals
Da-:-- A
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UNCLASSIFIED
Contractor: Akrmy Chet.iical CenterContract No.: DA 18-108-405-CML-518
Eighth Quarterly R--e=rt
Covering -z-e Perioc
june 16 - Seotember 15. 1961
Ti:le: 'hE ACCELERATED CORROSION OF METAIS
Prepared By
Sen;s. investigator: Henry Leidheiser. Jr.Assc-iate: David A. Jackson. Jr.. Research Chemist
5 Septet.n,7r Z6. 1961
Copy of Copies
UNCLASSIFIED
AST1'Ai- lb
I:-
-. -_ __- ; - __ _- - - - "__. . : . _,, , ,__ _
TAIBLE OF CON-TENTS
Page
ýntroduaction I
Descri-ntion of -Auparatus 2
E&cnerim ental Prc~ce-dire 5
Rescdts and Discussion 7
Exp~erimnents Planned for theNext Qi-arter 355
Bibliagrapiry 37
z -
RiTRODUCTION
In previ-ous re-ports (1). -,he oxidation of aluminum
in contact -with mercuric halides has been studied. and the
influence of rclative bumidi.:t-,r on the oxidation rate was
nctec - In this report period the Al -RgI, system bas again
bee-, used for continued quantitative measurements of the
oxidation rates- The rate .3-1 oxid&tion of aini= ~ a-..
in !:-e presenct- of Hg!, h-as been studied over z reiativ<
hum-iditv range of 36..4-100%~ at a constant te=ýzrature of
30@C.. A great increase in rate of oxidation- has been noted
inthe 60-80% RH range-.
DESCRIPTION OF APPARATUS
The aDparatus described in the Seventh Quarterly Report has
been further modified to in-clude a p~ressure guage (Fig. 1:B 3). which
was calibrated ag--nst the mercuxry manometer (C). This bellows-
type guage was specificzfly designed to measure the small internal
pressure decrease in the reaction chanber; atmnosp~heric pressure -was
the -reference- point. Once the g.-ge was calibrated, thc manometers
were disconnected. and the syste= z-cseaale-d A-!! oi~ f AWOZ
in- this revort are based on prc5sure rea-dings obtainedA !,: this g~a--t-
A pobt.ograen of the entire apparatus is seen in Figure I- The
vacuum pizmp) (J) was used interntittently to check the system for small
leaks. A detailed diagram of the reaction chamber (A) ma- be found
in the previous, reports (I)-
L 3.
-.2
r;;
-- 4.
ITDcs.:riptior of Apparatus for Figure 1
A. Reacucn Chamber
SB. Pressure Guage
C. Wfater and/or Mercury Manometer (:."ow nt i, use)
I D. Barometer
1 E. Conscant Temp~erature Bath Control Unit
F. Fan and Lramnp Control; Barometer ,A-justmcntIndicator
G. Constant Ten. errture f.-W'tr Bath
H. Variable Speed Water Pump
- Variac for Water PFlup
J. Vacuum Pump
3=r
17
IV
I. -
l r.L
~.Z.
: mo, . irlr i ' I ',, ! I I'q 'II
i ,..
EXPMERIENTAL PROCEDURE
Reynelds 99.999% aluminum cylinders 11'2: in- iiameter and 1/4"
thick "wvere degreased in acetone and ether. Exposed su-•face areas of
-hese -.-a-nples rmeasured ;-pproximately 1.25 cmn.
The cmidation of ;-e aluminum samples was initiated by the attack
of Hg-1 vwhich wa-. quici-y reduced to metallic mercury. The manipulation
of the ap•aratus for this is described in prev.;ous reportsjl). Upon
algamation. the oxidation proceeded; the rate berg -rea-ly deter.in- d
by the relative humidity inside the rec-a cba-nbe7. The desired relative
humidities were obtained by pla•ing various saturated - solutions in the
reaction chamber. Both thermal and humidi- e-euilibrium were facilitated
by the use of a smali fan which maintained the inte-rn-a atmosphere in a
continual state of mo-nemnent- Upon reachin-a e-uilibrium. the renction
Sas begun as described above. The oxygen consumed dinting the reaction
-"was "-- easured by the decrease in pressure inside the chamber. Since
pressure was the measured parameter. close temperature czntrol inside
the chamber vas essent-ial Temnperatuxas were maintained at 30. 0OCC+
""a- 0.30 throughout all the experiments. Measuremeats of tim-, te-m--erature
and pressure were -made at 5 to 10 zm-ime irn: -r-als un-il the oxidati.=
S_1_slowed cz -1 - Corzectious necessitated by changes i'-
baxromerric.)ressures were made.
