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Th nghim Cng ngh in ha ti i hc Bch khoa H Ni

Chng 1: Chun b cho cc th nghim in phn


1.1 Thit b v dng c dng cho in phn
1.2 Chun b b mt in cc th nghim
1.3 Chun b dung dch in phn
1.4 Hiu sut dng in. in lng k
Chng 2: Chun b cho cc o c in ha
2.1 S khi mch o in ha tng qut
2.2 Bnh o in ha
2.3 in cc
2.4 Lm sch nc
2.5 Ty ra bnh o v dng c th nghim
2.6 Pha ch dung dch. Np vo bnh o
2.7 Ti kt tinh mui. Lm sch axit
2.8 iu ch v lm sch kh
2.9 Vt liu ch to in cc
Chng 3: Cc th nghim in ha
Bi 1 Von Ampe vng trn in cc tnh
Bi 2 Phn cc nng
Bi 3 Voltametry trn in cc a quay
Bi 4 Phng php tng tr in ha
Bi 5 Xc nh tc n mn kim loi bng phng php o ng cong
phn cc
Bi 6 Xc nh tc n mn kim loi bng phng php trng lng v
phng php th tch
Bi 7 S th ng ca kim loi
Bi 8 nh hng ca cht hot ng b mt n qu trnh in cc rn
Bi 9 To mng pha oxit bng cch oxi ha kim loi trn anot
Bi 10 nh hng ca ch in phn n s kt ta ioxit
mangan
Bi 11 S ph thuc ca hiu sut dng in hipoclorit v clorat
vo thi gian in phn
Bi 12 in phn ch to bt ng
Bi 13 in phn iu ch km kim loi t qung
Bi 14 o kh nng phn b ca dung dch m in
Bi 15 M kn
Bi 16 nh hng ca nhit v mt dng in n hiu sut
dng in trong m crom
Bi 17 o sut in ng, in tr trong v dung lng ca pin
Bi 18 Xc nh dung lng ca c quy ch
Chng 4: Cc ph lc

Chng 1 + 2: sinh vin t c.


Mn in ha l thuyt: lm bi 1 (tun 7), bi 2 (tun 11) v bi
4 (tun 14).
Mn n mn kim loi: lm bi 5 (tun 4) v bi 6 (tun 5).
Mn M: lm bi 14 (tun 4) v bi 15 (tun 5).
TH NGHIM CNG NGH IN HA (i hc Nng)
Gm mt s bi c trng trong s cc bi th nghim sau:
1. Thao tc thit lp mt h o in ho c bit: bnh o 3 in cc.
2. Th nghim phng php in phn sn xut NaOH-Cl.
3. Th nghim tinh luyn, tch cc kim loi ra khi qung, tch cc hp cht bng phng php in
phn trong dung dch nc hoc nng chy.
4. Cc k thut tinh ch kim loi qu cng c thc hin vi quy m nh.
5. Pha ch, iu chnh mt b m in ho nh m Cr, Ni, Cu... Cung cp cc thao tc cn thit ph
cc lp kim loi (Ni, Cr) ln nn phi kim loi cng nh cc phng php kim tra v khng ch
lp ph.
6. Th nghim ph lp men trc tip ln nn kim loi vi mc ch trang tr v bo v n mn vi cc
nn kim loi.
Ch-ng 1
' ,/
'CHUN BXrtO CC THINGHIM IN PHN
U;V L 1 J _tl -L* AC- -Lfi- ffy$t feci /st Mk
1.1 Thit btva diincj c 011119 cho oin phan X A Jtr> a, D / A

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

Hnh 1.1 S thit b in phn


B - bin th; c - chnh l^u; A - ampemet; Rb - bin tr; BP - bnh in phn; K- cnh khuy; N- nhit k; - un
nng.

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 -

th xong mi tng dn ln n dng (hay th) mt chiu t gi tr yu cu


bt u in phn. Bin th ch chinh th dng v th mt chiu cho bnh in phn, mun chinh
tinh phi dng bin tr R.
Bin th c th t ngoi hay trong b my chnh tf$j.
Chnh Him c c nhim v bin dng xoay chiu thnh dng mt chiu cung' cp cho bnh
in phn. Trn my chnh thtng c nhiu cp in th ra phi hp vi bin th B v. bin tr R
iu chnh dng in mt chiu cho n khi t gi tr. y cu. 'i
Chinh tfu l mt t hp cc diot bng selen hay german ...lm vic vi mt in th v nhit
nht nh. V vy khng Bc da in xoay chiu (t bin the) c in the vt qu mc quy"
nh vo chnh tu (c ghi r trn v my chinh l\i) "v nhit trong my chinh teu khng Ve
vbt qu-75. Khi nng qu phi gim ti hoc ngng my v iu Chnh li th nghim.
Aquy: C th thay cho t hp bin th + chnh bng mt ac quy chi hay ac quy kim
np y in. Phn ln cc th nghim G th dng loi ac quy 6V. Ring m crorm, ty bng kim
loi, oxy ho nhm ... mi phi dng Soi 12V hoc hn. iu chinh dng in lc ny ch do mt
mnh bin tr R m
nhim. V vy phi chn bin tr c tr s v in tr v dng in ph hp, sao cho qu trnh in phn xy
ra bnh th- dng .
Btr R c nhim v tinh chinh dng mt chiu trong mch cho n khi t gi tr mong mun.
Mi bin tr c ghi gi tr in tr ca bn thn n v gi tri ti a dng in cho php i qua n. Nu dng
in trong mch vtt qu g tr ti a cho php ny bin tr s chy, hng.
C th mc ni tip bin tr vi bnh in phn trong mch nhi^hnh 1.1. Khi phi chn cc bin
tr c tri s in tr m R = E / I ; E i in th ra ca chlmh ftfu V (xem von mt trn chnh lK?u); I l dng
in trong mch (xem anmpemet A). N ch! c cc bin tr m tr s in tr ca n b hn g tri R tnh
ton th phi mc ni tip nhiu bn tr t t^c gi tr R tnh ton.
C th mc bin tr song song vi bnh in phn nhrf hnh 1.2 cho trng hp bin tr c tr s
in tr Rb ln v bnh in phn chl cn dng in I b.
4-0 r=

. oA
r
_0 ~\J~ :.:; j

Hnh 1.2 Bin tr mc song song vi bnh in phn

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 .4 Mu v gi , mc treo nghin cu n mn.

