I'
·~
BARIUM a&.CCHARA'.l!E INVESTIGATIONS
Research Department
MM,
1921the data gi Ten 1n the followbti paragraph a'UJIDlerlto tbe rooul.
ta
obtained lo oar 1nY•st1ga\1anarelati•• to
the4enpria1n,t
ot
mar 41aom'd aolaaHa.0111' pPel1m1DaZo7 1ttwat1gat1.ona led ua \o lH,lieve tba.t better re-1'11 t• ooul4 l>e obtalruMl b7 uetng bu-la oxlu ra.ther the
atrontla o.a
theaperlaetd plant ws:tb a. capacity
ot
400 lba.ot cl1tc&l"4
aoluau
pd!" dllif na 1natall and opern.torl tor al>ou, lbJ-ee 11.ontha. '111• plant 1noluded.a
Manator
recO'fof'tng G urttua OX14• •o that U algb\ be raauecltor
the preclp:ltat1 o'f tmffO tndetlnttely.!'he o"rattau
ofthe expel'btmta.l pl,mt
waa.ucceaistul tn
IJV&I"'I Pespeot. 'le wve able to delaana trte
the tioa'b1l 1't1
ot the ru.-1ua•-generaU on Pr-ooeaa to our ea\iafaotii:m 4 iu Bd41t1ou t<1Wl4 it to b• praotlcftl
to :recover mare
the GOO l'h•.o'f
Et!"ulattl4
tuft81"per
& T V ~ton of our dteoe.rd
IIOluaea.In the par'agt'al)Jl5follon , our coat eaUtmtea aro bn1 r,n the fol-lowing -pr•1•••i
1,, -
!he4eeugar111ng amtuall ot IOOOO tons ot
utoften.a 41toar4 aolaaM•.W -
!he tr•atMnt
Jlan.i to haY• a. cla1ly oapn..o1'1't
100 tons ofmoluaee
per 24 11.0'ID't oontm.uoua Operatlon, th• p1m1, to be op&rft.t«l ? Cl.ff¥•-per
week an4 ~00 4qa per7ear.
&-4 - l 4.&117 product1on
ot 800 b
on
,hit buiawe
eat1Mte thnt tho opfll"Bt!on Ol)sta r bogot
aqar produoe4
w111eO&Ult
\o fl"ll!l t2.713to
a.oo
per ba«.~ls ttm.tr•
tn-oluct.ee
the tolloWlZI&' eltl.'t.$til4awu,
lat .. Laber2114-
wr
3rd - Supplied
4 -11a1nurumoe
'!otfll.to.•
per bago.u ,. "
..
!t -.S.ll be
no
td.,
1t 4oea not 1nolwtea
OhAl'ge t<r olatn
de .... 11Yr.t to the
l t.nor
4oea lt 1l'lclud.• ony cmtrhoa4 OhBFge OOl"r•SJ,c>ruUneto
o\U" O.Ueral Otfloecharges. tnaurance
an4 !ASe1. 'ft 110tll4point
out that the pi>weJ" charge l bproba'blJ be a
oonatant
factor in O))Ol"t1t1on. charge. au 1 t u.p1-ienl"1 ad•taablet
cbate , ott a ln t1rtJe oontraot 'bala.
The ahn:rge•t
1• l&bOl',. 8Up-pl1•• end maintenana& will,. howe r. f'l otut1.te wit o41t1 pricos.Ill1)!3.}a$1gp.
CQt\14t1pon
the _.eque,t
ot tbe
e,ev
1:>op ia-en,.
our
·~1 · er1neDep1rtaumi h md.e the tollow1ntt • ti t•e of !natal.lats.on ooeta. 'lht>ue
eatlmate• 1nolud.e bu1141nga and all equl.
t
neoe••U7 tor pl"OOa11OJ>M'-a.Uon,
mt
4onoi tnolu4• the coat
ot
plant at.te.
the aoleotlonot
wbloh hu not b•• • • • Jqulpmc,nt alre~ o.e4bJ
the oiwpan;, oh u l)lffl8and
017atalllsv1 tor
Jobnl\Qllft tm41nntar•
t,;roJeo a, eto., have bNll
t••
tnto o
1ldero.tlona,
"111be
"11 1n the tollr,wiDg,Pl.a so .. 1,. 1nolu41 bu1l41nga
or
atoel tr an4 uheet 1:rou al41Dg tbJ' ou\, 4ea1 eel 10 ttin.t the sheet iron ma-:, be ropla.oed w!. th'brloJt
at a laterdate
1t d.ealrecl, 1118¥ 'beoonetl"ltcted tor a
totaloo•t
ot
*4&7000.00.ot
th1 1110tiDlt $136000.00 r411Teaenta uterlal alreu.d¥ omedby
the com
rmt 000.00, • ad.di ttonelc
tla~ ro
ired ..Pl.a.a o. ., provtdln
tor
etooltr
e w1 brick ct ol stulh bu1ldb1p adtle 60"'0.00to
the abo'fe, br 1n,s1q the total oaab tlt1y t~11000.00
and th41total coat
10truooo.oo.
The purchase of used equipment for a large percentage of the process machinery is incorporated in both of these estimates. In case new process equip-ment were used throughout, the estimate amounts to $666000.00 cash outlay and the
total cost to $802000.00.
Factors Affecting Plant Location:
In selecting a plant site, we would point out the following pertinent factors:
lat. - Power: It will be necessary for us to purchase between 70 and 75 kilowatt hours per bag of sugar produced, hence each mill ($.001) charged per kilowatt hour purchased amounts to 7 :,r 7-½" eta. per bag of suear produced.. The process is such that a constant power input is essential, therefore dependability of power supply must be given careful consideration.
2nd.~ Shi~ping Facilities: On the annual incoming freip.ht the following will comprise 9o% of the total tonnage: lst.-molasses from our VR.l"ious Steffens plants, 30000 tons; 2nd.- coal, 20000 tons; 3rd.- raw materials, salt and barytes, 1200 tons; and 4th.- miscellaneous, 1000 tons.
outgoing freight will consist of 240000 bags of sugar per year. 3rd. - Labor Supply: The process will require a total of ~pproxi-mately 135 men divided into three shifts, of vtlich 25 are foremen, chemists and assistant superintendents, 10 are mechanics, 85 are stntion men and 15 are laborers.
