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lyt -efloiJpcp
Trong phng th nghim, tin hnh mt qa trnh in phn nlV m in, cc. tinh luyn kim loi, in
phn ch to cc ho cht, tng hp in ho cc cht rtQ hu c ...u phi dng cc thit b v dng c
chnh tfc ni thnh mch in w nh-tf hnh 1.1
Bin thB thng dng loi v cp. in t mng ii 220V, 50Hz nbc bin th h
xung 0, 6, 12, 18, 24V ...ty theo nhu cu bng cch xoay nm vn. Th h p cng thp
th th v dng mt chiu thu tc s cng thp v
nc^G li. frtfc khl th nghim phi th h p mc b nht (=0 V), chun b mi -
. oA
r
_0 ~\J~ :.:; j
Khi tip im T chy n im a cui bin tr R) th in th E ca ngun ri ton b trn bin trd E
= En, v s 0. Khi tip im T chy n im b u bin tr Rb th in th trn bin tr Eb = 0 v 1 =
E/Rdd. Khi tip im T nm trong khong gia a v b th dng in 1 trong mch thay i 0 n s=
E/Rdd. in tr ca amporet rt b c h b qua.
Bin tr c th dng loi in r con chy, hp ln tr ...
mpemet mi em A : phi dng loi c khong o s v vch chia ph hp vi th nghim. Nh
mc ng chiu + v - vo ng h o. in phn, m, oxy ho nhm. ...ch cn ampemet c cp
chnh xc 2 S v vch chia khng cn phi nh hn 10 mA. Dng din cc i trong cc th nghim
th- ng c 5A.
Von m t v mlvo 171 t mt ch i khi cng #bc dng trong cc th nghim ny v lun phi
mc song song vi bnh in phn theo di bin thin in th ca bnh ny trong qu trnh th nghim
(khc vi vonmet trn my Chnh ^u ch in th u ra ca chnh ti). Trong phng th nghim thfl$fng
dng loi milivon mt t 150 mV tr ln v von met trong khoang 3 n 15 V (c 150 vch chia). Ch
mc ng chiu + v - .
B nh in phn c th dng cc thu tinh hay bnh c dng c bit bng vt liu bn ho nhitgm,
s, thu tinh, cht do ...Nhiu trng hp bnh in phn cn phi chu nhit, khng b bin dng, v khi
gia nhit. Bnh phi c cu to thun tin cho vic g lp cc dng c o, khuy, tho lp in cc v dung
dch.
Gia nh cho bnh in phn c nhiu cch :
un trn bp in c b phn iu khin c^ng dng din un. Khng t trc tip bnh in phn
ln bp in m phi c tm tyi amian ngn cch gia chng. Cch ny n gin, tin dng nhrfng
nhit dung dch bin ng nhanh, cn phi theo di cht ch v iu chnh kp thi.
t bnh in phn trong thit b un cch thu c b phn iu chnh nhit . Cch ny nhit dung
dch bin ng chm hn v lun bin ng theo sau nhit ca r^c. Ch nn dng un dung
dch ln nhit khng qu 60 -70 c.
t bnh in phn trong bp ct v vn hnh nhtf khi un cch thu nh- ng c th un dung dch ln
100c hoc hn.
Dng my n nhit bm lin tc dng nttc nng c nhit khng i vo o n-c ca bnh in phn
hoc ng trao i nhit t trong bnh in phn. Sau n"c tun hon tr v my n nhit v
^c un n nhit quy nh v tip tc chu trnh khp kn . Cch ny gi nhit rt n nh,
chnh lch nhit gia ntc v dung dch b v gn nhbf khng i. Bnh o cc thng s ca
phn ng in ho phi dng cch gia nhit ny.
Khuy dung dph l/c thc hin bng cch dung cnh khuy thu tinh do mt quay v c the
iu Chnh t-c tc quay ca n. Cng c th khuy bng my khuy t : con quay l mit nam
chm vnh cu lng trong ng thu tinh hn kn tc th vo bnh in phn. t bnh in phn ln my
khuy c mt nam chm khc dc quay theo lnh iu chnh tc , to ra mt t trttng quay, lm cho
con quay nm trong bnh in phn quay theo khuy dung dch. Thng cc my quay t c lp thm
c bp in iu khin 4/bc ng thi va khuy va un dung dch.
Bn cm : in cc dng trong th nghim in phn c nhiu loi khc nhau v vt liu cng nht'
v hnh dng. TMng th chng y&G lm bng kim loi, hp kim, grafit ...c hnh dng i loi nhu)hnh
1.3.
Hnh 1.3 Hnh dng in cc dng trong th nghim in phn
Cc in cc ny c th dng lm anot hay catot cho cc bnh in phn trong cc nghin cu R
in ho. Khi khng yu cu phi khng ch cht ch mt dng in trn in cc c th dng in k
cc dng a, e. Khi cn khng ch chnh xc mt dng in dng dng b, c, d. Phn din tch in
cc khng
cn Sm vic c th cch in bng parafin, sn epoxy, bng dnh... Din tch in cc " c tnh c hai
mt (k c mt dc theo chiu dy mu in cc nu cn). Tr-ng hp ch cn cho in cc lm vic
mt mt th mt kia phai cch in bng sn epoxy, sn elovinyl, polysterol, parafin+sp ong, bng
dnh ...
Mu nghin cu n mn th- ng c dng bn, dy, thi vung hay trn. Mu cn nghin cu
c S tnh sau n mn phi ch to theo yu cu ring v hnh dng v kch thc theo quy nh.
Cc mu thong c khe, l, quai .7. kp, treo mu. Gi , mc treo, kp mu phi bng thu tinh
hay vt liu cch in bn vi mi trng th nghim n mn. Hnh 1.4 sau y trnh by mt s
hnh dng mu v gi mu nghin cu n mn.
i kh cc u mt, cc ra mp v nhng ch c bit ca b mt mu cn thit phi cch ly
vi dung dch theo yu cu ca th nghim th lc phi trt hay sn ph chung bng sn dovinyl,
polystyrol trn vi toluen thnh bt nho hay parafin un chy vi sp ong hoc dng bng dnh c
bit.
Hnh 1.6 in 1- ng
k ng.
Dung dch ca in l-Mng k ng gm :
CUS0 .5H20
4 125 g/l
H2SO4 (d 1,84) 25 m/l
R= du etySic C2H5OH 50 m/l
ic 1 - 2 A/dnrr hin tng sinh kt ta ng ti, xp, bm km ln ln
catot do nng Cu2+ b ngho dn pha trn v st
Nhit phng.
catot.
in S^ng k tc mc ni tip vi bnh in phn cn
o hiu sut dng in vo mch ca hnh 1.1.
Hiu sut dng in thot kim bi trn catot ca bnh in phn - c tnh nh- sau :
H = 31,785. mS;100/aC , %
Trong m0 - trng yng thc t kim loi thot ra trn catot bnh in phn, g, c - trng Wng ttong
Wng ca kim loi y, g, a trng litng thc t ca ng kt ta trn catot in Mbng k, g,
31,785 - trng feting ibng tog ca ng, g.
Chng 2
CHUN B CHO CC O C IN HO
fi- *
Ch-ubng 1 ni v cc cng vic cn chun b cho nhng th nghim mn hc,
chi&mg 2 ny s trnh by vi nhng vic cn chun b cho cc th nghim c in ha
phc v nghin cu khoa hc, lm lun vn tt nghip i hc hay thc s, tin s...
2.1 S khi mch o in ho tng qut
Khi nghin cu mt qu trnh in ho din bin trn in cc theo mt ph- ng
php, mt k tht no th- ng phi dng n mt mch in t- ng t nh- s khi
tng qut hnh 2.1 sau
SPU PC Hin th
Phn mm M
My pht
Pot^Gal.
Bnh o in USJ
ho
Hnh 2.1 S khi tng qut mch o in ho
Thy rng loi thu tnh no c hm S- ng oxlt kim loi kim cao th bn ho
cng km. Loi no c" hm 1- ng xit ban, canci, ch, mage, km cng cao th bn ho
cng ln.
i khi ch vi cc tp cht t thu tinh tan ra cng Sm nh h= ng
n s din bin ea qu trinh in cc. V d khi kh trs ho cho anlon ferixyanua trong
cc bnh bng cc loi thu tnh khc nhau S! nhn - c cc kt qu khc nhau, nh- trnh
by trn hnh 2.2.
VI vy trong nhng r-dng hp c bit c th dng vt iu khc lm binh o hoc
phi dng mt ho ht n v hiu ha cc tp cht tan t thu tinh ra.
Nu tr- dng hp sn phm phn ng in cc tan vo dung dch th chng s
khuch tn sang in cc bn kia, v c th tc dng vi sn phm ca in cc y gy nn
sa s ong o c. Khc phc hin t- ng ny bng ch ngo ring khng gian atot v
anot bng mng thuf tinh xp ho tr- dng hp n phn khng qu Su v bng van thu tinh
nhm ho tr- dmg hp in phn Su.
0^4 0*8 1,2 1,6 2,0 -, V (SCE)
Hnh 2.2. - ng cong phn cc kh in ho
anion Fe(CN)63 trong dung dch K3Fe(CN)6 3,3.1(rtVL
1 - Dung dch mi pha ch; 2 - Trong ung dch c bt thu tnh yense ;
3- Dung dch ng trong bnh o bng thu tinh molipden 24h tr- c khi o;
4- Dung dch c bt thuy tinh molipden ngm 2h tr- e khi o;
5- Dung dch c bt moipden ngm 24h tr- c khi o.