Values of AP in mnm Hg were con'rerted to AWo? in mglcmz2 from
zh I -de follow•.g: vA
AW= T ..
?M;
I1L.,• i " T i l ', i l Jil in l I' II I ii I ll ,,
where VM remained constant tli.rcighouxt the experiments- Values of£ ''Z5R
.... W -xcre p~lotted vs. tim e i.r eac -'ceximn-t an h-lopes of the linear
portions of the curves -- ere determined-
Several satirate-d salt solu-uens and the associated relative humidities
under ecuilibrilum conditions are listed in Table A.
Relative Humidities of Severa! Saturav-d S-altsolutions (41 at 30'%C
Solution R- H.%M
Distillee. wate.: ion
(INII'4)HzP04 9Z.-9
BaCl2 lz- hO 85
(IHL),SO. 81.1i
-2'C O3 72.7
NaNO2 3.0
Br- Na ZHZ0 *56-.2
Cr0 3 +4_6
- Kal. 213,0 36-4
F- Etrapolated value (.2). (3). (4)
irN
I i
R SULTS AND D!SCUSSION
Whereas in earlier exneziments. the linear portions of the
oxida&ion rate curves were us-m-.!v preceded by 1-w-rate induction periods,
IIin the .present . -perintm~ts no g2. eat ;_nduction period seemned to exist excent
in one or two cases at high relative humidities.
By vlo".np --- e --. v-values of ,.Wc, obtained f-om oressure
r-ear--g-s. each rate curve exhibited a ch-nracteristic linear portion from
whic! .he skones -were gravhicaU,, dete-•ined. The slozes of the linear
portions o. !ie -Ate cux ,cs were -?!.:. --:-=- " anIe at any nar-icu1ar
relative humidity. However, as the relative humidity de:- eased, the
slopfs of the rate curves also decreazcd_.. The slopes of the rate curves
are listed in Table B. wi-fth the ex-sting relative h" miditie-s obtained from
the saturated salt solutions.
At low retolatc humiditnic& 64 RH anii bcnaw). thr extent of
oxidation was verv sall, and the associated sloveos fr the rate curves
could ordy be determined from the first few me-asur--r.ents in the 1.0
minute time intervals..
Figures 2 through 7 arc rate curvcs for ex::eriments at 10M R HI-;
Figures 8 --d 9 at 9Z-. 9 R.- ; Figures 10 through 12 at 81. -5 R. N.;
ig•u•res 13 thir-.ough 16 at 72. 7% . H-; Figures 17 through 20 at 63%R R H.;
'Figures Z1 through Z6 at 36.-Z , R.H.-; Figures 27 "h-ouig 30 at -4.4- 6 R.H. -
Figures 31 and 32 at 36. 4% R.H. Since th, variation in the extent cA
' xidat= -w-as wide, three diffement scales were necessary to plot accurately
the oxidation time curves.