•t
aola•••• ha.a be•:a lmfttar ....,,.,
~•an atlll haa been ••plo7eil wtt.b,aore or
l•••euooeH
1a:Suro
4at oae
plant 1n Oana4&. !.blmoat
.. rtoua ttttottltJ' • ouHrtd Int.tte
pll'OOeaa 1• then-aeneraun ot
bU'l•
oa14•hoa
llll caroou.u
.
•
to
etfeo,
thll 40Jffer,101t h1c\q NqulN• veq Ai t.eaperaturea. whtob om,. na4117 be o'bt.&1-4 OlllJta
t e l•otrto tvnaoe. ha •iho4
ot
oouv-er•1on noton1J
•ntaU• a111gb. patre1" coa,, i 111g to oauatto roperth• ot \.18 ma'\lrlal .baadle • t.
ooata
tor eleotr4dea
atl4 ~Mlnte!lanae
are exc,eaatve •
.bt prooeu Qt b.Vla
regenorauon
4ev1tedb7
llJ".:a ••
SU.fol"•to oo._r
hlohpattnta •••
e11 applte tor, 1
a
d.ea1ttti
ultt•• e!Ulale '41uo·,e.
~n
u.ratioa
11aaa
try wt obaaio&l
•~oda.
Ma &T014 the
u.w4 ••Unly
1etl7 •"tated. the ohflm1•trr
ot
tb!t prooe . . la . . tolio.1,xn.aolable barilll aaooba.r&te 1 a torr.11d l>J m1z.1Dg :aol.NMa
wt
thaolllt1cm
ot
barlaa bJdrate,. the bU'1taaaaoharaw
1a u41nto bari carbonate • 07 the a.ouon o.r OU'bou 1os14e •.
the
ba:ri• oU''bODa'8 111 the to.rm o -t a •l la con erte<I. iuto l»ar1aclllori • 1,7 brlllf:1 1t 111 0011
et
wtth hJd,l'o~hlor!c ao1d P*• !bl aol-ut.lonot
bari• Ohlor1 1a \hen tNat.e with ca.Q8Ue •odA wbeN1'7 bar1a hJd,rate la t0t'N4, whtoh. aepal"atea aa a oeysitu.11tw aoUd. from Gold. aoluUons. fhllb74r&.te
ta nowta
•uclltora
th& t 1\ can beue4
again ~or the preolpl \ationot
•ugar.the
:reaction beMtit oauttoaOda d ha
ohlortd•
gtv11 •odt• oblortcw In ad.dUion tobarta
hl'drak. 'I.bit sodt chlort • ls aubJ cted to electrol7at1 l'fhloh ,1,1 •oauatto •
•
hydrogena.m
ohlo:rlne.
theflJ'drogen and ohlor
b:aean
b'Qf'Md. to
tom the
vlpa
u•A la
oonvtrt
tng th• barl•ou"ouw to
'but•
Wllorla.t. f.lw o-arl>Oad.toxtt.
gl're.11ott
clu1ng th.ta reaot10ll mq " aed. to ecoapo-se thet'be tollowtne t'ml4ueztlal ohemtoal reaot1b:U clearq d.ettM the Yai"lou 1tepa tn , • prooeea,
lll
•
(oai.2 + q_ • 012u°t1::
012Hno11·o
• ll20; •
aq (2) Cu? 2o11. JaO + C0,2 e 01:UiaOll + OOs( laOO;f + + 2lf l (pa) c 12, • 112 • 00,2 + a
(4) : 8a (O ) 8 ll,20 • I l'ael +
(6) &Cl + lee\. cvrmt + • Zliavl! + + ! l • Aq ( ) 2lt + 2 ...
1 :
%ilOl4
uumN.r ot teat•
n.re
Melein
tht l bONtol'J'tn or4e•
to 4•• 12:18 thl NI coruUt 10u for \be .fOl'IIAtlOD oL lw.-1• I Clbar&Mre, t!a rate ot ag1tat1011 ot b ta hJdrate - aola " ' a!ztl:IN; t,,1:apu.•at.u.re cf t.ha
atxture, oono Atratton ot the 1110la.saeaa ra.t1o ot hr1a oa1de to ~ r. fbe eas. reaulb wer ol)ta.1m4
utnc
•la•••
d.tlut.ed tc> 40°-460
.rlxand bar1 b7drate ,olutton 0011ta1n1 3~
o.
fbe
molaaae1 ,.._. dad.1
ainutelonger.
Bit1o
·
o~ BaO to a
wu
1Dtll u4e
o
1n w ttb.water. (
•e• 1'1• aeobb.r e alt Itaa
fto 100.
!Illa
OUnot
eo1p1tatioa i!xperlaentalt.o ob 111 a tne tllter1n u1p1tate. ti
er
\best oo · lUona a recovery o.n ssigar aa aada. ,he D71"\lP bA4 a tna pu1•H7ot
9&-9f)1.·ooraioey teata N taadAt h1ch 1 lo te ·
t
buia as.ri,o te sl"Wtp ooul~ bt tr~ated i\lt.h "'l a tn a Ulall glaaa t ,.wttb ve17 little o•in. PO e r ae llled about t o.,..thtrd.a
tl"OII
io
to 3&&11••
bart• oarbOnat.e pe_. 100 SU• vatel' u ••bea.,, aa
u14 paaee4 OWJl through th.la tm:er. th11ftfON tn oJ'd.er to pro4uotl&Cl_z 101 tion ooniahd 50 giu.. la per 100 ••
ot
water u n.a only neoeoa&:7 ·to put thea
OYe elud.p \tlr-Ol1gh the towtr p t l1 a.ll thlcarbo.nate • • conTeru4 t.o hlorl
athen
~to
tlMIchloride aolut1on to
'P1"0uoe
a
t1al
ao1ut1on
ot
the
••1n4
eol'lOentra-t.ton. It wae al.ao toGhd th&\ \ha.&i.OOa
lud.ee .l."Ula1ne4 uutral o.rali{>"hUJ 4lkal1m 1rh11« ei.11 tnatt wl Cl a e t 11 \htt oarbona~
oonoontra.tton waa Ndu.oe
t.o .trca
1«,
2 puit•per
100pvta
ot nter.
oae
:or'k waa oauaUo mMl t.he oool!.Dg t.erec •
17ot
hJ
rau.
olu.t lou oonta1nill6 50
•
0 41'8:rmlDI \ ptl'CMA
•xo•••
ot
aa\Ul't n•••a..,r
oob,a1n
heh16htat
It wu d t!'u,t hon~ ba.r1 oblor!.