Ngn bng van thu tinh nhm s lm in tr ca h tng ln rt nhiu, lc
phi dng ngun in c in th ln (c th n 80V) dng din i qua t c- ng
yeu cu. Nh- ng - ng hp ny khng nn dng c- ng dong qu ln, v khi i qua
van s lm n nng ln, nh h- ng n tnh ng nhit ca th nghim.
o sc in ng ca h;
Thit lp - ng cong mao qun ...
Th nghim cn phi n nhit th dng bnh 2 v lm o n- c trao i nhit hoc ngm
cLbnh o vo my iu nhit.
Bnh o 3 cc (hnh 2.5) th- ng dng :
Nghin cu cu to lp kp;
Nghin cu ng hc cc qu trnh in cc;
Nghin cu cc hnh vi n mn vt liu;
Tng hp in ho;
in phn...
B phn chnh ca bnh - c t in cc lm vic w. Mun phn cc in cc w
bang dng in ngoi phi nh n in cc i c t mt ngn ring, c van 1 cch
ly cc sn phm in cc. in th ca in cc lm vic w khng o -c bng (Tin cc
i c v kh c dng in i qua in th ca in cc C s thay i i (khng const), mt
khc in tr ca lp dung dch gia cc in cc, nht l ca van 1 rt ln nn in th ri
trn chng rt ng k v kh xc nh. VI vy o in th in cc w phi dng in
cc so snh R . in cc ny khng c dng in phn cc i qua n, cng khng b phn
cc nng trong khi o nn in th ca in cc so snh khng thay oi trong sut qu
trnh o
sinh ch chy ri, nht l lc quay vi tc ln. u mao qun ca cu mui cng c
the gy xo trn ch thu ng ca dng chuyn ng dung dch.
in s m-v&ig quay ch to cn phc tp hn. in cc da lng p
vo mt ng cch in mng, ri lng in cc vng ra ngoi, ni u tip in, cui
cng lng p vo ng teflon bn ngoi (hnh 2.8).
0,000 - - 0,244
- Hatr 1M ZnlZn2* 1M
1 g004
0,076
SHE SCE
Hnh 3.13. So snh cc thang in th dim cc.
Hng tun phi ra binh bng axlt oxalic ho tan cn, oxit mangan bm trn thnh
bnh, sau phi ra li bnh bng n-c thdmg trng Si bang m~c ct.
M=c ct thu -c theo ch hnh 2.14 ni trn 6 dn in n nh, khng thay
i trong khong % = (1,0 - 1 .S.IO"3 ft-1 rrr1 25c . dn in ring c n- c sch l
ng pH 7 v 18c l X - 3,8.10^ Q~1 cm"1. Vy n- c ct hai ln, ba ln vn cn cha nhiu
tp cht. C th thy r iu ny qua cc cc i cfia cc ng c ph trn hnh 2.15.
N- c ct hai, ba ln c th dng nghin cu cc qu trnh in ho, n mn c
din tch b mt ln, cn nghin cu ng hc cc qu trnh in cc v nghin cu cu
trc bin gii cc pha trn in cc rn cn phi dng n- c ct nhiu ln v hp ph ht cc
cht hu c bng than hot tinh (nh- -ng 5 hnh 2.15). Mun v phi cho 2 -10 g/l than
hot tnh vo n c v gi trong 12 - 24 h, ri lc sch tr- c kh dng.
Hnh 2.15. - ng cong phn cc trn in cc git thu ngn (T = 15s) trong cc dung dch HgCh
2,5. l-4 M + K IM pha t cc loi n- c ct:
1 -n-e qua trao i ion; 2 -n-e ct mt ln; 3 - n-c ct hai ln; 4 -n-e ct hai ln ri ct
tip trong thit b hnh 2.14; 5 - n- c ct nh- im 4 c lm sch thm bng than hot tnh.
4 - cc thu.
2
Chng 3
CC TH NGHIM IN HA
VON AMPE VNG TR|N N c: TNH
1.1. Mcdch
Dng phng php von ampe vng (cyclic voltammetry) xc nh h s khuch tn D
ca mt h oxy ho kh, nhn xt v tnh cht thun nghch ca phn ng.
1.2. C s i/thuyt
Trong phng php ny in th 9 d/c bin thin tuyn tnh theo thi
gian X (hnh 3.1):
9= 9<J - VT khi 0 < X < X
v 9 = 9<J - vX + v(x-X) khi X>x
trong V - tc qut th, v/s
X - thi im i chiu qut th;
T - thi gian , s.
9 - in th ban u, V.
Q A d. I y ) J
;
M 'i %7
2. 297 K c tc f p,a - fp,c = 59 mv/n (tc khng ph thuc
qut th v);
3. 8 p,a / 8 P,J 1 .
v
O. Pung dch v bB? @: '
Cc dung dif H2SO4 c nng 03001 r.0,1 mol/s.
Binh o 3 cc8 gm w = bng Pt hay Au, c = bng P'.................R'"='in ec calomel
HA s<di@fc: hnh 3.3:
hi= i Mu chng trri $@
Chtng trinh o
mnh3
Ptentostat AOCyDAC PC Lu tr
Cho dfa mm (ghi chng rtnh o) o A ci my tnh PC,
Goi ch|?dng trnh theo mt mi. V d : > Lin,
Say khi chng 'trinh o hini ra lm ip c b:
- B& hp sng n start measuring. Bm Enter. ^a hp sing n Remark. Gi cs s, ghi
k hiu dung d|ch nghin cu. ng csi s.
- Chinh khng: hp sng n Zero adjust Lm ng tc chinh 0 mh4 mn
hnh hmg dn.
- io f,: ^a hp sng n Auto checking Ur. Enter.
- t gi tri in th u v cui.
- Chn Measuring mode (single, cyclic). Nu chn single thi dt hp sng m Change
otier value. Enter. t Tsample - 0,1; 1 ...
Nu chn cyclic th ghi Potential rate cn thit
- la hp sng n Do measure. Enter. i chung ku. Enter.
t hp sng n Draw graphics. Enter. Enter.
- a hp sng n Graph treatment Enter.
- Bm B. Dng mi tn trn bn phm dl?a con tr n on tng cong cn
thit Bm E. Enter. -
- ^a hp sng n Smoothing. Enter.
Ghi vo Number of repeating: 3. Enter.
Ghi vo Number of point : 3. Enter.
- Bm Esc.
- Ba hp sng n Sam to disk. Enter. t tn cho cHmg va ghi.
t - - AsA
0 %h
ll v, ,11 c% :
' iJ
p ^ tl K/ ^- '
_ rity
1.5. Tin hnh th t nghim :
- Chn khong in th, v 0,5 V d t 0,5 n
- Chn tc qut V = 0,01; 0,02; 0,05; 0,1;
0,2
^r
1.6. Nhffng s liu cn bo co s
- Th cc i anot v catot,
- Mt dng catot v anot cc i
- v th ip,c = f(v1),
IP, 4 >
..
tt { CVd l
t w, /N
)0 film.
1
. t M .
it ^ ttk (tt
& rS _
,94 J .
dM
c
ttc* \!1 tt . as,
C:,
0 A ; }'
(,
% M-H.
/
ill
Y r-
0,4 4N
tc o. ^
B 3
VOLTAMMETRY TRN IN ce MA QUAY
31h My i ( :
Dng ph og php qut th ln in cc a quay xc mh s ph tiuc ca dng khuch
tn gii hn vo tc quay in cc v xc nh h s khuch tn D ca mt h xy ho - kho
3ol * 8 thuyt:
Trong th nghim ny, mt h oxy ho - kh - C t d i iu kin khng ch khuch tn .
Red -> Ox & ne (1)
S din tch trao i n 1.
- ng cong phn cc - c ghi diu kin potentiostatic nh- hnh 3.8.
'>' Hr
-1C.-16 M'
0$^
lfM It tl H Utah Jk jiir m {ck"1 *> ^?
XC NH Tc N MN KIM LO I
BNG PHNG PHP O UNG CONG PHN ce
i.1. Mhim v:
2
Xc nh tc n mn ca st trong dung dch H2SO4 1N khi khng c v khi c
mt KI 1Q-4 N bng ph= ng php in ho o = drsg cong phn cc.
SdL St i $8 nghim :
5
Hnh 3.11 S th nghim t tc t in mn
1. in cc nghin ot w
2. in co ph c
3. in cc 10 inh R
4. Binh
5. GaSvanostat / Potentiostat
Php o ny = G thc hin vi mt h tsn ho gm in cc nghin cu, in
cc so snh v in cc ph. Trong din cc ph c din tch cng 8m cng tot, cho
s phn cc trong binh o khng bao gm phn cc ea in cc ph.
So3o Chiin te th nghim :
Sau khi p xng cc thit b o theo s , o & ng cong phn cc ca st
trong cc dung dch rn cn chun b:
- in cc nghin cu : ct mt ming st c din tch khong 1,5 = 2 cm2, em da
pava, ty du m, ri nh bng bng giy nhm hoc bt thu tnh. Sau lau sch
bng giy thm tm (n hoc kston r trng bng n~ c ct tr- c khi th nghim .
- Dung dch nghin cu : chun b t ho cht sch v n- c ct
Dung dch 1 : HaS 1N,
Dung dch 2 : H2S4 m * M 10-* N.
- in cc so snh : dng Sn cc calomel bo ho.