Dng c tip in Cc th nghim in phn thung ch tin hnh in

th rt b t 2 n 10V v dng in I t 0,5 n 5A. Vi th in tr ca mch cn phi rt nh, thng ch


c 10 -20 l Cho nn cn c bit ch n cc tip im, cc ch ni dy dn in phi m bo tip in
tht tt, tht chc chn dng in ^c thng mch. Mun vy thng phi dng cc dng c chuyn
dng ni, tip in dfltoc nhanh chng, tin li v m bo thng mch d dng. Hnh 1.5 gii thiu
mt s kiu dng c nh^vy.
9m f
1.2 Chun b b mt in cc dptthf nghim
Cc qu trnh in phn, nht l m in, c in ...cn phi lm sch b mt in cc phn
ng in ho xy ra d dng, thun li hoc sn phm phn ng gn bm tt ln b mt in cc.
Mun vy phi ty sch ht lp oxit trn b mt lm l r cu trc tinh th ca kim loi in cc bng
cch ty trong axit hoc kim (tu tng kim loi). Nhtf'hg b mt kim loi thttbng dnh bm du m, m hi
tay ...can tr dung dch ty tip xc vi b mt kim loi cn gia cng, lnr sch. V vy cng vic u tin
l phi ty ht du m trtc .
y du m c th tin hnh bng phng php ho hc hay in ho. Ty du m ho hc l gia
cng kim loi mt thi gian trong dung dch kim nng (i vi cc kim loi khng tan trong kim) hay
trong dung mi hu c (i vi cc kim loi tan trong kim nh- Zn, l..)
Trong dung dch kim nng, du m ng thc vt s bin thnh x phng tan ra, cn du m
khong vt (du m bi my, vazelin, parafin ..) s bin thnh nh tng bong ra.
Ty du m in ho th vt ty mc trn catot, dung dch l kim long hay mui kim loi kim.
Anot bng thp hay kn. Mt dng in 3 - 5A/dm2, nhit 60 - 90 c. Khi ty trn catot c HT phng
in thnh H2 , trn anot c QH -
phng in thnh 02. Dung dch -st catot giu dn OH ", tc dng vi du m ng thc vt thnh
x phng. Bt kh H2 thot ra; lm tch c hc khi b mt ty cc du m khong vt khng x
phng ho c thnh cc git nh. Thnh phn dung dch ty du m cho cc kim loi khc nhau
v ch ty = c trnh by trong ph c 1.
Sau kh ty du m, ra mu trong r^e m 60 c ho tan x phng ri mi ra nc l.
Ty ^u m cftfoc xem l t yu cu nu sau khi ra nc thm t u ton b bi lt kim o.
)
ru? g tin hnh trong dung dch axit, mui hay kim tu bn cht tng kim loi. C Jh ty g
bng phtong php ho hc hay in ho.
Ttf gi ho hc cho kim loi en trong dung dch H2S>4 hay HCI hoc hn hp ca chng.
i khi cn ty trng HF hay HN3.
ty ng, hp kim ng v mt s kim loi khc dng HN3 c hay long hoc hn hp
HNO3 vi cc axit khc.
V d khi ty trong H2S04 th oxit st Fe203 trn mt kim loi s - c ho an theo phn ng Fe203 --
3H2SQ4 - Fe2(8Q4)3 --3H20
ng thi st kim loi cng b ho tan mt phn theo phn ng :
Hydro thot ra trong khi ty g bng H2SO4 hay HCI s b kim loi ty hp
ph mt phn lm cho ksm loi tr nn dn, d v, gy. khc phc hin ting kim loi b dn hydro ngti
ta cho vo dung dch ty cc cht c ch nhbf: antraxen sunfonat, urotropin hay cc ch phm c cc
hng hiu khc nhau. Cht c ch c tc dng lm chm tc ho tan kim oi nn gim $c ^ng
thot hydro.
Thnh phn dung dch ty g ho hc v ch ty cc kim loi en v mu trnh by trong
ph lc 2 v ph lc 3.
T$ g in h@ C th mc kim li trn Ctot hoc anot Ty anot b mt thp cMc lm sch
ht mng oxit mt cch c hc do kim loi b tan nn lp oxit trn n t bong ra. Ty anot ch dng
cho cc vt' c hnh dng n gin, vt phc tp ty s khong u. Mt dng in ty thng 5 =
10 /dm2, in th
trn b ty 3 = sv.
Ty catot cng tin hnh trong dung dch axit hay dung dch mui kim loi kim. Hydro that ra
trn catot mt mt s kh lp oxit ca kim loi eatot mt khc bt kh hydro bc ra lm bong c hc
lp oxit khi b mt catot. Khng nn ty catot qu lu, nht l ty cho cc vt mng, mnh, dy, nhp, l
xo ...v s b dn, d gy. Anot dng kim loi khng tan trong dung dch ty nhtf ch chng hn. Thnh
phn dung dch ty anot v ch ty trnh by ph Sc 4.
Tf m Cc in cc hay mu th nghim lm t kim loi mi, sng, sch hoc kim loi tibc mi
c hc sng, sch ...vn c mt Sp oxit rt mng khng nhn thy bng mt thog. Soi b lp ny
cn phl lay nh hay cn g l hot ng ho b mt bng di nhng chng trong mt thi gian rt ngn
10 -2Gs vo dung dch axit long, mui kim ioi long hay kim long. Thnh phn v ch ty nh ghi
ph lc 5.
ut b mu th nghim : Trong cc th nghim thlng dng mu nh v t, nn cho tin c th
lm sch b mt bng c hc (mi trn my hoc nh giy nhm^v ty bng pSv ng php ho hc, c
th nh/ sau :
T
Chun b[ in cc v mu hng ng, ong thau, nhm:
Lau sch V nh bng giy nhm cho ht lp oxit dy trn mt, o Ra n|fc l (khng s
tay vo b mt k t y n cui th nghim), o Nhng vo HNO3 c: vi ng v ng thau
2 - 3s, vi nhm 3 ~ 5s,
Ra dti vi nn?c, o Thm kh b mt bng giy
lc.
Nu b mt sng, sch, nhn, khng cn vt oxt l t yu cu.
Chun b in cc v mu bing st thp:
Lau sch v nh giy nhm cho ht lp oxt v cc tp bn,
0 Ty du m,
o Ra n^e S (khng s tay vo b mt k t y n cui th nghim),
0 Ty trong H2SO410% nhit thng ong 5 10 s,
Ra f|i vi ijj?c,
0 Thm kh b mt bng giy Sc, nu cn.
Nu ch dng ngay phi ngm vo dung dch Na2C03 3% hn ch b oxy ho tr li. Tr0c khi
dng li phi ty nh, ra.
Chun bin cc v mu kim loi trc khi cn rvpn phn tch:
in cc hay mu nghin cu bng ng, ng mau, nhm hoc thp tritc in phn cn phi
cn bit trng nng ban u th cng phi gia cng nh^trn, ch khc l sau khi ty trong axit, ra,
thm kh bng giy lc cn sy trong t sy 105 -110 c khong 10-15 ph, ngui trong bnh ht m
n nhit th-tlng ri mi cn.
in cc hay mu sau khi in phn cn cn bit trng Ifefbng cui cng phi ra sch dtri
vi nbc, thm kh v sy nhy trn, ngui trong bnh ht m ri mi cn.
Trong qu trnh thao tc ni trn khng ^c s tay vo b mt mu, phi t chng trn giy lc
hay a thu tinh.
1.3 Chun bvdung dlch in phn