r
100• ot
~1r •hCO • or t.b1 tb4toretioal ~ou:o.t or o l.lat o imc, aaq r..nd. o(>Oled to
uo
v be lOTI tru.t ~w
99o~
ul e expeote ..\ .,.. ~uve
l,'f~:no
ft 1.)! aol 1 l ty of b.M-1 aa..ioh rat
tn w
tor
:ld btU" t •hJ'drate
,olu.t1ona
r
toua tn th.•ao
ter ne
-In o!\ie t.o
i the ,.tion
proo••••
a ,pl.14n · wu e1i;J'1'1t an .. equippeQ. to M lt 400 - 500 lba. of moltUHI per
dq,. ht l nt
a•
aau;>l t in 11 -1la J».;;.le u not only toa.i..o teat• on tbe r•ooYU"J ot au trm t · ta.r1im aacch~r.t•
ayrap. tile nt o al d c · ,nt olo chemic
con-trol a h'14 O'Hi"
aa.ob
stagot
the prcx:e a F,.t;all
tl•••
t.te pru,. 1 ~ o Ject
ct
the o ta toat
int thlpnwniu
oilit,'o
er
tlo.nproceaa
u tths
$&me tf.111 .rk u. t. oorta.1n en lnGer p.roulose foh o ld. ont, ·• •<>l••d'bJ'
t:xperleno. •.be pl.ct ma1 e divide
mt.o
three de ,ar-tmonta, Mmal7. the 11& OUStll t• lo;;;tonl aeqwancc tl"Om oth 'lie1f,Po1nta.
I11 ,~ dt110l:&8•1cll on the propo11t1 plant we ha.Ye ued. .all lculat.iom on t.be baa!•
ot
tre&U.q 100 ton-aor
tao 1110laan1 per24-hov Aq,
aont111uoua
f).P9raua u4a
:SOO-<lq openU;ng 0caapa1pper
7tar. his pr-~v1daa tor wor.idu 30,000 touot
110luaea a.nmu.ll,f-tbe
a••r• aowi\ ot ou
41
II04r4 O't'er a
period
ot 71ara.
crat
Jncooat
tt8',11'ea ue
"baledoa
ta
Noat1er7 ot clpt
bag•ot s,apr
·
per
t •ot
~Ql.YTIC HOUSE
Under this head will be considered, first, the Electrolytic Cell
Station for both caustic soda and chlorine and for producing the hydrogen required; second, the Caustic Soda Evaporation; third, Brine Purification Station; fourth, the Hydrochloric Acid Furnace Station; and fifth, the Electrical Substation for Electrolytic Power end the Repair Room.
Electrolytic Cell Station Experiment al :
The following equipment was used on this station: Ono G. E. direct current generator, 1666 Amp. - 6 Volt to f'Urnish current for electrolysis; one 15 H.P. motor direct connected for driving generator; one G. E. direct current generator, 3.26
Amp. -
116 volts for exciting the field of the large generator; one Allen-Moore electrolytic cell, 1000 A.mp. capacity. Theneces-sary excess hydrogen was purchased in ayl1nders. The quantity used was not sufficient to justify the installation and operation of a hydrogen electro-lytic cell.
All of the above is standard equipI:1ent and requires no special de-scription or discussion, except as their f'Unction bears on the operation of the process.
The acidulated brine described in a followine section was fed to the cell through a feed box equipped with a float valve so that a constant head of liquor was maintained on the cell at all times. The level of the
brine in the cell was regulated by means of an adjustable feed valve which enabled the operator to carry any predetermined level in the cell. The level must be increased from time to time as the diaphragm becomes clogged,
in order to maintain the proper flow of solution through the cell. During
the latter part of the campaign a small steam coil was installed in the feed box and the temperature of the feed kept at about 50 Deg. C. The cell flow was thereby increased about 15,b and the voltage decreasod about 715,. This means an important saving on large scale operations.
The cell was operated 1000 to 1200 amperes and 3.8 to 4.4 volts. About
o.4
volts was due to poor connections between the switch board and thecell. The cell flow varied from 11 to 13 11 ters per hour and contained 110. to 130 gm. lfaOH and 100 - 160 gm Na.C,l per 11 ter. The current efficiency was 90 to 95%. At 1000 amperes the oell produced at the rate of 70 - 73 lbs. NaOH, 64 to 66 lbs. Cl and about 1.8 lbs. H per 24 hrs.
The asbestos diaphragm was renewed once during the 55 day campaign period. This renewal took place after about 6 weeks operation. The diaphragm was found to be clogged with slimy material which had been precipitated from the brine solution. The following is a typical analysis of this material:
Moisture
Insoluble (HCl)
.Loss on Ignition (Organic) Total Bao Fez 03 A12 03 Cao MgO NaOH NaCl BaS04 BQUlz 54.07%
7.87%
8.85 1.12 4.55 6.83o.sa
1.22 11.57 3.12 1.52This analysis indicates the importance of doing good work on the brine purification station.
There was no noticeable deterioration of the anode during the aper a ting per i od •
Proposed Installation:
In ad.di tion to the Allen-Moore cell (mfg. by the Electron Chemical Co., Portland, Me.) used in our experiments, there are at least two other electrolytic caustic cells on the market worthy of consideration. One of these is the Nelson Cell (mfg. by the Warner Chemical Co., N. Y. City) and is similar in general design to the Allen-1.foore. The other is the Marsh Cell
(mfg. by
c.
W. Marsh of N. Y. City) a somewhat recent development, but pre-senting certain apparent advantages. All these are known as diapiragm cells, which general type is now most widely used both in this country and abroad.As to capacity, the Allen-Moore is built in 3 sizes to economically work at 1000, 1500 and 2000 amp •. oapacity; the Belson in one size at 1000 to 1200 amp. and the Marsh, being of flexible design, handles up to 5000 amps.
At a constant amperage and with uniform operating conditions, the voltage requirements for any of these cells vary with the age and condition of the diaphragm as has been pointed out. This factor causes as much as .6 volts (3.3 to 3.9 voltsl increase during tho life of the asbestos diaphragm. Hence, in our power estimates we do not feel justified in counting on less
than four volts per cell.
In our calculations, we have used the 200() amp. Allen-Moore cell-not because we know it to be the best, but because there is available in Denver a rotary converter which will meet our needs if we do use it and which can be purchased at a reasonable figure.
A 2000 amp. cell will produce about 144 lbs. of NaOH per 24 hours.