- Bnh o - c ra sch bng H2SO4 c, sau ra tip bng n- c (khng t hn 6
ln) v trng li 2 ln bng n- c ct.
5.4. Cch tin hnh o :
Lp cc thit b o v bnh o sao cho khi nhng in cc st nghin cu vo
dung dch th l im ni cui cng ca s o.
Sau khi lp ton b th nghim, chng ta phi lm sch in cc bng cch
phn cc catot n trong vng 30 pht vi dng in 1+3 mA. Sau o qu trnh phn
cc catot t gi tri dng ln (khong 10 mA) n gi t dng nh v mi gi tr ca
dng n lc gi t 1 n 3 pht hoc gi n khi gi tr in th c t- ng ng t n
nh mi ghi li. Tip n ta ngt dng ( = 0) o in th n nh q>cor (in th n
mn). Sau khi o xong qu trnh phn cc catot v in th n mn ta o cc o tip
qu trnh phn cc anot theo h- ng t in th n mn n in th d- ng hn, c
ngha l o t gi tr dng nh n gi tri dng ln, mi gi tr la gi khng nhiu hn
30 s v ghi li gi tr in th anot t- ng ng pa (mi qu trnh phn cc ta o t 10 n
15 gi tr).
Sau khi th nghim kt thc ly in cc nghin cu ra v o chnh xc phn din
tch in cc nhng trong dung dch (S).
o trong dng dch sch H2SO4 1N tr- c, sau thay dung dch v thay din
Cc st mi o trong dung dch H2SO4 1N + KI 10"4 N.
5.5. Kt qu th nghim :
T cc s liu thu - c lc, c, la, a v din tch lm vic ca in cc st (S)
qua cc ln o trong dung dch H2SO4 1N v H2SO41N + KI 10^N ta xy dng cc - ng
cong phn cc - Igi trn cng mt th.
Sau khi i xy dhg c ~ ng cong phn cc ta dng ph ng php ngoi
suy xc inh tc n mon. Ngoi suy c th = c tin hnh cng chnh xc nu
" ng phn cc cng thng. Trn - ng phn cc catot; anot (hoc c hai) khong
mt dng trng bnh (c ngha la khng phi ong min gn
din th n mn, cng khng phi trng min phn cc qu ln) c mt phn l on
thng th ta ngoi suy t phn thng ny n in th n mn cor xc nh dng n
mn oor . ngoi suy - c chnh cc th trn cc nhnh ca - ng cong phn cc
phi c mt on thng trn min in th ln (khong 50 = 100 mV). Tc n mn
-c ngoi suy t c hai nhnh, v t hai nhnh cn phi cho cng mt gi tr lcor
Nhng kt qu Gn r m:
a. Tc n mn ca st trong dung dch H2SO4 1N,
b. Tc n mn ca.st trong dung dch H2SO4 1N + KI HCHlN,
c. So snh in th n mn, tc n mn ca st trong cc dung dch trn. Rt ra kt
lun v tc dng ca KI i vi qu trnh n mn st trong dung dch H2S4.
53
Bi 6
XC MH Tc N MN KIM LO BNG o 7 PffljONG
PHP TRNG LNG V PH13NG PHP THTCH
ft
Ph= dng php trong != ong l ph ng php trc tip da vo s thay i trng i- dug
c mu kim loi (Am) xe nh tc in mn. cn cn mu tr- e v SSU' kh th nghim
xc dph Am.
Am c th l gim trng s~ ng ca mu kim loi trong thd gian th nghim X (sau khi
sn phm n mn =e ty sch khi mu)
Am c th l s tng trong 1 ong ea mu kim loi trong thi gian th nghim X.
X anh tc n mn kim Soi bng ph= ng php th tch S du vo I- ng kh
hydro thot ra hay s= dng kh Ky gim i trong dung d|ch trong qu rlnh n mn tnh ra
tc n mn.
@J. Nhim v:
Xc tnh tc in mn st trong dung dich H2SO4 1IM bng ph= dng php
trng l ong v ph= og php th tch.
doi. M &o
nghiiMi s Hnh 3.12 :
A
/\
Nh- ta thy trn hnh 3.13 vng n mn hot tnh, cn gi l ho tan hot tnh, ea
kim loi = c phn bit vi vung n mn th ng bi in th th ng f p ; vng th ng c
mt dng in thp nht c tnh t in th Flade p n in th fT (S in th thot
oxy). Trong vng ny kim loi nm trng thi th ng gy ra bi mt mng (th-dng l oxt) st,
hu nh= khng c l thng. S hnh thnh hay bin mt ca mng ny xy ra trong khong
in th t <PP n f F o Min ny - c gi l min to mng th ng hay min chuyn tip.
Mt s oxt kim loi c c tnh bn dn (v d nh oxit ca cc kim So Fe Ni, Zn 4 .
Bs vy in th ddng > fT , mt dng bt u tng khi tng tip in th, do thot
oxy theo phn ng :
2H20 - 4 -> Oa + 4 H"
Ngoi ra cn c mt s tr- ng hp qu trnh n mn li vn tip din in th <p > T
, do mng oxit ho tr cao c kh nng b ho tan . VI vy vng ny cn gi l vng qu th
ng.
S to mang th ng c ngha thc t to ln v nh m tc n mn gim i
ng k. Chiu dy mng th ng c th l vi nanomet, cng c th dy n hng 100nm
i vi kim loi nh- AI, Ta, Ti ...Chiu dy mng th ng ph thuc nhiu vo thi gian th
ng v in th.
i vi Fe, mng th ng gm -Fe203 v pha dung dch v Fe304 rt mng pha kim
loi. Trong dung dch axit, Fe kim loi -c bo v nh mng Fe203, cn trong dung dch kim
nh mng Fe34. i vi Fe v mt s kim loi khc nh- Cu c th xc nh - c th tch
mng oxit v do s tnh - c chiu dy ca mng oxit. Ph- ng phap nh- sau : Sau khi to
mng th ng mt in th no trong vng th ng , qut in th v pha m, se
xut hin mt pic catot Din tch d- i - ng kh l in I- ng Q cn thit ph b mng.
Q quan h vi chiu dy s ca mng theo cng thc sau :
5 = Qv / nFSr (1)
y V - th tch phn t oxit, - hiu
sut in tch, s - din tch
in cc, r-h's g gh.
Chiu dy mng oxit s thay i theo thi gian th ng X tun theo ph-ngtrnh:
1/ = B - m.lnx (2)
ym = RT/anFaA<p
A<p - in th rdi trong mng oxit, a - khong
cch n b mt kim loai, n - s in t trao
i, a " h s chuyn vn in tch.
C theo ph ng trnh trn th d- ng nh thay i thi gian X l c th to -c mng th
ng c chiu dy bt k theo mun. Trong thc t th khng phi nh- vy, v s ln ln ca
mng s drg li kh phn ng to mng t n trng thi cn bng (mt dng to
mng im 0). iu c ngha l : tng mt dng to mng im v mt dng n mn icor
ng bng mt dng th ng p.
Thay i thi gian th ng X iu chnh trng thi n dnh ea mng nhm kho st
gi t m trong ph ng trnh (2).
7.3. Tin hnh fh nghim v inh gi k qu
Gc th nghim sau y - c tin hnh vi in cc Fe v dung dch m phthalat pH
4,9. Tr- c khi o, mi in cc bng giy nhm mn. Sau phn cc in cc ch kh
ti in th - 800 mV trong 5 ph. Th nghim ny gm ba phan:
TJ.f. &@ i= ng <smg iphn cc
o ng cong phn cc ch dynamic (qut th v ghi i dng p ng). Tc
qut th 10 mV/s, t in 'th - 1000 mV n + 1400 mV (SCE). dng rong phn c thu -
C ch thy mt cch nh h- ng cc gi tri in th v dng, cc vng trn .
Bnh gi: Hy dh! ra cc gi tri sau:
in th hn hp ca qu trnh ho an F@ v thot Hla. o in
th th ng; o in th Fis o in th bt u thot xy, .
Mt dng in ti in th th ng, o Mt
dng din b nht vng th ng.
O2o ph thng m w@ 1? ;
S ln ln ca mng oxit (mng th dng) & c nghin cu Hn 'th P 2 = ioo m
(SCE) . Qu trnh Sn hnh nh~ sau :
u tin Sm th & t ti f 1 = = 800 m (SCE) trong 1 ph, sau fi tng n =
900 m to mng. C sau mi thi gian to mng l 0s, 80s, 100s 3O0S, 6008, tin hnh
kh ptnfcdynamic (qut th v pha m) vi tc qut 5 mV/s cho n 1 . =ng
ong kh si <8=8 ghi li trn my. Trn - drag cong ny sfi xut hin mt n hai pie biu thi
ho qu trnh ph 8 mng Pe2Os v F34. in c n ~ c phn c 1 ph ln
th f 1 tr- c khi tip tc thu ng VI cc % tip h@Q. n0:
Tnh chiu dy s th0 pb= ong trnh (1), vi p = Ss24 g/m3 (khi l= ng ring ca
FeaOs) s Q?s 1, n = 2s r s 1 Th hin quan h S-T dng bn Sog.
V quan h s - Ig-r im gc nghing m a = ng thng ny;
Tho lun kt qu th nghim, so snh vi l thuyt
zs.a ph tSie m w@
Trong vng th ng, chn 5 gi tri in th <q>i ...f<5 sch nhau khong 200 mV/
Phn cc in cc ti in th 9o = - 800 mV trong 5 ph, sau chuyn n q>i. Th
ng trong 10 ph; mng c kh potentiodynamc n gl t o v tc qut * 50 mV/s.
ng cong kh c ghi ll . in I- ng Q cn thit cho qu trinh kh c o bng cutong
met hay bng inh ton trn hnh. Cn.