Hocht thng dng loi sch (P) pha ch dung dch. Trong mt s trng hp tht cn
thit c th dng loi siu sch (PA), nh^ng cng c khi ch cn dng loi k thut l (v d cc dung
dch ty chng hn). Chn loi ho cht no l tu mc ch yu cu ca th nghim. Khng nht thit
lc no cng phi dng loi p hc PA tn km m khng ch g.
Cn ho cht c th dng cn k thut cn cc cht cn trng Itng ln, hay cn nng ln
hng trm g/l hoc pha cc dung dch ph tr nh*? cc dung dch ty chang hn. Dng cn phn tch
cn cc cht pha vi nng nh, cn chnh xc cao, nlW cac dung dch nghin cu chnh, cc dung
dch phn tch, cc ph ga c nng rt nh. Try/ng hp ph gia cn nng qu nh, kh cn, c
th cn vi ydrsg v pha thnh dung dch tng c ri dng buret hay pipet o th tch cn thit
chia c vo dung dch nghin cu n nng mong mun.
Khi cn nht thit phi ho cht trn a thu tinh, trn giy ...khng - c php ho cht
trc tip trn mt i cn .
kts v pha ch ung dh dng pha ch dung dch phi dng rt/c ct. Mt s dung dch
chnh, cn nghin cn vi chnh xc cao phi dng rdc cat has ln. Khi pha ch, lng n#c
ban u ch nn ly'bng 1/2 n 2/3 th tch CUI cn c. Cc ho cht cht kh tan phi ho tan tr-
e tin bng rtc nng, khuy cho tan ht ri mi tip tc cho thm tng cht khc vo cho n
ht.
Khi tan ht mi th ho cht cn pha, b sung thm nttc n ng th tch mong mun.
Cc dung dch cn nng chnh xc phi o th tch trong bnh cu nh mc, cc dung dch ph
khng cn thit phi c nng tht chnh xc th o th tch trong ng ong hay trong cc chia .
Pha ch ng th tch
xong mi cftilbc lc dung dch . Sau khi Sc th tch c th b hao hut t nhiu, h{)g dh v th m b
thm nHe vo I
Nu phi lm nhiu sn th nghim trn cng mt loi dung dch th phi pha ngay t u mt th tch
ln dng cho cc in th nghim .
1 =4 HlSu sut dhg dim* BD lng k
Xc nh hiu sut dng in (H) phi da trn has quy lut v quan h
gia Ittng sn phm bin i trn in cc VI ltf?ng in i qua dung dch in phn:
1. Trng tt/ng bin i trn in cc ca mt cht t l vi in^ng i qua, v
2. Trng ung bin i trn in cc ca cc cht khc nhau kh cho cng mt in Mng
nhbf nhau i qua th t l vi <%ng tng ho hc ca chng.
bin i trn in cc mt y!ng tng gam ca mt cht bt k u
cn n mt irtng bng mt ilbng i-iig in ho, tc 1 faraday hay 26,8 Ah.
V 1 F - 96493 culong, m 1 cuong s 1A X 1s
nn 1Ah - 1A. 36GS 3600 cuSong do 1F = 96493/ 3600 =
26sh.
Gi s cho dng in fi ampe qua dung dch in phn kt ta kim loi trong X gi th I-
mg kim bi kt ta m tnh ton theo l thuyt s S :
m = I.T.C / 26,8 g (1)
Trong c - trng ng t/ng Sfng ca kim loi kt ta, =5 /n
A - trng Hng nguyn t ca kim loi kt ta (xem ph lc), n - bin i ho t ca
kim loi y.
Nh- ng nu cn in cc oatot tr^c v sau in phn s tm G IH/ng kim loi thc t kt ta
mc trn catot. L" dng ny thng b hn fefcng tnh ton theo l thuyt:
mo < m
iu chng t ch! c mt phn trong tng i4og in i qua -dc dng kt ta kim loi .
Phn in cn li dng cho cc phn hg in bo ph no , nh^phn ng gii phng hydro
chng hn.
T s tnh theo phn trm gia trng s^ng kim loi kt ta thc t m0 v trng h/ng kim loi
kt ta tnh theo l thuyt m gi l hiu sut dng in H :
H = 10Orrio / m , % (2)
Hay H = 100mo. 26,8/lxC, % (2 )
Nu bit r dn tch s ca catot c th tnh c chiu dy trung bnh s ca lp kt ta cng
nh^th gian kt ta X theo cc biu thc sau :
s - ic xmH /y60.1000 , mm (3)
X = Sy.60.1000 /ic m H, ph (4)
trong s = chiu dy lp kt ta , mm t - thi gian in phn, ph ic = s/s - mt
dng in catot, A/dm2, m = C/26,8 = S ng kim loi kt ta sau 1 Ahs g c
- trng I- ng - ng S- ng ca kim Sol kt ta, g H hiu sut dng
in, %
- trng I ng ring ca kim Soi kt ta, g/cm3.
Biu thc (2 ) cng iibc dng tnh ton hiu sut dng in anot. Khi m 0 l I^ng cht thc
t bin i trn anot sau in phn.
L^ng vt cht bin i trn in cc t l vi tytong in i qua , v vy c th dng mt qu trnh
in ho o l-ng l-ng in i qua, nu qu trnh in ho ch xy ra s bin i ca mt cht dy
nht v cht y c kh nng o m d dng.
Dng c xc nh in - ng bng cch xc nh 1 ng vt cht bin i trn in cc sau khi
in phn gi l in lung k. C cc loi in I- ng k sau
in I- ng k chun : I- ng cht bin i trn in cc tan vo dung dch in phn, xc nh I-
ng cht ny bng ph- ng php phn tch chun ;
in - ng k kh: sn phm phn ng in cc l cht kh, - c xc nh bng cc thu nhn kh thot
ra v o th tch ca n;
in I- ng k trng I- ng : sn phm phn ng bm trn catot hay tan khi anot - c xc nh bng
cch cn trng I- ng in cc tr- c v sau in phn.
Ti rong phng th nghim th- ng dng in I- ng k trng l- ng : in I- ng k bc cho chnh
xc cao, sai s ~ 0,005%, nh- ng t; in I- ng k ng r hn nh-ng cng km chnh xc hn, sai s ~
0,1 - 0,05%. i vi cc th nghim k thut dng in I- ng k ng l kh ph hp.
Cu t.o in lng k ng
in -ng k ng chnh l mt bnh in phn ng mc ni tip vo mch in phn. N gm
mt bnh th tinh (hnh 1.6) c 2 not ng in gii dy ~2 mm, treo i din nhau v st thnh bnh,
cch y 1-2 cm. Cc anot
- c ni vi nhau bng dy dn (ng) ri u vo cc dbng (+) ca ngun in mt chiu. Catot ca
in l-Kng k bng ng l hay nhm l, -tc treo song song vo ga 2 anot v cch u nhau. Din
tch catt (c 2 mt) phi chn sao cho mt dng in trn catot ny nm trong gii hn 1-2 A/dm2. V
vy mi khi thay i mt dng in cho qu trnh in phn cn phi tnh li xem mt dng
in trn catot in Iffbng k cn nm trong gii hn trn khng. Nu ra ngoi gii hn phi thay
catot in Mng k c din tch ph hp.
Khi in Iffdng k lm vic qu 2h phi khuy dung dch ca n bng cch khuy hay sc kh C02
san bng nng trong ton khi dung dch, trnh