Our requirements will amount to 20 tons per 24 hours, necessitating a minimum of 278 cells. ~o this we add 12 cells as a factor of safety for operation, making a total of 290 cells ready for operation, but only the 278 in the
cir-cuit. With an average voltage drop (including line losses, etc.l of 4 volts per cell the overall voltage of such a system installed in series would be 1112 volts. Arranged in two parallel circuits, the voltage drop of each
cir-cuit would be 556 volts with an input of 2000 amps. per series. !mch an
arrangement can.be operated with a 4000 amp. 550 volt rotary converter such as is available. (See Western Chemical G.~. Rotary at Denver).
Labor required for operating such a system would consist of two attendants per shift of fairly high class men which we have estimated. at 1ji4.!')0
per man shift. The principal duties of these attendants consist of replacing cells in the series with others from the repair shop, checking performance of
the series of cells and individual cells. attending solutions. solution flows,
gas line leaks. etc. They are to be assisted by one "flowboy" at $3 .50 per
',
shift who checks solution flow :from each cell each day and by one repairman for one shift per 24 hours, who replaces worn carbon anodes and rene,vs the diaphragms on cells cut from the series.
The power required is consumed entirely by the cells as all solutions Oow by gravity. This amounts to 2511.5
I(r.n
per ton of caustic produced actual-ly consumed by the cells. At 93% Rotary efficiency the total power chargeable to electrolysis of NaCl would be 2700 KW!{ per ton of NaOH or 54000 Y.WH per 24 hrs. on the A.C. side. This figured at ~0.007 per KWfI (see Colorado Power ~o.proposed Contract) amounts to ~378.00 par 24 hrs.
On the supplies for this installation the raw materials are con-sidered under Evaporation and Brine Station.
Maintenance, according to the Electron Chemical Co., consists entirely of asbestos and Aoheson Gra~hite for renewals. Under this they re-commend 302 lbs. graphite at 26 cents per lb. and 35 lbs. asbestos at 75 oents per lb. per 20 tons caustic produced, amounting to ~69.72 and i26.25 per dey respectively.
Vle have allowed $60.00 per day for miscellaneous maintenance. This operation, it must be borne in mind, is accompanied with the handling of cor-rosive gases in large quantities, hence tho liberal allowance. There also enters into this amount the question as to the correctness of our estimate on asbestos, which depends upon purity of brine used in cells, especially since it is possible that our recovered salt may contain matter which is not present under the operating conditions on which the figure is based. our experiments indicated this, but they also indicated the possibility of eliminating this trouble in a properly designed unit. We believe the above amount will care for this feature
in case it is encountered to a serious extent.
On electrolytic cells tor the production of hydrogen (see Hydrochloric Acid Station) there are two cells v.hich havo been investigated in a preliminary 'W83 at this time; lat. the Electrolabs cell (mfg. by Electrolabs Co. at Pittsburg-also known as Levin cell) and the Leuning Reconstructed. Burdett cell (mfgd. by
Burdett Oxygen Co.) The former has a capacity of 800 amps. at 2 volts, the latter
ot
2ono
amps. at 2 volts. The latter is the cheaper cell to install and operateso far as we have investigated. With sufficient rotary converter capacity, it would be possible to install these latter cells in series with the chlorine cells.
Each 2000 amp. cell will produce 768 ou. ft. of H. per 24 hrs. our requirements amount to 26000 cu. ft. per 24 hrs. requiring 35 cells. In view of the fact that this installation would consume about 165 KW and that the voltage capacity of the proposed rotary is loaded, we are recommending the installation of a motor gener-ator set of such capacity as to handle this amount separately and to Operate on power produced from our own steam a.head of evaporation or from purchased power as desired. This nexibility would permit us to keep our HCl f'urnaces lighted at all
times in case the chlorine cells are temporarily down due to power trouble - an operating feature which we feel inclined to recOl!l!lend very strongly.
These cells are to be manned by the crew attending the chlorine cells. The power.consumed will amount to approximately 4000 K\7H per 24 hrs. which is
to be produced from our own plant at <f0.007 per KWH amounting to i2B.OO per d~.
Supplies are negligible as the raw material is distilled water. Maintenance is included in the above figure of $60.00 per day.
At the time of this writing the Burdett Oxygen Company has indicated to us a desire tc enter into an agreement whereby they would use the oxygen from this hydrogen equipnent, but such an agreement while apparently feasible from an
operation standpoint has not been considered in this report.
The cell house should be well ventilated and all steel and wood painted with "58" pitch to preserve it against the tuines and moisture.
The cells nre to be installed in rows with at least 5 ft. aisles and
arrangements made so that they can be lifted off their base with chain blooks, and taken on a trolley to the repair room for changing of diaphragms and renewing of anodes.
The cells must be insulated from the floor by means of glass plates. the brine feed line from the header to the cell must also be of glass to prevent leakage of current tr...rough the feed lines.
The chlorine lines should be constructed of tile. For all the other lines wrought iron can be used. The hydrogen and ahlorine lines should have ample slope so that any moisture carried over will condense and run to the low point where it oan be trapped away.
The cell effluent line must be trapped from the cell through a. U pipe to prevent air from being drawn into the hydrogen line as it is necessary
to maintain a small vacuum on the cells. The cell effluent drain to the pump from the cells should be a pipe line and care taken to keep the caustic from the air as much as possible to prevent the formation of sodium carbonate.
Partial specifications for proposed installations are as follows: 290 - Only - 2000 Ampere - Allen-Moore sodium chloride cells,
~ype K~ - dimensions 8' 10" long x 1' 2" wide x 3' 6" high. fhe above dimensions co•rer gauge glasses on ends
of cell and all bolts and connections: actual length of
tank of oell 8' l". Bus bar copper connections to be 3/4 x 2'. 35 - Only - Burdett (Leuning reconstructed type) 2000 Ampere.
Experimentru.:
Hydrogen and Oxygen cell. Dimensions of cell 18" x
24" X 4' high.
CAUSTIC
SODA
~VAPORA,TIONThe effluent from the electrolytic cell which normally contained. about 12% Na.OH and 13 - 15~ Ma.Cl by volume was combined with the fil tra.to from the barium hydrate which ordinarily oontained about lo% NaOH and 15 - 17% NaCl by volume. This
solution was sent to the evaporator and concentrated to about 40% Na.OH by weight. The crystallized salt was washed to free it from caustic and sent to brine system
and treated as described below. The caustic soda was stored in iron drums and used
as needed 'fl1fl the precipitation of barium hydrate.