Bn g:
Tm quan h g hlu dy mng 8, in 1= ng Q v in th f. V th v so snh
kt qu o e vi l thuy.
Bs
ANH HUNG CA CHT HO T NG BMT
N QU TR NH IN cc R N
8.1. Mc ch, ngha
Khi kt ta in kim loi c rt nhiu yu t nh h- ng n cu trc ca n nh- : bn
cht v thnh phn dung dch, mt dng in ctot, nhit , i I- u dung dch ... Ngoi ra
con c mt yu t nh h- ng rt mnh n qu trnh kt ta v cht I- dng kt ta, l cht
ho t ng b mt.
Tnh cht in ho ni bt nht ca cc cht hot ng b mt c trong dung dch l
hp ph ln in cc lm tng phn cc catot khi kt ta kim loi, kt qu l ich th- c
tinh th gim v lp ph phn b ng u hn trn ton b b mt nn. Tuy nhin nh h-
ng tt nay ch c mt so cht hot ng b mt thch hp v dng vi mt nng nht
nh no d m thi. Trong nhng tr-ng hp ng- c li, cht hot ng b mt khng c tc
dng hoc co hi, thm chi' gy nh h- ng xu rt trm trng.
Cc dung dch kt ta din kim loi c phn cc catot nh s cho kt ta tinh th th,
i khi si thnh hnh nhnh cy. l cc dung dch sunfat km, cadimi, thic ... hay dung
dch ch flosilicat, ch tloborat... Nhng dung dch y lun phi dng cht hot rig b mt
thch hp khc phc cc yu im trn.
Th nghim ny chn dung dch km sunfat khao st anh h ng ca cht hot
ng b mt dextrin n cht!- ng Sp kt ta km v n - ng cong phn cc catot
ea n khi in kt ta km.
Tr- c khi lm th nghim ny cn tm hiu : o Phn cc caoi trong khi
in phn hoc trong in kt ta kim loi, e Ph- ng php o sc in ng v
cch tnh ra in th in cc.
Q Quan h gia phn cc catot v cht l= ng lp kt ta. o Cc yu
t nh h" ng n phn cc catot khi kt ta kim loi.
8.2. H@ ht,
- Catot bng thp l 20 X 50 mm 4 ci dng v thit n
= Bnh in phn 250 mi (cc thu tinh) " 4 ci ho th nghim.
= not km 4 b o dng i, v
- Dung dch in kt ta km 4 dng cong phn
loi cc I (tham
- Ngun in mt chiu, bin tr, ampe k 500 mA 1 b kho bi 1)
- Bnh o in ho 3 cc (250 ml) 1 b
- in cc eaSomen 1 ci
- My tnh c phn mm thch hp qut th,
8.3. Tin hnh th nghim
Th nghim gm hai phn :
- Xc inh nh h-og ca dextrin trong dung dch n hnh thc, cht 1= dog v cu
trc Sp km kt ta in.
- xc nh nh h ng ca dextrin n in th kt ta km v xy dng = dng
0009 phn cc p-i.
Phm mio Blm kt im km @Bj 4 mg Is mas:
Thnh phn dung Dung dch 1 Dung dch 2 Dung dieh 3 Dung dch 4
dch, g
Km sunfat 250 250 250 250
Phn nhm 30 30 30 30
Dextrin 0 II 5 15 30 I
Chuyn i Monitor
Keyboard'
Cc in cc w, c ty ra sch, t vo bnh, rt 150 ml dung dch s 1 vo bnh.
Phn cc caot cho w 3 pht Zn bm kn b mt in cc w. lu khin bng key oosr
h thng my qut c tc thch hp trong mt khong the thch hp, nhy vte ph!
mn hnh ca Monitor hin Sn & ng cong quan h f - va nht L u rsg ph
cha im i = 0. Ghi li - ng cong bng my in Printer hay bng a mm ti my tnh PC.
Cc thao tc trn my tin hnh nsh- ni bi 1.
Ly in cc w v c ra, ra sch, ty trong HCI1:1, rs sch, trng 0 s ct Thay
dung ch 1 bng ung ch 2 trang bnh ba cc. Lp cc in cc vo nh~ lc u tip tc
lm. vic vi dung dch 2 theo cc trnh t nh- trn mi c th cho n dung dch 3, dung dch
4. (Nh thu hi dung dch sau mi sn o v bnh ba cc phi ra sch, trng n-c ct r!
trng li bng dung dch sp o mi khi thay dung dch mi).
Vi 4 & ng cong thu c trn cng mt th ri so snh, nhn xt v r ra kt lun
v nh h ng ca dextrin n phn ctyte catot khi kt ta km v lin h v nh h= ng ca
n n Snh thc, cht L ng Sp km t thu & G phn 1.
Bi 9
T o MNG PHA OXIT BNG CCH OXY HO
KIM LO ITRNANOT.
9.1. Mc ch, ngha :
Nhiu kim loi t sinh ra mng oxit ngay trong khng kh hay trong dung dch c
tnh oxy ho lm th ng b mt kim loi, khin cho chng bn hn. Tuy nhin cc mng
ny th- ng rt mng, kh nng bo v khng cao hoc khng bn lu. Th ng ho b
mt kim loi bng ph- ng php oxy ho anot s cho mng pha oxit dy hn, c nhiu tnh
cht th mn yu cu mng mun.
1 oi
Mgum in mt chiu, bin tr 1 b
Nhit k 100 1 ci
Dung dch aSyzarrim i = g/s 500 m!
Dung dch ty AI2O3 1 lit
(gom H3PO4 45ml/l * CrOs 20g/l) .
Dung dch ty bng AI 1 lit
(gm H2SQ4 c 28% +H3PO4 50% + CrOs 4% + m-c 18% theo trng S-
ng. T trng 1,7)
ioio Tin tr nh th nghim
9.5.1. un b m ) Mi mu u ct i nh- ng ch- a t (xem hnh v) sau
khi oxy ho s ct ri thnh hai na em kho st ring.
Mu Al lau sch du m bng giy See tm axeton, rte n= c nng, ra n- c Sanh
ri ty trong trong ung d|ch ty bng 80 90c trong 2 4ph . Ra n- c snh. Mc vo
bnh in phn" Rt dung dfch H2SO4 v d va ngp ht mu S - Co
9.5.2. @ k Oxy ho AI vi Da s 2A/dm2 bng cc in 8 ng khc nhau
cc nhit khc nhau theo k hoch ghi bng 1.
Binh s 3 phi ngm trong n= c ngay t u t nhit ~5G r= c khi dng.
Bnh s 1 v 2 c th dung chung (hnh 3.17).
Theo di dng v iu chnh R kp thi lun -c I = const. Ghi nhit
th nghim, in th lc kt thc mi th nghim ...
Bng 1 ____________________________
Mu Nhit Dng in, Thi gian, Bnh in Ghi ch
s A ph s in I- ng thc
A.ph/dm2 cui
1 Phng 40 1
2 Phng 20 2
3 ~5c 20 3
Oxy ho xong, ngt in, ly mu ra ra n- c lnh (khng s tay vo mt mu), ct
ri mi mu thnh hai na :1,1*; 2,2*; 3, 3*.
Cc mu 1,2,3 sy kh o xp, dy.
Cc mu 1*, 2*, 3* khng sy, em nhum mu ngay ri kim tra do, gn
bm ca mng.
9.5.3. Nhum nhm
Cc mu 1, 2, 3* nhum mu vng trong dung dch sau :
Alyzarin 5 = 6 g/l
Bnh 3 Brl v 2
HMi 3.17: S thit b oxy ho nhm
Nhit 75 - 90c
Thi gin 10 pht
Vt ra, ra n-c lnh. Luc trong n-c ct 20ph 90 100c . sy kh,
nhn xt v th tnh cht:
Un mu quanh trc thp (> 8 mt vng ri quan st vt rn nt ti ch un. Ghi
li nhn xt.
Ly mi dao nhn rch ch thp trn b mt oxy ho v cy xem lp
oxlt c bong ra khng? Rch trn b mt ch- a oxy ho so snh cng ca chng.
.,4. Bo Mp
Cc mu 1, 2, 3 sau khi sy kh, cn ln 1 dc cc trng I- ng Ai, Az, As
Nhng vo cc du my v un n 100 110c trong 20 pht.
va r@s lau ht du tha, lau k li bng giy lc. Cn ln 2 c Bi, B2s Bs.
trong Ngm mu vo axeton ri lau k cho ht du trong l xp. Ho tan oxlt
H3PO4 (c) 45 ml
CrOs 20 g
N-cct thm n 1 lit
Nhit 90c
Khi t ngihg phn bg, i thm 2 pht na cho tan ht AI2O3 (A8 Echrsg b
tan). va ra8 rite n- c lnh, ys cn - de cc trng I- ng b dng hg Ci9 Ca, C3.
oMo 7 tm w @
Trng l= ng du hp ph trong mng B-A (g) my (cm3)
0J> g/cms
(-Vr
3S14 g/cm
100Vte/rvWfe)
V/(1-0,01X) '
r (1 - 0.01IX).
m-
Tng th tch s xp3 bng th tch du hp ph Vte s
trng s= ng ring ea du Y = Th tch nhom oxit (cms) VOK
ss
trng s= dng ring ca Old! nhm m = B xp th tch X ca
rong (%): X- lOOVfe/Vr, =
Vn l th tch mng.