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

Mun nghin cu mt qu trinh in ho no trn din cc lm vic w phi cho bnh


o in ho" vn hnh theo mt k thut, mt ch , mt ph- ng php nht nh nh my
pht c b phn potentiostat / galvanostat m nhn. V d my pht c th la mt scanning
to ra mt th hay mt dng bin thin theo mt cch thc no (nh- xung vung, xung tam
gic, bc thang ) gia in cc Sm vic w v in cc l c ; hoc c th l mt my pht
tn hu xoay chiu hnh 'sin, tn sf ...Kh vn hnh h thng, cc thng so ca qu trnh o
theo yu cu ca ta nh- tc qut, khoang th qut, s chu k, dng din ... " c ci t,
thit lp tr- c trn thit b ny.
Tn hiu ca cc qu trnh in h xy ra trn in cc Sm vic w s = c chuyn
vo" SPU nhd eac in cc" w v R. B chuyn i SPU c nhim v thu nhn tn hiu,
chuyn i, x l tn hiu ...cho ph hp vi81 ngn ng ca my tnh PC. My tnh PC c ci
t phn mm t- ng thch vi k thut chn cho php o x S cc s Siu thu nhn ri
hin th Sn mn hnh monitor hay & c
Mt s k thut o - c trinh by trong cc bi th nghim ch- ng 3, ti ch- ng
ny s cp n nhng vn th ng gp nht trong cc th nghim o c in ho nh-
binh c, in cc nghin cu, in cc so snh, n- c, dung dch...
.2 Binh Sn h@
Bnh o S mt bnh in phn c hnh dng c bit hoc hnh dng thng
thing, cha dung dch nghin cu v cc in Cc, cho php tin hanh c phn hg phc
tp cn kho st. Nhiu th nghim in ho cn chnh xc cao nn vt liu v cu to
bnh o phi m bo mt s yu cu nht tnh.
2.2.1* Yktts wktom
Vt liu bnh o phi bn ho hc, th- ng bng thu inh loi c bit Thc ra cc ioi
hu tirsh ny vn khng tuyt i bn ho, mt stf thnh phn trong thu tinh c th bi tan vo
dung dfch mh- cc cation a ho tr, cc anion silicat
lm bn dung dich nghin cfiy. Bang 2.1 lt k mt s loi thu tinh bn ho.
Bng 2.1. bn hc ca mt s loi thu tinh dng trong th nghim
Loi Thnh phn, trng 1- mg, % Tn th trng 1- Qg (mg) trn 10
thuy . em2 bmiMm si 3 to
tinh Si3 23 I2O2 MgO Ca BaO NazO ICs Ha H2S4 NaOIB Na2S04
(c) M I 2N

N22 68,4 2,3 3,9 - - 9,4 7,1 0,30- 0,14- 40- 8


0,84 0,40 59
N29 3,7 3,5 - 3,5 10,0 3,0 0,20- 0,26 38-
68,6 6
0,70 59
Pyrecs 80,5 12, 2,0 - 0,5 - 4,0 1,0 0,36 0,52 4 27
0 - - - -
Yense 74,9 . 7,4 5,3 1,2 3,4 8,0 0,45 0,6

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.