A single effect vertical type evaporator was used. (See Dwg. No. 323 RL
& 324 RL.) The evaporator was 21½'1 in diameter and 5' B'' high overall.
Twenty-five square feet of heating surface was provided in the form of 111 diameter Shelby
Steel tubes l ft. long. These tubes were arranged around a 10" diameter well to allow free circulation of precipitated salt. The conical bottom was arranged to drain direotly into the salt basket which was 42" in diameter and 811 high with
dished head and bottom. (See Drg. No. 366 Ht.) It was provided with a perforated false bottom overlaid with 20 mesh screen. The solution containing solid salt was circulated through the salt basket and
1aallk
into the evaporator by means of a 1" Deming gear pump.The evaporator was operated under 10" - 15" vacuum and with 30 to 50 lbs. steam pressure. Under these conditions 400 to 600 lbs. of water per hour was eva,... porated, depending on the concentration of the solution and the amount of salt in
suspension. From time to time the tubes became coated over with salt to such an extent that it was necessary to pump a part of the solution from the evaporator and dissolve out the salt by taking in fresh water or condensate. At intervals of about two weeks the tubes were boiled out with dilute acid to remove the small amount hard scale 'Which is formed.
The principal difficulty on this station was washing the precipitated salt free from caustic. There were two reasons for this, the salt basket design
was wrong, the ratio of the diameter to the depth being too great, the accumula... tion of organic matter caused the salt to separate in very fine crystals, which, together with slime like impurities, tended to render the layer of salt impervious.
A number of schemes for washing the salt were tried. The one which finally gave the most consistent results was to circulate evaporator sunply solution down through the salt and back to the supply tank until no more caustic was removed and then wash once with fresh water. By this method it was possible to reduce the caustic on the reclaimed brine solution to 1% - if~. This figure is higher than commercial practice p3rmits, however, since salt washing equipment for large scale operation is being successfully operated, we feel no concern about excessive caus-tic losses at this point in the process.
The following is a typical analysis of the unwashed salt: Insoluble (HCl}
Moisture
Loss on Ignition
Total Acid Soluble Bao Ba.C03 Ba.S04 NaGl Na.OH Na2
co
3 Fe2 03 & j.J.2 03o.41%
12.45% . 4.65 3.81 4.91 .10 56.10 12.17 3.16 2.61The following is an analysis of slime taken from the salt basket:
Soluble in Water Insoluble in Water
N~l 57.0 7.50
NaOH 7.40
Organic Matter 2.76 14.40
Fe2 03 & Al2 03 6.80
B~ 1.20 31.00
c~
2.00MgO 4.10
~2 18.00
These analyses indicate olearly the importance of thoroughly washing the
salt, not only for the removal of caustic, but for the removal and separation of
insoluble matter. This point is further emphasized in the discussion of the
pro-posed installation.
Proposed. Installation:
The Caustic Evaporation Station in the proposed 100 ton plant will
handle a feed of 46.76 tons of caustio soda, 75.18 tons salt and 334 tons water.
This amount contains all cell effluent solutions, the solution returning from the
precinitation of the barium hydrate by means of caustic from barium chloride and
such wash water as is used in washing the salt produced in the evaporators before
sending it to the brine purification system ahead of electrolysis.
Of this mixture 257 tons of water is to be evaporated, 38.65 tons of
caustic in the form of 4CY}b NaOH solution (by wt.) is to be produced. and
approxi-mately 95~ of the salt is to be crystallized.
The problem of concentrating caustic solutions is much more complex
than is the case of sugar solutions with which we are familiar. Factors entering
into it and which we have taken into consideration are:- 1st., rise in boiling
point with concentration; 2nd., heat of chemical combination between caustic and
water; and 3rd. heat losses due to disohar~e of crystals.
After considering 20 different combinations and methods of operating
multiple effect evaporators in connection with this problem (see blue print
No. 418 RL) we have ohosen a quadruple effect counter current flow which will
con-sume 180,ono lbs. of steam at 42 lb. gauge pressure per 24 hrs. This oombination
because of lower pressure in the first body - necessary to our minds because of danger to operators through possible breakage of sight glasses and caustic burns, etc. our calculations included quintuple effects, the most efficient of which would consume 5600 lbs. ooal less than the one chosen which at ;.i5.oo per ton amounts to ~14.00 per day. The maintenance on an additional body would probably amount to ~10.00 per day, leaving ~4.00 to be charged against insurance on the above.
It is worthy of note here that in small electrolytic plants engineering practice seldom uses more than a double effect on caustic. This is apparently due
to two things:- 1st., higher concentration of finished solution with correspond-ingly high increase in boiling points, and 2nd., lower prioed coal which will not offset additional maintenance for extra bodies. In larger plants, however, the triple, quadruple and sometimes quintuple effects are used successfully, accord-ing to our information.
In connection with de3ign, it should be mentioned that vertical tubes from 6' to 8' long are generally used in apparatus for this work. Steel tubea are generally used and one installation is using copper or brass (Berlin Mills -Brown Co.) Erosion of tubes due Bl)parently to crystallized salt pnssing through
them at high velocities is the principal cause for high maintenance. Chemical action due to improper control of brine to cells allowing formation of ohlorates upon electrolysis is also listed as a source of maintenance troubles. We have calculated the heating surface at 2500 sq.ft. per body, based on a heat transfer of 200 BTU per hr. per sq. ft. per l Deg, F. temp. difference.
Washing the salt fl'ee from caustic before dissolving it from the salt basket has been r:1entioned as a difficulty encountered in the experimental work. As was brought out, this was partially due to design of our eXJ>erimental
in-stallation and partly to precipit~ted slime(primarily barium carbonate} whioh accompanied the salt in the basket.
Judging from information which we have, the salt basket has never been Rn entire success from a washing standpoint, although it has been possible to loso only
1/z;
o
NaOH on reclaimed salt. In the usual operation of an electroly-tic plant only 40 - 5o% of the salt fed to the brine system is reclaimed, the re-mainder being fl'esh.According to our flowsheet, fully 951, will be reclaimed, hence both the caustic lost and the acid required to neutralize it (in the brine system) aro doubled.