TIMh th tch mng (cm3) vm =
Trng 3= dng ring ca mng C@/cms) m -
Bi 10
ANH HNG CA CH IN PHN
N SKT TA DIOXIT MANGAN Mn2
10.1. C SI thuyt
Dioxit mangan Mn02 - c s dng rng ri lm cht hot ng in cc d- ng
cho pin. Ngoi ra n cn - c dng cho mt n phng ngt, hp ph cc hi c nh- CO,
hi thu ngn. Ph- ng php in ho iu ch Mn0 2 - c p dng ch yu trong cng
nghip v co nhiu -u vit hn ph-ng php ho hc - c th tin hnh in phn trong
dung dch clorua, sunfat hoc nitrat mangan.
Kh in phn dung dch MnS4 trn anot xy ra s oxy ho Mn2+ n
4+
Mn :
Mn2+ + 2H20 - Mn02 + 4H+ + 2e
Trn catot hydro phng in
2H* + 2 - Ha
MnS04 ch to bng cch nung piroluzit 600 - 750c. Mn02 b kh thnh MnO, sau
ho tan n trong H2SO4 60c theo phn ng :
Mn02 + H2SO4 -> MnS4 + H2O
MnS04 to thnh - c lm sch khi cc kim loi nng.
Qu trnh in phn iu ch Mn02 chu nh h ng ca nhiu yu t nh- : axit,
nng , nhit , mt ng in v cc tp cht khc...Khi nng Mn2* trong dung
dch nh th hiu sut dng in nho, bi vy nng MnS 4 khng =c nh hn 50 =
60 g/s. Trong dung dch c pha thm mt -ig H2SO4 do tng dn in. Mu
in phn nhit th" ng v mt dng in ln, sn phm to thnh c dng bt. Kh
in phn nhit cao v mt ng in thp thi sn phm Mn bm thnh lp gn
chc trn b mt in cc.
Vt liu in cc (anot) cng nh h- ng n hiu sut dng in.
Trong qu trnh in phn, mt lp Mn2 to thnh trn b mt anot. iu dn n
gim hiu sut dng in-v qu th thot O2 trn Mn02 nh hn trn chi
Khi khng c mng, mt phn sn phm anot b kh trn eaot thnh MnSQ 4 Sm
gim hiu sut dng in. C th dng vi lm mng hay bc anot.
a s cc tp cht (AI, F@, Co, NI, Cu, p u c th lm gim hiu sut dng in,
nh- Fe v Cu trong dung dch s gim hiu sut dng in n 30%.. Kh c AS mt lp v
c to thnh trn anot dn dn b mt anot b hng.
10.2. Mciehth nghim
iu ch - dc mt != ng MnQ2 theo cc ch khc nhau v xc nh mt s ch
s c bn ea qu trnh in phn.
HO. Tlrs Mmh th nghim
MJotf. umb wm(
un nng H2SO4 n 40- 50c cho nh k mt 1= ng MnS04 (khong 3g), sau khi 1
ng tr= c ho tan ht mi cho tip tc 1= ng sau. Khuy lin tc, ho tan cho n kh t
nng yu cu, phn tch ti nng MnS04.
1 Jf o msg pbp psiB < ndn MMP
Ho cht cn ht:
Dung dfeh EDTA 0,01 y (0,05M)
Dung dch Zn2" 0,02M Dung dch m
NH4CI-NH 4OH Tinh th mui hydroxylamin, ch!
th ETOQ.
C&8 huyt:
Khi cho EDT vo dung dch in phn c lm 2+. Chng s kt hp VI nhau to
thnh phc teo ph= dog trnh phn hg :
Mn2' + IHaY2 ^ MnY2 2ST pHi s = 10 khi ch vl hft chi thf
ETOO vo dung dleh th dung dich c mu icanh lam.
Khi c lon Zn2-> trong dung dfoh, Zn2,> phn ng vl EDTA tya to thnh phc Zn- 2
tb@ ph ng trnh :
HaY-* = Zn y-2 2kf
Mu EDT phn hg ht, dung .dfeh si chuyn t mu Manh iara sang mu im.
a teo s ny te c th tin hnh Mc ph nng t Mo2* trong dung dch in phn theo
ec b= sau :
Cch tin hnh:
Ly khong 2 ml dung dich in phin nh mc n 100 ml (dng binh nh mc
100 ml) bn n= c c nhm pha Song dung |ch.
Dng pipe! ly 5 ml t dung d|ch pha Being trn <= a v binh tam gic 250 mS,
cho v vi hf tinh th hydroMylaroin . Sau cho v bnh tem gic 10 ~ 15 ml dung dch
EDTA 0,01 M . tsn hnh chun te thm 3 - 5 ml dung d|ch m v vi ht ch! thi
ETOO, sc u, dung dch e mu lanh Sam.
hun bng dung dfch Zn25- 0,02M. im t dng = mg, khi ta ch thm mt
2
git In * dung dch s chuyn t mu xanh lam sang mu tm.
Lm 3 ln v ly gi tr trung bnh ca th tch dung dch Zn2+ phn
ng.
Tnhtoan
INng Mn2"' (CMna) tnh theo cng thc:
Trong :
10.3.3. in phn:
Tin hnh in phn hai ch khc nhau :
Ch 1 Ch 2
MnS4 180 g/l 180 g/l
H2SO4 36 g/ 36 g/
Da 5 A/dm2 1 A/dm2
t phng 80 - 90c
in cc: ano l tm titan, t gia 2 tm catot bng ch hoc grafit S in
phn nh- hnh 3.18 sau :
Thi gian, h
Hnh 3.18.: 1 - Nng oxy hot ng theo l thuyt; 2 - Nng o hot ng
trong QO; 3 - Nng o hot ng trong QO3- ; 4 - Hiu sut ng in ca oxy kh. 5 -
Hiu sut dng in ea oxy hot tnh.
11.4. Yu cu t nh ton v bo co
Gii thiu qua (ngn gn) c s l thuyt;
S th nghim v m t cng vic;
Lp bng s liu thc nghim;
Tnh hiu sut dng in NaCIO v NaCI03, v - ng cong H% - T (Hiu sut - thi
gian).
M t thay i in th theo thi gian.
11.5. Phn t ch dung d ch
11.5.1' Phn t ch NaCIO bng ph ng php it:
Da trn kh nng ca NaCIO tch u t dung dch KI.
Ly mt I- ng dung dch phn tch, cho vo bnh tam gic, cho mt t dung dch
kl, axit ho bng CH3COOH 30% v chun -ng 2 tch ra bng tiosunfat natri:
NaCIO + 2K! + 2CH3COOH = NaCS + 2CH3COOK + 2 + H2O Hm I" ng
NaCIO trong dung dch - c tnh theo cng thc:
A = 100. a.T774,64/2C. 158 , g/s
Trong A-hm l= ng NaCIO trong dung dch, g/S;
C-- ng dung dch ly phn tch, cm3; a - ng NaSaOs dng
chun I2 , cm3;
T chun ca dung dch NaaSas, biu din bng g/cm3;
158 - trng I- ng phn t ca NasSsOs;
74,46 - "trng l ng phn t ca NaCIO.
11.5.2. K hNaCIOs
Da trn c s dorat trong mi tr- ng axit oxy ho st II thnh st III.
Dng ppet ht dung dch trong bnh in phn ri b vo bnh tam gic V cm3,
nh vi git H2 O2 30% vo phn hu ht NaCIO:
NaCIO + H2 Q2 = NaCI + H20 -s- 02 Sau un si dung dch phn
hu ht H2 O2 tha; lm ngui bnh; rt vo bnh ung dch sunfat st II ( axit ho) v li
un si ( oxy ho ht Pe2*) 6FeS4 + NaCIOs^ 3 H2 SO4 = WaCI +3Fe2(S04)3 + 3H20 +
+ K2SO4 + 2MnS4
Hm l= ng NaGI03 tnh theo cng thc:
: A = 1000(a - b).5 X 106,46 T / 6V58,03
Trong > - hm 8= ng NaGOa trong catolit, g/;
a - S cm3 dung dch KMn04 dng chun X cm3 dung dch FeS4
b = S em3 dung dch KMn04 dng chun cm3 dung dch n gk- 106s46 trng
8 ng phn t NaC03 ;
158,3 trng l" ng phn t KMnO .
Dung dch axit st II c pha teo gm :
F0SO4 30 g
H2SO4 (1,84) 300 cm3
H2O TOO
cm3
1 aa Hllu sut &Bi iifm ca HaCi hay ca NaClOs - c tnh theo
cng thc:
H = 100. gt/git % .
Trong gtt = l= ng NaCIO hay NaCIOs to thnh theo thc t:
9u = C.V
c = nng dung dch g/l ;
= th tch dung dch, lt;
9* - 8= ng.MaCSG hay WaCS3 tnh theo nh lut Faraday :
g 3.I.T = M..x / rsp
3 & mg 8 ng in ho ca MaCIO hay MaQQ$;
8 ~ c= dng dng los ;
X' = thi gian in phn, h ;
M = trong 8= ng phn MaCSO hay htoClOs ;
n a 2 s v MaOO v
- - vi MaCIOs
p = 20s8Ah (s Faraday).
Bi 12
IN PHN CHT o BT NG
12.1= L thuyt
in phn bng dng in mt chiu s nhn - c bt ng trn catot t dung dch
n- c.