Hnh 2.3. Mi S loi van v np nhm, a - van n; b - van cha; c


- van np; d - np nhm m; e - mp nhm kp. (phn gch cho l c - c
php bi trott bng m chm kng cao; van cha chng khng kh lt vo
bnh o).
Nhiu tr- ng hp oxy trong khng kh ho tan vo dung dch nghin cn
gy sai lch kt qua thc nghim, nn bnh o phi c trang bf ng sc kh tr (Na, Ar, He)
n b h@ ui ht O2 ho tan tr-c khi o c.
Ngoi vt Siu thu tinh c th dng vt Su cht do teflon ch to bnh o. Nh-ng
bt tin ch teflon khng trong sut, d bin dng v cng khng phi hon ton bn ho. N
c th tc dng vi hn hng chte nhiu kim loi kim.
Phi m b dung ich trong binh o khng tip Ke vi ca su, cht do, da ...v
chng l ngun cung cp cc tp cht hot ng b mt, nh hng n qu trinh in cc.
Bnh o h ng c np nhm, van nhm, kh thao tc, vn hnh chng phi cn thn.
d vn hoc d ng m cn thm dt chng tr= e bng chnh cc dung mi dng pha ch
cc dung dch nghin cy (ro- ct, dung mi khng n- ..). Hn hy ch php bi trdn bng
m chn khng ca ti mt s cnh, mp ca van v np. Hnh 2.3 gil thiu mt s van, np
mi nhm.
al Bd @ ym w
Binh o in ho ti thiu phi c 2 in cc thng dng Sn qua dung dfdfo nghin
ey, nh= ng cng c th c 3 'in cc hoc hm ...
h ym pnh 2.4) t- ng dng :
o Lim sch dung dich tr= c khi in phn, nghin C0J, o c ...
o o dn din @ dng didh bng chun fi ;

Hnh 2.4. Blfflti o in ho 2 cc.


w - in cc lm vic; c - in cc i; 1 - van ngn ring khng gian anot v catot; 2 - ttg iu phong trnh khng kh lt vo bnh; 3 -
- ng sc kh tr vo dung dch.

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

Hnh 2.5. Bnh o in o ba cc


1 - in cc lm vic W; 2 - in cc ph C; 3 - van; 4 - ma qun Luggin;
5 - - ng kh tr vo; 6 - in cc so snh R; 7 - ng thu phong.

Nh- ng trong dung dch lun c in th r, nn nht thit phi o in th


ti mt im c nh, st vi in cc w. Mun vy phi dng cu mui c u
21
mt vut nh thnh mao qun, t st b mt in cc W, cn u kia thng vi in cc S
snh RL Bn trong cu mui khng xut hin in th ri, vl mg in phn cc ch? i trong'
dung dch qua hai in cc W v . VI vy u mao qun ca cu mui cng gn vi b mt
in cc W th in th ri trong dung
dch gia n v in cc W cng b v in th in cc W o c cng ng tin cy hn.
Nh~ mg du sao u mao qun cng lam thay i s phn b dng in trn b mt in cc
W, do lm bin i mt ng th ca n khi c dng in i qua. iu ny c th gy nn
sai s khi thit lp dmg cong phm cc. Himh 2.6 trinh by cc kiu u mao qun nhm
hm ch sai s mi trn, trong " kiu c l tt nht
, u map qun____;_____ _
f

1
0
w w w
a b c
Hnh 2.6. Mt s Msa ia mao qun t st
in cc w.