It therefore is necessary to keep this salt washing operation entirely within control. Again, in standard operation of electrolytic plants fresh water is used to dissolve the salt frorn the baskets after it is satisfactorily washed. 1'he solution coming from the basket is only 5cf/4 saturated whence it is sent to dissolve fresh salt in the brine system. With ou~ flowsheet it would be neces-sary to saturate this solution to at least 95%
and
as the rate of dissolution is somewhat slower during the last half of such an operation than during the first, it is at once apparent that our baskets would be in the dissolution portion of the operating cycle more than twice as long as in standard operation, necessi-tating larger baskets and undoubtedly sacrificing control of solution concentra-tions going to brine purification.For these reasons we are recommending that the salt be collected in baskets which can be discharged without dissolution and that both washing and dissolution be completed in the brine purification system. To accomplish this,
it ·will be necessary to design a salt basket which can be discharged at will or to employ a system such as that devised by Mount of the Glamorgan Foundry Company
(Virginia) for this particular work. Such an arrangement, allowing for separate washine of the salt. also permits the recovery of insoluble barium carbonate men-tioned above. and its return to the process.
Of the two possibilities we nre inclined to favor the salt basket with bottom dump arrangement and ~eans for sluicing it free from salt. The flowsheet further provides two triple deck Dorr Classifiers to be used in a counter current washing process. Inasmuch as the classifier is a continuous apparatus and salt baskets are to be discharged intermittently, it will be necessary to provide an
equalizing tank so that the rate of feed to the classifier will be uniform at all times. We have used the "mother" solution from the barium hydrate precipitation which runs about lo% Na.OH as a first wash for the salt and fresh water for the finish. The classifier is in use in at least t\'10 :plants in the United States tor the purpose which we have outlined.
All wash waters from the classifier are to be returned to the caustic evaporator storage with one exception. ~he actton of the classifier is such that finely divided slimy material such as barium carbonate will leave the ap-paratus with the wash solutions rathor than with the salt.
Taking ad.vantage of this fact, we have provided a. thickener in which to settle out this slime from the wash solutions, taking it together with some caustic sod.a to the Barium Chloride Pllrifioati on Station where the mixture is used as a reagent as will be described later and the BaC03 returned to the
pro-cess.
(This barium carbonate is formed, we believe, by absorption of carbon dioxide from the atmosphere by both the oell effluent solution and mother solu-tion from barium hydrate precipitasolu-tion. However, it would appear advisable to provide against such absorption in the handling of these solutions, thus elimi~ nating both losses and difficulties as far as possible.l
Partial specifications for the caustic evaporation station are as follows:
4 - Only - Evaporators - 2500 sq. ft. heating surface each. Each evaporator to have two salt baskets ( Special design).
2 - Only .., Simplex triple deck Dorr Classifiers, Approx. 30" wide, 25' long.
1 - Only - 14' x 6' Dorr Thickener with mechanism and super struc-ture.
1 - Only - Duplex Vacuum pump and 15 H.P. 440 Volts - motor direct oon,nected.
Brine Purification Station Experimental :
It is necessary to send a pure, slightly acid (HCl acidity) brine solution to the eleotrolytic cell. Impurities, especially lime, magnesia, barium, iron or any suspended solids quickly cloe the cell diaphragm, causimg high electric~l resistance and consequently high power consumption and unneces-sarily frequent dia}ilragm renewals. The presence of sulphates, or of alkalinity causes the formation of oxygen - chlorine compounds which attack the graphite anodes of the cell and also cause corrosion of the evaporator tubes.
The equipnent on this station consisted of one l" Swaby centrifugal pump for circulation, two wood stave tanks 3' O" dia. x 4' O" deep, three wood
stave tanks 3' O" dia. x 3' O" deep.
Tank #1
(Saturator tank) was provided with a false bottom of coarsescreen upon which a supply of salt was kept to make up losses
or
to balance the cell supply in case the supply of fresh salt from the evaporator failed to meet the needs.Tank
12
was the circulation or make up tank. Sufficient water was added to this tank each day to make the proper amount of solution for the fol-lowing dB¥' s run. The solution was heated to a.bout 80 Deg. C. and circulated through the evaporator salt basket and if necessary through tank #1 untilsatur-ated. The saturated solution has a sp. gr. of 1.200 at 20 Deg. and contains 26%
NaCl by wt.
The saturated salt solution was drawn into tank
f3
where sufficient sod~ ash was added to precipitate limo, magnesia and barium. The solution was then agitated with air for about 30 minutes and allowed to settle for 24 hrs.The clear brine was then decanted to tank #4 or #5 and acidified with
HCl to about 0.01 ~ 0.02% acidity. The theoretical amount of barium chloride was added to precipi ta.to the sulphates. The bnrium sulphate required 16 to 18 hrs. to se~tle after which the clear solution was-fed directly to the cell.
Ordinary ice cream salt of the following composition was used to charge the saturator tank:
NaCl
CaQ & :UgO
S03
96.9%
o.a%
0.75'
;
Later table salt was used, but it proved no better than the ice cream
Bal t.
Proposed Installation~
As was pointed out above, the primary object of a brine purification system is the reduction of the maintenance charges on cell and evaporator equip-ment. The processes employed in tho system consist of precipitation and the
In our reclai.l'!led salt thore wiJl be no sulphates present due to barium
in the evaporator system and previous to it. On the raw salt, i.e., the salt used
to replace losses in the system, sulfates must be removed by acidifying the
solu-tion and precipitating with barium chloride. Inmediately after th.e precipitasolu-tion
of the barium sulfate, our flowsheet provides ~or the mixing of this raw or fresh
salt solution with the solution of our reclaimed se~t and the precipitation of
alkaline earth salts from this mixture by means of soda ash as carbonates. The
insoluble solids in the mixture now consist of ba.t·iwn sulfate, and barium, oalcium
and magnesia carbonates which are separated by sedimentation in a Dorr Thickener.
The weight of this precipitate is small and there mey be some question as to the
advisability of installing a thickener mechanism to handle it. However,
con-tinuous sedimentation eliminates the human factor to such on extent that it appears
very desirable. With continuoi;.s sedimentation, a means for discharging the settled
solids is essential, hence we have provided the thickener mechanism.
The clear brine coning from sedimentation tank is to be acidified with
muriatic acid before feeding to the cells, and we would recolilllend the designing of
a meter which will measure tho above solution to an acidifying tank. which meter would also control the addition of the requisite amount of acid.
On the operation of these stations we have allowed one man per shift
for operation of the evaporator and one mroi per shift as helper who is also to
operate the brine purification and salt washing system. As it is planned to have
all of this process as automatic as :possible, such provision as we have made would
seem ample. l!'or the mechanical attention required we have allowed one repair man
per 24 hours. It will be noted that we have alreruly provided one repair man per
24 hours under tho cells and it is our intention to provide a third man under
Barium House. It is our idea thus to provide one repair man per shift for the f'Ull
24 hours operation.