Qu trnh xy ra:
in cc catot: Mene+ + ne - Me
2H+ + 2e -> Hz
in cc anot : Me - ne Mene+
Ket ta kim loi in cc catot, phn bit thnh 3 dng (trong c ng):
1. Dng kt ta kim loi rn, dy sit : bc lp kim loi em nghin thnh bt (tr- ng hp
ny Dc < Dgh)
2. Dng kt ta kim loi mm, cc ht kim loi lin kt yu vi nhau, d dng nghin thnh
bt, gi l dng sa thch" (tr- ng hp ny Dc Dgh).
3. Dng kt ta kim loi xp, b, phn tn cao. Bt kim loi nhn - c trc tip trn in
cc (- ng hp ny c > Dgh).
Chri iu kin in phn -c sn phm dng kt ta bt, phi l Dc > Dgh. iu
ny " c biu din trn th 3.20a : - ng cong phn cc catot, v th 3.20b: cht I-
ng kt ta kim loi ph thuc vo De (A/dm2) v CMB* .
13 Jo Tinh h dung d ch
Dung dch ho tan thu c ngoi Zn2+ ra cn cha nhiu ion tp cht, gy nh h-
ng xu n qu trnh in phn v cht I- ng sn phm km kim loi sau ny, v vy phi
tinh ch dung dch tr- c khi in phn :
Dng phoi km hoc bt km kh cc ion kim loi tp cht c in th
d~ng hn km, nh Zn + Cu2* - Zn2* + Cu
y l qu trnh kt xi men, ph ng php ny -c dng rng ri tnh ch
dng dch.
Dng ph- dng php thu phn : thay i pH dung dch n cc gi tr kt ta
ion kim loai tp cht d- i dng Me(OH)n , nh- ng ch- a kt ta ion Zn2*. V d lm
sch lon Fe2+ khi dung dch bng cch thm 2 + 5 mS H2O2
vo dung dch, un nng n 40 4- 50 c , khuy lim tc chuyn ht Fe2+ thnh F3*, sau
dng NaOH 10% chinh dung dch n pH 4 kt ta ht st d- i dng F@(OH)s (xem
hnh 3.21),
o lon Ch tp cht - c kt tu vi lon g* bng cch nh tng git dung dch long
g2S04 vo dung dch cho n kh khng cn xut hin kt ta trng.
G Lc Sy dung dch tinh ch.
o Phn tch nng Zn2* ( c c s pha thnh dung dch in phn)
o Pha long hay c c dung dch, tinh ch c dung dch in phn (ch
- c php cha 10 4-12 g/s ion Zn2*).
iu chinh n pH 4.
2 3 4 5 6 7 8 pH
Hnh 3.21. Gi tr pH xut hin kt ta Me(OH)n Dh thuc vo nng M'".
1 -l 2 - Fe3*: 3 - In.3*; 4 - GsPl-S - AP; -& 7 ~F 8-Zi^; 9-Cd2L
(theo B.. Gromova).
13JL [Pteia & m & B En/B i Lluulj
Ly 10 ml dung dch, cho vo cc 250 ml AxSt ho bng 1 4- 2mS HCS (n pH 1 4-
2); tip tc cho 1 4- 2 mS cht @xy ho H2Q2 , gia rshS dung dich chuyn F2* r>
F@s2 Cho hm 5 ml n~o ct v NfrioH (i:1) kt ta Ai(OH)s v F@(OH) 3. lc v ra kt
a Thu tt c dung ioh floe v n~ fa kt t vo -binh nh mc 250 ml roi thm 0 c ct
n vch.
xc inh hm l-ng km ly 1/10 dung ch a pha, thm 10 20 m n-e ct v 10
ml dung dch m (gm 54 g NH4C + 350 ml NH4 OH 25% pha thnh 1 lit) v 0,5 g cht ch th
mu (gm 0,1 g cht ETQO + 3 g WaCI, nghin k). Sau chun dung dch bng triton B
0,1 N ho n khi chuyn thnh mu xanh da tri.
Hm I- ng km tnh ;
Zn2* = 10O0V,T/V2 , g/i
V = s mi trilon i dng chun - '
2 = s mi dung dch cha km Sy d chun T *
0,003269 khi trtonB l 0,1 N
Trllon B nng 0,1 H - pha ch bng cch ho tan 8,6'13 g triors B vo 1 lit m=
c ct
13 A Tin hnh th nghim:
Th nghim thu sn phm km kim loi v chn ch in phn ti
-u .
Tin hnh in phn 2 ln : Dung Ln 1 Ln 2
dch in phn pH dung dch Nhit 200 ml 200 ml 4
in phn Thi gian in phn 4 nhit phng 30
Dc nhit phng 30 pht 1 A/dm2
Anot bng Pb phut 0,5
Catot bng AI A/dm2
Tr-c khi in phn kim loi sch. 30 X 50 X 1 mm
30 X 50 X 1 mm
in cc phi lm v sinh, ty ra, bo m
Sau mi th nghim phi phn tch nng ion Zn 2+ trong dung dch. Cc kt qu
th nghim ghi vo bng 2.
S th nghim :
Chth. ch:
Gi - trng 1- ng in cc T- c in phn G - trng 1- ng in cc sau in phn G - trng 1-
ng sn phm km in phn.
catot
/)
Bi 15___
M/4 KN
1S.1L Mc fch, |'ngha
M kn thttng ibc dng to ra lp bo v -trang sc trn cc vt bng st
thp. Do in th tiu chun ca Ni (-0,25 V) dw'ong hn ca Fe (- 0,44 V) nn Ni l lp m
catot i vi st thp. Vi vy mun bo v tt lp m Ni phi kn. Mun th lp Ni phi
dy, v phi tfc m trong iu kin m bt kh hydro thot ra d dng, khng bm lu trn
b mt khi ang m trnh to thnh l thng trong lp m. trang sc tt ngy nay
trtfang m Ni bng trc tip ngay trong b m. Nhtig cc ph gia bng lm tng nht
cho dung dch nn bt kh hydro kh thot ra, d gy thng cho lp m. khc phc phn
no nhMc im ny cn phi m nhit cao v phi khuy dung dch, ng thi phi
m nhiu lp Ni chng lri nhau.
Mc ch ca th nghim ny l so snh xp ( s l thng/ cm2) ca cc lp m Ni
m, Ni bng v lp m Ni kp (Ni m + Ni bng) c cng chiu dy. ng thi kho st
dung dch m Ni bng bng bnh Hull.
15.2. Ho cht , thit b|vt t cn dng :
- B ngun mt chiu + Bin tr + mpemt (c thang o n 0,1 A)
- Bnh m : cc 250 ml 2 ci + anot N 2 b.
- Bnh Hull loi 267 ml 1 ci
- Duna dch ma Ni m SOOml Ni bna 500ml
NS4 250 g/s 250 g/s
NC 15 gl 15g/
H3 BO3 (Ts/i 30 g/l
BK-1 -u U 0,8 -1 m/!
Sacarin - 0,7 = 1,5 g/i
pH 4=5 4=5
1
De 3 Nm 3 Nm2
Nhit phng 50 - 60 c
- Giy nhp mn 1 t
- Cat :-thp l, kch htbc : 2cm X Tem 3 ci.
= Giy lc 1 td (nh)
Dung dch ty du ho hc 110 EC 50g/l 250ml
- Dung dch ty nh H2 S4 60 g/l 250 ml
- Dung dich o xp Ni 100 ml
gm: S<3 Fe(GN)6 1g/ + NaCI 20 g/l.
r. .
1S.3 Tin tinh thl nghim
15.3.1. M Ni m:
- nh sch catot bng giy nhm mn
- Ra.
- Ty du ho hoc 60 - 70 c, trong 5 ph -(cho c 3 catot).
- Ra (khng s tay vo mt catot)
- Ty nh trong H2SO4 60g/I 10 -20 s .
- Ra.
- M Ni m theo S nh/ hnh 1.1 . iu chinh sao cho catot chm 5cm trong dung
dch v dng in tng vo h l 1 = 0,6 A (t#ng ng vi Do = 3 A/dm2, din tch m
s - 2 (2cm X 5em) - 20 cm2).
M trong 20ph nhit phng.
- Ra, sy ch o xp.
15.5.2. MMi&mg,.
Thay binh m Ni m bng bnh m NI bng ( $e un nng tf/c n 50 - 60 trong
binh cch thu). Catet te chun b, ty ra v m nh-tf mc
15.3.1. M Ni bng cng dung s A, s 20 cm2, thi gian m 20 ph nhit 50 = 60
cT
M xong, ra, sy, ch o xp.
15J.5. ' M M M p mcJf * N^s
- Lp li th nghim m Ni m d catot 3, nhifng ch! ma 10ph. Wfa xong khng cn ra,
chuyn thng sang bnh m Ni bng cng nhanh cng tt.
M tip Ni bng th ch nh mc 15.3.2 nSiSfing chtrong 10ph.
- Mf xng, ra, sy, ch t xp.
' 153*4 Km m mmg k M mg Svwmg Md8 MmS
- Lp anot NI 6cm X i cm vo binh Hui;
- Catot bng thp l hay bng ng S 5 kch thtc 0cm X 8cm ei). Chun
W b mt eaM lm nhg| i ni. 15.3.1. Lp vo bnh Hull; '
- Rt 250 mS dung ich m M bng vo binh Hui. iu chinh mgum din sao cho dng
in tng qua bnh S l 1 A . Mf 20 pht nhit th^dng.