..... . ... - - - -
a 1 8.J
TABLEE
Values z,.r the slozes of oxidatý: rate curves~ at d~iferentrelative humidities at S3541e-
SaI. -d alt Relative Sic~pe(mn) Ave- Slope (i±.-sohutzon used Humidity ro) MFOIcn 7nr. mOImlii
DiL~dWater 100 *0. 630
it 0.570020-622 0. 6141! 0- 616II0. 59 1
2: it0p567
22 0. ;66
0-566 ~ 0-583BadI7,>.. 2Ho *0-613
222 o-556 .5.1 ~~*0-565 0 5
81.1 0.o-5A4IS 2.*0-515
U *t *0 = 0..520
H 0.4962. ~ 0.487i
'Na(N0C3 ) '?Z-7 -10425
23 tb_.Ing 0--409
22 *1 0.3SINa4O,)63.0 0.2,70
2- 0.270 .7
NaBr ZHr,O *e-o 2~ 193
0.180a 21 12 0,200 o~
~ .1. H0. 240
U U 0.210
Table B (continued)
Saturated Salt Relativo Slope(m) Ave. Slope tFSoh-"tion Used Hum-idity (Ii'gcr 2 mn ngo:Icm2 Ir&
Cr03 44. -6 0.1370. 130 0.136
2! 0-139:1 0.138
----- 36-.4 0-083vI t 0-076 ..01-OS
Values talken fi-oe Sev-enth uaeryReport
'Short-term o. cidation
FExtra-aolated value (2). (3). (41
The inFluence, of the relative humiffity on the oxiL.....tion rates is easiliy
n.o'ted in Figure 33, wuhere !he average vallues of the di~erent slopes are
-Diotted vs. -he rela.-zve humidities a-, which the sloves were determined. The
change in- slopes with change in re-asi-ve humi-dity- has the appearance of a
lazv-S curve. In the 60%- i5e, R- H- range. there is a we~s-defiacd increase
iu. oxidadion rate-
T'z.-%m~rage values -1-r th'e slopes at high ela R. H--. (particularly near
l00ro R- H-.). as well as the widde ranges at each %R-. H- leasis the
to Beclieve that the gradual taffig-off of the cu=-.c -a.L uuc .- e.o ý-ea
cui-;ficzlty with whch eouili riu-m -waz ;.b:--ized- it is believed that thr; mo~st
likelly path for the curvue to follow in this region is somewh-at hig'her tlhan
shown. and should approach the higher limits of the-individ-"al ranges..
The extent of oxidation in the 60-75%~ R- H- r-an2e: indicated a more
j pranounced increase than is shown by in values in Figure 33- Vai:Oation of
10.
oxygen -consumed uitin %R. H- during a 150 min-=e effective oxidaticn
p.trzca disregazdiag induct-ien 2iAsamd by iextrapolation of the dAW vs.
turn - t.rves for s nort-term reactionsl indicated that little significant
oxidation occurred until the relative hritli-ty :reacl-e-d 6ove R-H. At
av rcximately 6T~ . H the ofun 0 oxyge- c:Dnsi-med suddenly increased
with increasEina R- -H.;i at 4 0 54 R- H. an average of cnly 7 r-ng oygen
wenc--)insxz-med in 1581j minutes. %vhereas near !OV,2 R- H-. annro-ximateiy
83 mno ozyzgen were consumed in the sam-e period.
A t~ei~c16 r--- mnwrie -a-.~ made of two alurmnum samples~
sim--azzeo-aslr ox-d~izmcg at different relative humnidities; - =amnnle near
80V, R- H.-i and the other near I00 WFLR H. Evnthough th-,ere -Mas -270t~
difference ;n reaction, a more str-ikidng. difference was desired for the
tunet-la7nse films. This will be accompalished at a later date by p~hotgraphing
e-n.-riments near 45%s R- H- and I00o R. -H.