For the operation of this station we estimate 55 KV/ will be required,·
or a total of approximately 1330 KWR per 24 hours. Al though this will be supplied
from steam ahead of our evaporators at a cost of from 3 to 4 mills per KWH, we
have chareed it into our estimate at 7 mills. the same as would be charged for
On supplies we have provided for two tons of salt per 24 hours to make up our losses at ,15.00 per ton. This price should be ample for this material laid down at our plant from the Kansas fields. As a factor of safety, we have
allowed for the use of 2 tons per day as against our estimated requirements of 1.5 tons. We have also included one ton of 10 Deg. muriatic acid per 24 hours at a cost of i60.00 per ton, this in spite of the fact that we expect to produce
this ac1d in connection with our daily operation at a coet of possibly one half the above. 80 lbs. of barium chloride required for removing sulfates from brine is
charged at the rate of wl00.00 per ton laid down at our plant. The coal consump-tion of this station we estimate at 16 tons per day (based on figilros previously
given) at a cost of ~5.oo per ton delivered.
Maintenance charges on evaporators will be colD!)a.ratively high as has already been pointed out and in the absence of a more definite basis of calcula-tion we have allowed 4~ of the estimated cost of our installacalcula-tion, namely,
..-15,ooo. In addition to this, we have allowed ~1800.rm per year each on the salt washing and brine purification systems. (For details, see Operating Charges, Items 2.220 to 2.224 inclusive).
Partial specifications for equi'pment are as follows:
1 - Only - 30' x 8' Dorr Thickener - mechanism and super structure complete.
1 - Only - 16' x 16' Dorr Agitator - meohanism and super structure complete.
l - Only - 5, X 7, Wood Tanlc
1 - Only - 5, X 12'
"
,,
2 - Only - 6' X 8' pt
"
2 - Only -14' X 15'"
,,
Byers pipe to be usad from acidulated brine storage to cells •
l]Y.drochloric Acid Station
~rimental:
Hydrochloric acid was produced by burning the hydrogen and chlorine from the electrolytic cell in a cl~sed furnace. (See dwg. No. 405 R.L.l
The rurnace was bull t of fire brick with a. oombusti on chamber 6" wide 8" high and 12" long. The back one-half of the combustion chamber was la.id with checker work to insure thorough mixing and complete combustion of the gases. The
gases were led into the furnace through a stRndard fused sil ioa burner made by the Therual Syndicato ~o. Lead and iron pipe were used to _conduct the chlorine and hydrogen respectively to the burner. li'used silica pipe, ''Vitreosil ", was used to
carry the hot HCl gas to the to,Ners.
About
lcfp
excess hydrogen over that produced by the cell was used in the furnace to insure complete combustion of the chlorine.Special precautions were taken to make the 'furnace and all pipe lines air tight. The presence of oxygen causes the formation of oxygen-chlorine com-pounds or requires an excessive amount of hydrogen for combustion.
A gasometer was put in the hydrogen line to serve as a vent in case of explosion.
Design Slld Operation of ?roposed Installation:
The operation of the hydrochloric acid fur~1.ace is de-pendent entirely upon the methods of installation and operation of the cells. mine practically no difficulty was encountered. on our smnll scale operations, we recommend that every possible effort be made to render this station foolproof and to guarantee constant operation. With this in mind, we recommend an installation of not less than eight or preferably twelve furnaces. ~he lareer 11umber of units, while it complicates operation and installation somewhat, has the ~pparent advantag-e of reducing the volumes of gas and chances for violent explosion in ar;.y one unit. !he methods of lighting and starting a hydrochloric acid furnace as known to us are very crude and accompanied with some explosion risks.
Espeoially is this true after shutdowns of short duration whon sufficient care may not have been exercised in :freeing the combustion ohamber of unburned hydrogen
be-fore applying the toroh. To eliminate this lighting operation as far as possible, we believe it essential to draw the gases from the oell installation to the indi-vidual furnaces in such a way as to insure against shutdown of the furnaces. With this in mind, it seems advisable to connect a furnace with a certain number of oells in each series of cells in the cell house so that if it should beco~e necessary to shut down one cell circuit for a few minutes, the furnace would oontinue burning with gas from the other series at a lowered capacity. This would eliminate furnace shutdowns due to difficulties with cells.
The next thing to be provided against is shutdowns of the entire cell installation because of rotary or power supply difficulties. It will be remembered that we have recomnended. a motor generat,r set with 2000 amp., lf5 volt D.C. capacity for supplying the hydrogen cell requirement. This set is of sufficient size to sup-ply 12 - 2000 amp. chlorine cells in addition to the hydrogen cells. However, we believe it advisable to install these chlorine cells to be operated from the motor generator set, the latter to be installed ond be operated from either our power
(steam) or from purchased power. (The former is preferable beoause it furnishes an independent supply.) The gas from these cells will be piped to the furnaces through an independent system and utilized in pilot burners. In this way. operating diffi-,,. culties would be materially lessened..
With 12 furnaces installed, arrangements for cutting out any four
fur-naces so that eight can carry the full load will be desirable. 'l'he burners on the furnaces should be made of Vitreosil pipe, the inner. or chlorine lino to have an
inside diameter of
1f•
and an outside diameter 2-1/8, while the outside pipe (Hydrogen) should be 2-3/4" inside diameter with the ''Y" connection l¼" diameter inside. This gives an average velocity, operating f'urnaoe at full load, of 960 ft. per minute. This figure should be checked against manufacturers' reconunendations as it is based only on short experience at the experimental plant. The coobustion chambers, based on our experience should be at least 12" x 12" x 48" long. This recommendation should also be checked if we can get the available data. These furnaoes will 'Pro-duce a total of 18.:-s
tons of HCl per 24 hours.We would also recommend individual acid lines of Vitreosil pipe from each furnace to the towers, these linos to be supplied with jug dampers and
ar-ranged so that all furnaces can be operated in connection with either set of towers desired.
As to operation costs, we believe that one attendant per shift will
handle the furnaces. The gas pumps from the barium chloride towers should also be under this man's control as he should control the vacuum under which the cells are operated.
No power will be consumed directly on this station as the pumps will be charged to the towers.
To cover supplies and maintenance we have allowed ~1060.00 per year. This should be ample as there w.l.11 be practically no maintenance on the furnaces proper and the silica pipe will last indefinitely, except for accident.