ch to kiu mao qum c mg= d ta dng mt dy Pt rt mt t nghing 45 vo iu


ng thuf tinh, hn tn ri mi phng u, sau ngm vo ng thu R tan hi f ra i
mh tn fiu mao qum mh= hnh 2.6.C.
Bnh o cn c ng thu timh nh fitf sc kh tro qua dung dch. Tf mg hp o qu th
thot hydro can phi sue kh hydro qua ng ny. Lc tim mht l dng n cc hydro
Sm Sn cc so snh RL tnh cho dung dich trong binh o tip xc vi khng kh bn ngoi
cn y kn binh o bng cc St nhrir, ring = ng thot kh ra khi bnh phi C ng thuf
phong.
Hlnh 2.4 v 2.S tnh by hnh thc v cu to ca bnh o 2 cc v 3 cc Soi trung
bnh, tu the tnh cht v nhim v m c th thay ts hnh thc v cu to m gim hn
hay ph&e Sp hn cho ph hp vi su kim v yu cu o c.
Khi o c th= ng c yu cu phi in phn mt Sc Sm sch dung dch tr- c
khi bt u Sy s Siu. Sm sch c th tin hnh trc tip ngay trong binh o, nh= mg lc
phi dng irs cc ph r khc thay ch cho din cc W, in phn xong b in cc ny
i v t in cc w vo bt u o c. Cng c th in phn lm sch dung dch mt
binh ring (nh= hnh 2.4) sau chuyn dung dch sang bnh o chnh thc.
1=3= ln cc
Binh o in ho c nhiu loi in cc: in cc Sm vic w, lm cc i (hay in
cc ph) G, in cc so snh R "...chng co cc chc nng nng. Vt liu in cc v cu to
ea chng cng rt khc nhau . Su y ta s xt tng Soai in cc y.
2.3.1. in cc lm vic:
in cc git thu ngn : Git thu ngn - c to ra t bnh cha Hg trn cao, -
c tip in v c ng ni n mao quan c - ng knh nh chy ra thnh tng
git nh k tip nhau. in cc ny c-u im l :
- B mt in cc lun - c i mi nn rt sch, khng b nh h- ng ca tp
cht, ca sn phm phn ng;
- B mt git rt nhn nn d tnh - c din tch thc ca in cc lm
vic;
- Phn cc u trn ton b b mt hnh cu;
- Thu ngn d lm sch dng li.
Tuy nhin Hg rt c nn hn ch s dng.
to - c in cc git Hg t yu cu cn ch :
Chn ng rriao qun c l trn u, khng mo, vt v nt n ...lm nh h-ng
n tnh cht dng chy ca dung dch in phn v tnh lp li cc kt qu thc nghim;
- Chn chiu di I v bn knh ming l r ca mao qun da vo nguyn tc sau :
Mun Hg chy qua ng mao qun - c v to thnh tng git mt, lin tip nhau, ch
khng chy thnh tia lin tc th p sut p ca ct thu ngn (tnh t y git n mt
thong trn bnh cha) khng - c qu b hoc qu ln, m phi tho mn bt ng
thc sau :
2.0 la < p < 16.1 .T] / r2 .g. Y (1)
trong - sc cng bin trong git Hg;
a bn knh git thu ngn, r bn
knh ming mao qun - trng I"
ng ling ca Hg; x\ nht ca
thu ngn;
I - chiu di ng mao qun; g ~ gia
tc trng tr- ng p p sut ct Hg .
Nu gi m l trng I- ng ca tSiu ngn chy qua mao qun trong 1 n v thi
gian th
m n r 4P / 8.1 T|
v trng I" ng ca git hu ngn ti thi im X s l :
rm s 4w a3y / 3
cho nn = (3sm / 4rey )1/s
Thay gi tr ca a vo (1) s c.
2.0 / (3mt / Aiq )m < p < 16.1 .TJ / 2 .g. (2)
T (2) cho php tm ra kch th- c 1 vr ca mao qun tt nht lm in cc git
Hg. Th-dng r S 50 pm v I 15 - 20 cm.
i khi cn phi khc phc hin t" ng thm thu dung dch in gii vo bn trong l
mao qun, gia thu ngn v thnh ng, bng cch ph mt lp silicon khng thm n- c.
Mun vy nhng mao qun vo silicon, sau ly ra, thi eh silicon lng trong mao quan
ehy ra ri say mao qun nhit cao*
Ngoi Hg ng~ i ta cn ch to in cc git t nhng kim Soi nng chy khc nh-
Bi, Ga, hn hng ...nh- ng phc tp hdn rt nhiu, v phi gi nhit cao kim loi
Sun d trng thi sng.
Bn B in cc rn tin s dng hn nn - dng rt ph bin. Tuy nSn
Schi dng in cc rn phl 1 u :
- Vt liu in cc phi rt sch. Ngay khi dng vt Siu siu sch r m kt qu o
vn sai khc nhau bi v cu trc b mt (nh hng inh th, eSing SoS v mt lch
e chng khng ging nhau.
- Cu tric b mt in cc rn khng ch! ph thuc vo cu trc vt liu ban u
m cn vo cch gia cng chun bi b mt in cc rfe (mi, t in ho, x !f nhit, ch
phn cc ...)
- Cu re b mt cn c th bi thay i ngay trong qu trnh o c. Nh= ng mu phin
cc in cc the mt ohb ong trnh c bit hl c th iu khin & cu trc b mt ft
mun.
- B mt thc 3* ea in cc rn b&o S oGmg Sn hn b mil hnh hc s ca n.
T s S / s chnh S nhm b mt. S*/3 cng >1 nhm b mt cng Sn, kt qu
o cng sai Sch v cng Sth lp li. Whl so snh, i chiu v giS thfeh cc s liu thc
nghim cn phl 1= u n yu t ny.
- Khc VI b mt tln c lng, b mt tin cc rn c ning 1 ng khng ng nht
(tc bit S vt liu a tinh) Sm kh khin cho vic nghin cu v gii thch cc quy lut cu
te ip kp cng mb ng hoc cc qu trnh tln cc.
- kt qu o trn in ete rn ~ c lp li fli khi phl dng cc bin php 0= img
bc lm s M lin tc b mt in cc ngay trong qu trnh nghin cu, o c, nhm loi
tr cc cht hp ph, cc cht gn bm Sm bin cht b mt ...bng cch Sm ch in
cc quay v ip xc VS vt lu mi hay 1= 08 dao c bit (bng , xa phia).
- Hnh thc v kt cu in cc rn st a dng, c loi m gin nh cc in cc
dng trong in phn (hnh 1.3) hoc phc tp 1 mg t nh~ cc in cc da quay (hnh 2.7
v 2.8). Vt liu in cc c th l kim loi hay lp xit cn nghin cu, cng c th l in
cc tr bng Pt, Au ...Hnh dng s th S dy, l, ng, da, S i ...tu ngha, mc ch
ca tng th nghim.
Bin (Siyus quay w m^Wing fsay
in cc rn dng a quay 0 = u im ln S mt dng in phn b rt u
trn b mt in cc v dong in c lin h nh S" ng vi nhu thng s in ho nn
in cte ny r e dng kh ph bin trong nghin cu lrs ho. '
dh to ira a quay cn phi cch in sc mt bn oa n. Thc
hin iu ny bng cch c, hn in cc trong khi thu tinh hoc Sng p cht th kim
Soi vo ng teflon. dung dch in gii Scbng thm vo km gia Sm loi v ng
teflon, ts tm si phi c <= ng knh 8n hn = ng knh lng ng teion, tr- c khi lng
cn sy nng ng teflon cho n mm roi lng p thi kim loi vo, ngui cho teflon co li
m cht kht vi kim loi. Mt u gia cng thnh b mt in cc a, u kia - c tip
in v ni vi c cu quay (hnh 2.7). iu quan trong cn -u l trc in cc phi trng
vi trc quay v mt phng a phi thang gc vi trc quay. Nu khng th khi quay s
3
Hnh 2.7. in cc a quay.
1 - trc, 2 - teflon, 3 - kim loi in cc (dng a)

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).