- Tnh mt dng in cc b v ti cc y s ta 2, 3, ...10 cm trn catot the cng thte
sau v ghi vo bng 1 :
Dy = 10 J.(5,1 - 5,24 logy), A/dm2
y khorsg cch dc theo chiu di catot tinh t u gn anot nht, cm; s - dng
in tng & vo binh Hull (c th eh 267 ml) A;
- Nhn xt chatWdng Sp m ti cc y - 1, 2, 3, ... 1Gcm (tc ta cc Dy khc nhau) theo
cc quy iG : mng M, nhn H, bng B, gai G, chy c, bt ri R. Ghi vo bng 1 ;
- Kt Sun vng mt dng aeato D cho Sp m tt nht
Bng 1. rnmtmmgi&Mm
y 9 cm By m/em2 rah gi cht I- <ng Nhn xt, kt mm
1
2
3 -
10
\
15.4. o xp.
Ba mu m thu Vc trn phi gi sch, khng s tay vo b mt m.
- Ct giy lc theo kch thtoc 1
cm X 2 cm 6-8 mnh
- Nhng mnh giy lc vo dung dch o xp ri p st vo b mt m. Mi
catot p 2 mnh 2 ni khc nhau, dng a thu tinh nh thm 1 git dung dch o
xp na ln mi mnh giy lc y. Tnh gi.
Sau 10 ph bc giy lc ra, ra dti vi ntfc, sy kh giy v m s chm
xanh trn giy. Mi chm xanh l 1 l thng ca lp m. Ghi kt qu vo bng 2. Mu
xanh l do dung dch th chui qua l thng ca lp m vo gp nn st, xy ra phn
ng, cho sn phm c mu xanh :
2K3Fe(CN)6 + 2NaCI + Fe = 2 K3 NaFe(CN)6 + FeCI2
nn xanh
15.5. IVnhchi&j dy lp met
Chiu dy trung bnh s ca
lp 5 = Dc.3.H.T.y -1 , m dKc tnh theo cng
thc 2
Do - mt dng in, A/dm 3 - - ng u/ng in ho ca sau :
Ni = 1,095 g/Ah H - hiu sut dng in ca m Ni = 93 %
X - thi gian m , h $tr .
- khi l ng ring ca Ni = 8,9 g/cm3
im
Bng 2. Kt qu th nghim
Dc X m dy xp, /cm2
Lp m Ghi chi
/dm 2
ph um ln 1 ln 2 T.bnh
Ni m ~~
Ni bng
r~
#
.
Ni kp
1SJL . Cu hi
- u im, nWxic im ca 3 loi lp m NI th nghim. Gi thch.
- Ti sao cho php m Ni md xong khng ra, chuyn thng sang m Ni bng, v ng
tc ny phi lm tht nhanh ?
- Tc dng tot v xu ca cht bng trong m NI.
- -c lp m .Ni tt v bo v, p v trang sc theo anh ch cng
ngh m Ni phi nn nh= th no ?
- Lp m NI bng lm mc 15.3.2 c cht S-ng ng vi vng no trn catot rri
trong bnh Hull ? b g ch- a tht khp nhau khng, ti sao ?
B i
ANHHtMG CA NHIT V Mr DNG IN
N HIU SUTEHDNGIN TRONG M CROM
ISkL Y ngha BHC ch
M rom -e hg dng r rng ri. Dung dch ma rom gm Cf0 3 v H2SO4 . Kh
ning phn btf v hiu sut dng in ca dung ch m rom thuc loi thp nht. Cht 1" dng
lp m cram v biu sut dng in m rom ph thuc rt ntlu vo hai yu t : mt dng
in v nhit . Thay s 2 yu t ny 0 th thu c lp m rom bng (khng n mt
ph gia bng no) hay rom ftga trng hoc rom xm ms xu ...v hiu sut dng in c
th t ti a (12 -15%) hay rt'thp ...
Th nghim ny nhm xc tph oh h= ng ca nhit v mt dng in n hiu
sut ng in atot v ht != ng lp m, qua gii thfch ho c inh kh nng phn b
thp a dung dteh ny.
tlioc fr3 crom hfi9 vll orv <p>j U Sh)
ragjfeifm m Dung CrOs 250 g/s ich m roms 1st:
Dung dich dSn l H2SO4 2s 0/1 ng k ng , 0,5 lit:
Kiu sut dng n ; it: a dung dfch niy bng 100% nn
mt m dng mkh usa.5HaO 125 g/i h oH din 8= ng i thng
qua mch. [H2S04 25g/
Xem mc 1.4 ni v R- u etylic 50 ml/l in i= dog k v ch x fnh
Do* 1 - 2 mm hiu sut ng n. S
Nhit phng thit b m crom, xem hnh
- I + Bin tr Ampemet
+-=2.
Ngun
Ko
+ (Cu) + (Pb)
-8 mcrom
Hnh 3.24. B
in 1- ng k un cch thn
3.24 :
Chun b 5 catot bng thp l hay ng l c hnh dng v kch th- c nh- hnh v. Kch
th- c phn nhng vo dung dch m cn tnh ton sao cho din tch s (c 2 mt
catot) l :
Mau 1,2 , 3 c = 0,2 dm2
3 cm
0.5 cm
Mu 4 c S = 0,1 dm2
Mu 5 c s = 0,05 dm2
Chun b 2 catot cho in I- ng k ng, din tch c 2 mt l 1,2 dm2.
Catot 1 dng cho cc mu m 1, 3, 5.
Catot 2 dng cho cc mu m 2 v 4.
(nh s cc loi catot trnh nhm ln).
16.3. Tin hnh th nghim:
Lm sch b mt cc catot ca b m crom v in l-ng k nh- ni bi m Ni hy
mc 1.2. Sau thm kh, sy 10 ph 110c, ngui v cn trn cn phn tch, ghi trng
I- ng ban u ca cc catot vo bng.
Sau khi kim tra mch in, mc catot 1 vo b crom v catot 1 cain
!= ng k vo in " ng k! ng mch. iu chnh bin tr - c dngin
ch trn ampemet ng vi catotl l 10 A/dm2 (cn tnh ong dng in v xem thang chia
ca ampemet tr-c thao tc lng tng lc ng in). K hoch th nghim trnh bay
trong bng.
Mi mu m 20 ph.
Cc mu 1,2, 3 kho st nh h ng ca t n H%
Cc mu 3,4,5 kho st nh h- ng ca Do n H%
Sau mi th nghim , ngt kho in, ly cc catot ca b m v ca in g k ra, ra sch,
trng n-c ct, thm v sy kh. Cn c hai loi catot v
tg, % 3, B 2. __
S 2 0,2 45 10
LK2 1,2 phng
S 3 0,2 60 10
LKl ' 1,2 phng
S4 0,1 60 25
LK 2 1,2 phng
S 5 0,05 60 5C
LK- phi
1
Th nghim ny cn nhiu thdi gian, v vy phi chun b k t tr- c, tnh ton
v b frf thi gian thao tc tht hp l. V nn un dung dch cho mu 2 ngay trong
kh ang m mu 1; un dung dch cho mu 3 ngay trong khi m mu 2 ...M crom
dng dng in ln nn cc tip im phi ni cn thn, cht v din tip xc ln. Khi
m c anot ln catot u c kh thot ra nhiu v lin tc, mang theo dung dch, gy
nhim khng kh, nn phi lm th nghim trong t ht kh mnh.
Da vo kt qu th nghim tnh ton hiu sut dng in H% nh mc 1.4. Trong trng!~
ng - g L n ca Cr bng nguyin !- dng (52) chia cho ho(+6).
Xy dng thnh 2 th|:
Hiu sut dng in - nhit Hiu sut dng
lo mt dng in o L gsi cc kt qu thu - de x@m c
ng quy Su khng.
Nhn xt cht l- ng cc lp m thu - c v gii thch.
38A tthi
(Chun b tr- c khi th nghim)
1- Tnnh by khi nim v15 hiu Mt dng in oatof v cch xc arm n.
2- Th0 l thuyt thl hiu sut dng din thot crom ph thuc nh= th [no v De, nh h=
ng ca tiu ny n ning phin b ea dung d|ch m crom.
3= Hiu sutft dng sn thot aom phy thuc vo nhit rah= th no, l do ?
4- Su kin tt nht m crom bng Si g ?
Bi 17
O sur IN NG, IN TR TRONG,
DNG LNG CA PIN
17.1. o sut in ng ca pin Vn in 17.1,1' Sut
ln ng E ca ngun in ho hc
E (p+ (- (1)
Trong <p+ - in th cn bng cc d- ng <p- -
in th cn bng cc m Sut n ng c th
xc nh bng:
Hiu s in th ca cc in cc cn bng theo (1);
Tnh t cc thng s nhit ng : E = -AG/ nF;
o bng thc nghim : Sut in ng ca pin l hiu s in th hai u cc ca pin
kh mch ngoi h: I = 0.
Lr
Milivon met
P
,2-
K
\ V,
o
cu IZ
A---------- [R :
Hnh 3.25. S o in tr trong ca pin.
p - pm cm o iE trong f; K - ko; V - von mt;
- mspg mt; R - bim te.
olnthVigviecgitir i S3 OJA; Qs2k; ,A; 0S4A. t l bng ec
fay tl w M 00 th rn bin tr R.