Substaj;ion and Repair S1'!2J2,
The substation will receive purchased power and is to be equipped with the rotary converter and motor generator set specified below.
One man per shi~t will be ample for its operation, while for supplies we have eight sets of brushes at ~100.00 per set per year which, to-gether with oil and miscellaneous, runount to t4.50 per day. For maintenance we have allowed ~1000.00 per year.
The repair shop listed here amounts to a work room for replacing electrodes and diaphragms in the chlorine cells. The repairmen specified under overhead will man it and aside from power and maintenance or poRsibly a drill press and planer, no charges have been made against it.
Partial specifications for pro~osed installation are as follows: 1 - Only - Rotary converter - type H.c.c. - 16 poles 2200 K.W.
450 R .P .M. 590 volts maximum 4000 a.MJ:)S. 6 phase ...
60 cycle - shunt field winding efficiency at unity power factor to be 95 or better at full load and 93 or better at 1/2 load weight of machine 67000 lbs. height overall -104" length 151 .. , width 115''. 1 - Only - Aluminum - cell 3 phase lighting arrestor complete
with tanks ,horn gap and disconnecting switches. 1 - Only - Operating lever with trip coils combining overload
and under voltage protection. l - Only - Reactive volt ampere indicator. 1 - Only ..Armneter.
1 - Only - Watt hour meter.
1 - Only - D.P. inverse time limit reley.
3 - Only - Single phase type
w.c.c.
60 cycle, 900 K.V.A.13200/6600 volt primary and 405/2025 volt secondary
water cooled transformers w'i th 10% tape above ond below 13200 volt windings.
Undltr t.b.1 a he ill e oond eN4.
i.,,
U.11 l a a.ncmat.eorweraloa atattcm for ooth
ISU't•
Oul»onate a:nA SU1pb14t; 2nd, \beBari• Chlol"i • solutioa purltl a\l
tor-
NDllY•lot
1rOA ancl orpmc•It.l's
3 •ua
1•
~ ahnotpl tat~oa Stat.ton,
•th•
~ Jutsacta
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botban•
oar'bou\l and. •ulp
t
ac..
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bli!R!rwnt.l
.
Jart
car
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Cal'bouttoa tiltu·•
na
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(1'I x ,,a-
wood at.aTe"-*
pro't14e4with
a
41.e ara 1.ta\or a.ncl.a.
U,P oa
•lwt
tb undel" tlowtroa
lh•U'l• o lor141 Ni'1bc tank. tbl ooa»0aUloll
ot t
eladpwu
out 11"la
UOs• 16-18
12•
u4. U•lance wa'9r. It ... uoenaq to
Mba
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ot
th1• coa»oalUcn 1D ordel' o oota..llla
IO'INrt••
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at tbl • • • tilu pr011uoe a kriua oblo,.lde aol 110'1ot
w
req tNd con.c ntrat.ioa (uoat I~ - U c12 ltJ wt) ..
! tower• (tbNt la naabtr) Nft 1t11l1t ot 18" •1bltle4 unr pipe au4 pao.imct In 'tht
nplu u7, ao
to ha.ff ~ •old•• with:1-1/2"
z
1-1/a- wood. pe.cldng~ Blx. and. one-half feet of paoktng . . .,. pa.,illto aaob
ionr.
.i.\owera
weJI••t
in
30• 1 . . .*'l'
wooto. •·
( e
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e8 .~. &36
.L.) •
.A
l" SW
1n,i-ttqal
ptlllJwu
provtdall
ineach caae to ciroula•
the al · h'CII tbe
t
01'er the top of tbe t.ower. th• ROlcu
troa
tlMl ,r.,,..wu
le 111 Jut at.err, 1beaolut
!OD l•ftl 1Jlt
erf 1.
fbe 002 to.NIAb7
tile aot1011ot
the aolil on \bl b&rta O&l'bOD&te t t?er wl tll ..&llJ'Q.1'.lCQllbllltcl acl4 waa taken
ott
th• toot
the towr a:ad. tntro4:acc4 intotower
fl•
tollowt
\Maaae aotaae throa,gb.Oai
. , . , .
aa 4-I01"l 41.tor
fl'Oll
tc.r
fl,. D.1•
~uat.er •1nta1Dt4 a
au
tvaou• on
the•utt.re
towera,a,aa.
theRCl
fl.U'naaeand
,ne
cel.l., fba Ytle\'tUIIIamounte4
to &bwtl/4"
Ofwater a
ell an
•
• • tht
albltntt1
1n t&ftl'f
l.
wa.11
N4UtHl toa,ou,
i
i
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\he eolut ton wao pa11p1:d
to
tba ltul chloride utilintau.
i haaI
waa pampe 1atot
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flwaa
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ta
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·
curs-
l1'0lltb.e alu4
mtztug tank.!'he te :.el'&tVe
t
\ne
sl 1a towel'• f2 c4- 3wu
bp, at,o
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~
.
lt wu 'foWld n.oe1aa.r., to al:ntaln these t.a,p1i-at11ne topn
.
...
Collied th• t.,_l • .&t Id . ~ tdptl"at.urea wr-7 llt\le t-car
w
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nne
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ot
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gtWJeo,.;rr,oeomu\ &uJ!lA!tl:D
~ 4 or.a. v •x,pertelt(lil 1n tha e:pcut menw work • • abaorpt 1oa of' hya.rocnlorf.o. ac11l gae ma alll4j'I ot b&rlWD o vona e aD1 b0.1-1 Chlo.ria.
aolut1on (approxt•i.
oampordtt@ anOMi alK»vt) wtl.1 nqul.re&llout
12& 011.tt.ot
t
r-apace
pel"taa of
l abaorbe ,per
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tthla 11eoeatdiai,a •
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ot
tower a.pace(b>.cluding paokt.ng). !hi• ul.4 neoe .. ltah an lnatallat!OU of & tower••
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•»wJ•
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ln 41auter. bl a4d.U1on to t.h1a it l•oeea&17 t.o prov!
a apace a o••
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or '1:te
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e
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or
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a
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1 • erhn ,. f.bftao
t.01'1
whiohraptd. H'Odon o ed
bJ'
the apeolt •
1A•~ •oul at1 ate the probable lUe ot 004 pa.old at att aont;ha.
prea n\1 oonat&erable
wt
\.
heme • 414
e carried
1
th• U 111 o~ I.be toqr- oJt>allla.1011
•x•te•
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