I = in cc vng; 2 in cc a; 3 - teflon; 4 - dy ni in; 5 - xuyn tip in cho in


cc a; 6 = xuyn tip in cho in cc vng; 7 - u ni cch in.
Khi in cc a v in cc vng phi m bo hon ton cch in nhau. a v vng
phi ng tm v cng nm trn mt mt phng thng gc vi trc quay, nlr ng c hai ng
ip in ring. Binh in phn dng cho Soi in cc ny phi c thm mt in cc i
na phn cc cho in Cc vng.
C cu quay ch cc toi in cc quay ny c th m mua trn thi tr- ng. Tc
quay phi iu chnh " t nh n 3600 vng/ph hoc htn.
'ZZ B m s
in Cc i c th Sm t cc vt iSu khc nhau, nh~ mg h= ng S Pt v n bn
trong nhiu mi tr= dng. Hnh dng c rs c th i dy, S, S= S.. x hnh th nh~ hnh
1.3. Khi c bng in cc git thu ngn th in cc c th dng ngay S Sp thu
ngn ISay bnh. Nu in cc i = dt khoang ring c van thu inh nhm each Sy
th in cc i khng gy nh h= ng gl ng ng n qu trinh rn in cc W cng nh=
n in phim Gia in cc W.
ZZL Bm c so snh
Khi f n ho trong cc dung dtoh r> c tb= ng dng nht l cc n cc 80
snh hydro, caSoroeS, bc orua, tbu ngn xt... in th ca mt s cc in cc i snh
= e ghi trong bng 2.2.

(so v dn th agin cc hydro tSo chun 1M)


Tn Sm cc Hthng in ho in th, V
Hydro iu chun SHE P lTfe(l5m)l H Um 0,000

Hg! HgaCb ,KGS bo ho 0,244 = Q,0003(t = 2S)


Calomel bfie ho 8CE Calomel
HgHCb.Ka 1,0i Hg I 0,283
iu hum Calomel 0,1 ftl KCl
SdgaCla, KCS 0,1 M 0,33 = 0,00007(1 = 25)

g I AgCS , KG bfio ho 0,199


Bc oru, bio h@ Bc eSorua,
ggCS, KCS' 3,5 M AglAflCi 0,205
3,5 y KCS Bc clorua, tiu chun
.KCI 1,0 M 0,222 = 0,0003(1 = 25)

TThu ngn xit, tiu chun HglHgO KOH 1,0 M 0,098


Thu ngn xit HgingOsCOH 0,1 M 0,165 - 0,0002(1 = 25)

ng sunfat, bo ho ng Cu CUSO boho CuS4 0,318 = 0,0007(1 = 25)


sunfat, tiu chun Cu 1,0 M 0,337

8ng 2.2. B&B 'S su S m os &f


Bm h$fm
Sn cc hydro (hnh 2.9) gm mt S hay S= i Pt = de m in Pt, nhng mt
phn vo dung dfch HO1,1811 ( c hot IHP bng 1) v sc kh hydro qua dung
dch ny cho n khi t p sut ring phn S 1 atm.
M Pt ln Pt tin hnh nh sau: l hay I- i Pt ty nh trong o ng toan si (1 th tch
HN03 c + 2 th tch HCI c), ra n- c 2 ln, phn cc anot trong HCI 1M 10 - 20
mA/cm2, ra li 2 ln trong n-c ct, phn cc catot trong dung dch H2SO4 0.05M 10
20 mA/cm2, ra, nhng vo dung dch m gm 1 - 2% H2PtCle . Kt ta Pt mu en thu -
c ti mt dng in 2-6 mA/cm2 trong 0,5 - 2 h sao cho t - c 3 5 m"g Pt/cm2.
in cc m xong ra 2 ln bng n- c ct ri phn cc ctt trong H2SO4 0,05% M. B
qun in cc trong n- c ct hai ln.
in cc hydro s dng tt trong khong pH kh rng ca cc dung dch n- c. Nh-
ng ring vi cc "dung dch trng tnh in cc hydro ch c th lm vic bnh th- ng nu

Hnh 2.9. Mt kiu in cc hydro.


nh- dung dch c tnh m tt, bi v kh c mt dng in d rt nh 'di qua cung
cho on Hr xut hin thm hay mt bt i, Sm cho pH b thay i, do in th cn bng
ca in cc hydro s thay i theo.
in cc hydro c th dng trong di nhit kh rng, tuy nhin dng nhit
cao phai k n vic p sut ring phn ca hydro gim i (do p sut hi ca dung dch
tng ln)/
Ct dung ch t ghi xp ( phn tn kh Ha) m mt thong cng ln th phi dng
kh hydro c p sut cng ln (>1 atrm).
Tr-c khi o phi sc kh hydro qua n cc 20 - 30 ph dung dch HCI t n bo
ho Ha. Ng ra b mt Pt rt d b ng c nu c mt cht hu ed, kim loi ...hp ph ln,
rt t Do khng c dng ng cao su ni cc b phn thu tinh trong h th nghim (v
sunfua t cao su thi ra Snn ng Pt r nhanh).
Do nhng phin phc ni trn nn ng- di ta hay dng cc in cc so snh khc tin
dng hn thay th cho in cc ny.
Bin im Gamei
Calomel l tn gi ca HgaCl. in cc calomel l mt trong nhng in
cc so snh c dng rng ri nht vl n- kh tin cy li n gin, d s dng (hnh 2.10).
T ph ng trnh Nemst rt ra in th n cc ca calomel l :
<Pcai 0,268 (RT/F)ln 3cr
Vy in th in cc calomel cng m khi hot ion G- trona dung dch
cng Sn (xem bang 2.2). Thng dng nht vn l in c calomel bi ho (SCE), trong
dung dch KCI & trng thi bo ho nh ng vn ho thm c tinh th KQ vo d tr. in
cc calomel hi Sm vic n 70c v trn 80G calomel b phn hu, va sai s Sn v
gy c hi. Tr=dng hp tht In thit phi ni in cc calomel qua mt cu mui KCI bo
ho, c m qun dn n st in c Ssir vic (nh= hnh 2.6), rnh Hg 2Cl2 t in c
ny c th thm nhp vo dung dch nghin U hoc ng- c li.