Preliminnarr mn-icros-zopic investicgatiens at ro0m condlitiomns on thse
oaidation- of alumr-inum initiated by Hgi, were begun.m A-- zaoýsr~ea =-.I n-
sainnle was cement-ed to a slidce and obser-ved as a ziny crvsta; of Hg!, as
brought in contact with the -nma The reaction annea~zed ict-k. nlace in
several st.ezs- F-ýirst, the salt se-m-ed to =cat.t instantly causing adark
area to :o--=, which in turn snr~ead rapidly from !he pouint of contact over
* a relaztively large area- This dark area anoeared to be a clear licuid ui-,Aer
vwniclh small bubbles of gas soon developed and came to the surf-ace. The
length of time this gas evolved depiended on whrether the point of co-nact of
the salt w-as on the edge of a sample, or on a 214t surface iar removed fromn
Sthe edge. Gas evolution lasted longer when the salt was placed in the centra IDart of the s•*- -
As th.e gas evolution diminished, the meitaUic appearance of mner-cur-
developed. A ti- avyer of clear liciuid still covered the surface of the
-- ercury at this point. Soon, this k--.ar lin-id dis•appeared followed by
un~o.--m -ormaao- of a .im over the s-jrLce, causing the metalliz luster te
be dulled greatly. This film grew mo-e and more opaque umtil the presence
o-f the white oxide was aonarent as the film thickened. This oxide formazion
was more ra--iA at the extremities of th- darkened area, especially if the
area was at -he edge of - sample.
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cri•-czl role o!eyea by •ler -•-r. .•-s = stev 1o•-•rds •ders•-v-';•r•z =mzsset es
=r•i•l ro!e. ii is vl•nn.e•. ;o c•r.•" out •.e ful!o•ring t•o " of ex•erz•_•_n•. = "•= °-.
r•icroscope, eleclron •f;'z•.•on, •.u• X-re.y ""-'* -- -•
size and Feilds z d•r•clian =•ern r•.•ie-al o• z•norvh•s :•.aSeri•s. !I
S"• e.•Lz: e r•zl•-°-
{Z! Che-•nic•l sr.,di=• •iil be -•_-e-de in •u e.Hort 1o " " -- ';--= the
zz=ount of•- i=-'-co=•,•'-'i--d in the •---x:•d•.•on .•-':•---•-" .. •-•,c_• • s•-•,•.• •.II be
-'.e•. • --'•dt oer_•use s• le •.• .... .= •..z':•.e.=-=- • •lso ooss-•ly ---•r•o-•e so•---=
S,•_rc•-v. z_•a•ea" -.n" --•e v..-o•nc," . •s iz ;s •orzne•. Tire exmc• o-o•e•ure to
Soe •o'Ao•ed- • De b•-sed on prelizninary • •ne-•< in •ich the prodec•.S•---•:11 be ]:e•ted •t I]O'C. for l• hours z•.d ".he •eig'-•-•• !oss .--i_'A! be de• ed-
• O=•=•-. .-:-•-='•: :•-:i--•, zn" w•_.i:• the .or•d•ct •-=AI be des!co-ted a• room te-•=•-•. -- -
rare, •6.'_I] --!so oe •, •ee o-•.
S-
m • 1 .... .. '
36-
Qiuanzit;a: ye rhaL nthe rate of ox--cation of alumininun in
o~ resence w! HI~, have been lite o wcure alur-Lnintnn A few Studies
!I ,ý c~r:ied out durine the neict cuarter on less nure alu=min-um and on
azuun-mz.a at!vcs- 'The C =,e.; "-fths will~ Wbe DCoezermin~ed ypelmnr
ItiS wc' tlat iron has a moi=Fate :-i a~. ozidation (or rusting)
-n h-:ghly inu-mid atm'-n ipheres - D-1--ring --he ;-ez! quarter oreliminary and
qualittive enienson iron will be be-u to-trin h a-eo
ofS~n 0! ~n zn h=-d--: !h~sn~c - re 1vresence of iva-rious metal sal:ts-
I4
3L~
L~D'-dA jack-sor. jr. *and -Heary Leidheiscr. jr..
"ý-ithh. Sixth and Seventh Qi.trvRenor~s 'to theArmy Chf-mical Center under CoziLract No-. DAIS-IGS-495- -_518, janua-ry 19, 1961. AprR 2. !961, and
2- D_ S_ Ca~rr and B_ L. -H arris. Soluti;ons ior 11a;minaingConstant _Rl"_r lndustri~u1 and Engineering
Chemistry. -41. 201.1( 19419).
L-ange's lAa.=SDoork -3f S h Ediftion, 1454..55(1952!0-
- -- nzue's HaxmAbook of Chemist-r. 9th BEd~ton. 14ZO-27
(196N
Vp