Pk I r
Mi oi A /ln'x
r------
0,2 '
0-3 A
... . 0.4 A
terns bMa:
Ci
GMdk: Dng pin i phng ht yrsg l= ng & mc 17.3. o r capineu. 0 nhanh hng nh h= ng n yng 8=
<pg pin. .
p - pin cn o dung 1- ng; V - von met; A - ampe mete; - in 1-
ng k ng; R - in tr 4Q.
Phng in cho en khi in th cn 0,75 V th nghg (thi gian phng khong 400
pht). ].
T
17.3.3. Xc inh dung # ng ca pin
ung -ng Q ca pin c th xc nh bng 3 ph= ng php:
a) Q = ItbX T , Ah ' \
Itb l dng in trung bnh xc nh trn th mL \
% l thi gian pin phng in n in th cui V ^ 0,75 V
b) Q = v l / R , Ah
Vth l in th trung bnh xc nh trn th V" X
c) Xc nh theo in " dng k ng : Theo nh lut Faraday l- ng in i qua
bnhin phn t thuii vi l= ng vt cht to thnh trn cc in cc, y l
- ng ng bm trn catot.
Q K . m - 0,84 m , Ah Vi
K= 26,8.n/A = 26,8X2/,63,54 - 0,84
Trong m l i= dng ng thot ra catot ,g;
A S khi I- ng nguyn t ng bng 63,54; n l
ho tri ca ng n = 2.
<Sh : Nhn xt v gii thch kt qu xc nh Q theo ba ph drag php;
Dng pin phng ht in o in tr trong ca pin cG.
Cch s dng, vn hnh in i- ng k ng lm nh- mc 1.4.
/v
IU Jl- K-- 1
L L A 4___
1 -1e,u A
(I, 93
. 1 -j>
. ----------------------^--------
r TK> [
V - IW
1 * ~ ,m 1 4 )
V )
Qj ::: 1 l y cf
f?=s;G,
u ,//
Bl f a
XC NH DUNG LNG
CA AC QUY CH
HSJo CisB tay
Ae quy chi hot ng da trn h thng n ho : e
PblHaSOjPbQa $'
Phn ng phrsg np tng :
{*-> Pb "5 PbiV 2H2SO4 2PPS04 * H2O
Dung s= ng Q ca ac quy ch ph thuc vo hng lot yu t: cu to, u kin phng
n, thi gian bo quanh.. Trong th nghim ny xc-nh s ph thuc dung b ng ca ac
quy vo dng m phng.
S dng quy 3 ngn 6VS mi (ngn phng n c Sp vi nhau .
Ao iih) raiMm
so
L 1
A
V cc - ng cong V - X v I - T ca mi ngn.
Xc nh trn th cc gi tr Vtb v Itb ca mi ngn.
18.3. Xc nh dung lng ca c quy theo hai phng php
a) Q = Itb. T
trong Itb l dng in trung bnh xc nh trn th I -1
T l thi gian phng in n in th 1,8V ca mi ngn
b) Q = Vtb. X / R
trong Vtb l in th trung bnh xc nh trn th V - X R l in
tr t I cho mi ngn T l thi gian phng in
n in th 1,8 V.
Ghi ch : - Nhn xt v s ph thuc dung I- ng ca ac quy vo dng in
phng
- Dng in s c nh h ng g n in th ca ac quy khng ?
- Nhn xt v kt qu xc nh dung - ng theo hai ph- ng php.
Chng 4
Cc ph lc
Ph lc 1_____________ Ty du m cho kim loi
ng, ng thau Thp
Thnh phn (g/1) v ch Hohc inho Nhm Ho hc Hohc in ho
NaH 10-20 20 - 30 10-20
Na2C3 20-30 25-30 30 10-20 25-30
Na2P04.12H20 25-30 25-30 30 30-50
Thu tnh lng 5-10 3-5 30 5- 10 5-10
Nhit , c 70-90 50-60 60-70 70-90 60-70
Thi gian, pht 5-10 1-2 5-10 10-30 catot 2 -3
anot 1-2
Mt dng in, A/dm2 3-10 5-10
m 9
Ph lc 4 Ty g in ho cho st thp
H2SO 50 = 60 g/1
4
HO 25 - 30 g/1
NaCl 15 - 20 g/1
Mt dng in anol 8 -10
Nhit A/dm2
Thi gian 60 - 70pht.
10 -15 c
Pta IC Ty nh da Mma tat
Thnh phn (g/I) v ch Thp ...._ ng Km j9Mm
H2SO4 30-40 30-50
8 1 Ui
u%
KCN
Nhit c phng phng png phng
Thi giam, s 30 60 5-10 3-10 3"
Hydro Ha O H* + e sf
Hi + 2QH- o 2H20 + 2e -0,828
22O 0 H2O2 + 2H* + 2e + 1,77
30H- 0 HOa" + H20 + 2e 4 0988
Natri Na 0 Na* 4- e
. -2,71
Niken Ni 0 NP + 2e -0,23
Ni + 20H- 0 Ni(OH)a 4- 2e -0 72
Ni(OH)a + 20H- 0 MOa + 2H20 + 2e 4 3,49
Titan Ti o Ti2+ + 2e
-1,75
Km Zn o Zi2* + 2e -0,763
Hng
Kimsloi
vt lZnea
Dng mt s nguyn
Dang=t [Zn(CN)4] 1- <Dig m ho
+ 4CN- -2 Ctos:
' 4 2e -1,26
Oxyho Trng
iSguyn t KTu Kh 1- ng-[Zn(NH
T trng - ng 1- ng -ngl-ng
Zn + 4NH3 o 3)4 4 2e -1,04
+
Nguyn t]: g/Ag/cm3 2 Ats/g hohoc fllfpLg in ho, Aog/mg
g/Ah
Nhm Zn + 40H- = [Zn(OH)
0,33 ] + 2e -1,216
AP AI 2,982 0,093 0,335 10,73
1 4 h
Nhm TF '2 26,98o 2,69 8,99
St Fe *34+ 20H-55,85>
Zn Zn(OH)
5 7,86 2 + 2e 27,925 1,042
-1,246
St
Vng Fe -
Au* Fe
197 0,694
19,3 1,441 187,21 0,193 5,184
7,358
Ph lc 8 2+
Fe
u324 * Fe
197 1,042
19,3 0,960 65,73 0,289 3,456
2,453
Caimi
Caimi G2 Cd
112,40 2,097
8,64 0,477 56,2 0,592 1,717
2,097
Coban
ca
CO
Co *2
* Cd
58,94 2397
8,8 0,418 29,47 0,664 1,507
1,100
og Cd(OH>2
Cu 2
*3 Cd
63,54 2,731
8,93 0,366 31,77 0,758 1,320
1,186
Oban Co
Cu*24 * Co
-63,54 0,733
8,93 1,364 63,54 0,208 4,808
2,372
Asen Co3 '
As *24 Co
74,91 1,099
5,78 0,910 24,97 0,305 3,275
0,932
Mage
Kn Mg2
Ni * 2+ mg
58,71 0,454
8,8 2,204 29,345 0,126 7,936
1,095
Mangan
Thic Mn
Sn 2
* Mn
118,70 1,023
7,28 0,975 59,35 0,284 3,520
2,214
MnO-T
4
Sn * Mi
118,70 0,632
7,28 1,592 29,675 0,175 5,716
1,107
4 E04- 2-
Bch kim Pt * M Mnt
195,09 4,434
21,4 0,226 48,80 1,230 0,812
1,821
ng
Ri Cu3*2+
Rh Cu
102,91 1,186
12,3 0,843 34,30 0,329 3,036
1,280
Ck Cu*
Pb 2
* Cu
207,21 2372
11,34 0,422 103,60 0,658 3,8651JI
Bc QiQ
Ag* Cu
107,88 3,690
10,50 0,271 107,88 1,050 0,975
4,025
Kn
Antmoin Sb Ni5*34- Ni
121,76 0,730
6,69 1,370 24,352 0,203 4,933
0,909
Ni 62+ Ni 1,095 0,913 0,304 3,288
Crom Cr * 52,01 7,1 8,67 0,3235
Ni(OH) M 1J29 0,578 0,481 2,082
N(OH)3 Mi2* 4,095 0,244 1,135 0,882
Thic SQ*- Sn 1,107 0,903 0,307 3,252
2+
Sn Sn 2,214 0,452 0,615 1,626
Thu ngn Hg2+ Hf 3,742 0,267 1,039 0,962
Hr Hg 7,484 0,134 2,079 0,481
Om Pt?* fb 3,870 0,270 1,074 0,930
PbO Pb 4,126 0,241 1,152 0,867
PbS04 a 5,661 0,177 1,572 0,637
PbO Pb2* 4,461 0,224 1,239 0,806
Bc Ag* Ag 4,025 0,249 1,118 0,894
AgaQ. Ag 4,345 0,231 1,207 0,828
,.., Ag 2,313 0,432 0,642 1,556
:
Crom *cF Q 0,323 3,094 0,090 11,111
C3* Cr 0,646 1,548 0,180 5,555
Km Zks* Za 1,220 0,819 0,339 2,950
ZnO Za 1,519 0,658 0,422 2,368
Zn(OH)2 Zfi 1,854 0,539 0,515 1,942
Ph lfc 1 T rmg $a MI s Un
ng thanh nhm Bt7 7,8 ng thanh thic BrTlQ 8,7
ng than L68 8,60 Tompac L90 8,78
Hp kim Pb - 6%Sb 10,89 Thp !Crl8M9Ti 7,8
Thp xy dng St-3 7,84 Thp khng gi CM3 7,75
ti liu tham kho
B