Hnh 2.10. Mt kiu in cc calomel.


- mp tip in; 2 - mt v mittg b suag dung dch; 3 - mt xp (bng thu tinh); 4 - ti
ICQ; 5 " ag thu tinh bn trong; 6 - dy P 5 tn vi np 1 v gm cht vdi ng 5; 7 - Hg;
8 - Hg 4- HgG (nghin chung thnh bt nho); 9 - nt xp; 10 - nt gn kt ng 5 vi 11; 1! - v
m tinh ca in cc; 12 - trng dch KQ ho ho

Bn <5c bic loras in sc so snh bc orua (hnh 1.11) ung c dung rt


rng ri v u to n gin, tin y ao, d s dng. M - c dng trong c nghin
eu ti phng th nghim pH, lm in c hn lc n, lm u d redox ln hp,
dung trong h bo v catot hng n mn, dng trong y t v khng c, dung o trong
cc mi tr- ng n c v khng n- c, c th lm vic n100"c.
in th in c bc dorua :
^Ag/Agci " 0,222 = (RT/F) In cr- , V
Vy in th ca n cng m khi nng ion Cl trong dung dch mg ln (bng
2.2).
Hnh 2.11 sau y gii thiu mt Soi u to a in c bc lorua. Dy bc -
c ph mt Sp AgO bng ph" ng php kt ta nhit hay kt ta in ho,
t vo dung dch KO trong mt ng thu inti, mt u ni vi phn tlp in, mt u thu
nh vi nt s xp d nhng vo dung |h 5 in c Sm vic w cn o c. V AgCI d
tan vo dung dch KCI m c nn khi ch to in cc bc clorua cn cho dung dch KC - c
bo ho AgCI tr- c ri mi np vo in cc. Nh- c im ca in cc so sanh bc dorua l d
b nh sng lm phn hu AgCI thnh Ag, d b cc ligan to phc nh- CN~ , NH 4+ ...to vi Ag
hoc AgCI thnh cc phc cht d tan. Cc cht kh mnh hay oxy ho mnh, cc sunfua ...ln
vo cng lm h- hng in cc.

Hnh 2.11. Mt kiu in cc so snh bc clorua


1 - dy ng dn in; 2 - nt gn; 3 - dy bc; 4 - lp AgG; 5 - dung dch
KQ IM; 6- np nha; 7 - l rt dung dch; 8 - vng nha do bt l rt dung
dch; 9 - v u tinh, di 130 mm, - g knh 12 mm; 10 - Et s xp.
Bn es su ngn mt
in cc Hg I HgO, KOH c dng o trc tip trong cc dung dch kim m
khng cn cu mui trung gian . in th in cc Sol tiu chun (1M) l 0,098 V; loi 0,1
M l 165 V (xem bng 2.2).
Bn em ng mft
in cc ny " de dng trong cc th nghim v kt ta ng v c bit hay dng
o c trong n mn v bo v kim loi, v d gim st cc " ng ng thp t ngm
trong t ang - c bo v catot u im l n gin, chc chn d ch to.
ng ra in cc Cu I CuS04 khng phi l mt in cc so snh thc th v in th
ca n b nh h= ng i cht bi cc phn tig ph khc nh phn hg n mn ng do tc
dng kh ca oxy h tan trong dung dch ca in cc ny. V vy in cc ny ch! - c
dng cho cc tr- dng hp khng i hi chnh xc cao.
Cu to ca in cc ng sunfat e gii thiu hnh 2.12.
1
2

Hnh 2.12. in cc so snh ng sunfat dng trong nghin cu n mn.


1 - o e cc; 2 - nt gn km; 3 - thi ng; 4 -Ttang dch Q1SO4 bo ho;
5 - tnh th CuS04; 6 - nt nha xp; 7 - ng nha chc chn.
smmg gm ikgm S
Thao spy - 6c in th irs cc hydro tiu chun c gi trf l 0,000 V, t c
thang din th hydro SHE nh= hnh 2.13a. Wh=ng din cc oaSomal bo ho tin dng hdn
nn hay dng in th in cc esSomoi Sm mc chun t o Sn th cc Sirs cc khc
(hnh 3.13) theo thang SGE. Cc gi r in th o theo thang SCE khi i sang thang SHE
Y V/ 0.096
0,340 s
0,310 GujDu *iy 0,074
Cu|CuS4 bioho

0,244 Hg I HgsCla IKCS b.ho - 0,000


Hg I HgaCla I KCl 1M
0,222 =0,022

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.

phi cng thm 0,244 nk


2.3.4. in cc dng in phn tfc
Nhiu dung dch sau kh pha ch phi in phn x l tr- c khi dng. Vic chn
in cc cho qu trnh in phn tr- c ny cn phi thn trng. V d khi dng Pt hay Pt
m Pt lm in cc in phn x l tr- c c th Pt s chuyn vo dung dch d l kim
hay axit ngay c khi dng in th anot rt thp. Sau Pt t dung dch x l s kt ta
catot ln cc in cc nghin cu khng phi l Pt gy nn nhng sai lch trong kt qu
o c, cho d I- ng Pt ho tan ny rt nh.
Tt nht l dng in cc in phn tr- c cng loi vt liu vi in cc nghin
cu. Bt k tr- rig hp no can dng 2 hay nhiu in cc in phn tr- c u phi
m bo rng in phn tr- c khng gy nn mt nh h- ng ph no.
2.4. Lm sctch nc.
Tp cht trong dung dch in gii v trong vt liu in cc s lm sai lch cc kt
qu o c ca cc th nghim in ho. V vy cn phi lm sch n- c v cc dung mi,
cc ho cht va thuc th v c hay hu c, cc kh v vt liu in cc ...dng trong th
nghim in ho.
N- c my ch- a sch cho cc th nghim in ho v: mt l n- c my cn nhiu
muoi v axit ho tan lm tng dn in, hoc tham gia vo cc qua trnh in ho trn
in cc . Hai l cc cht hot ng b mt c trong n- c my hp ph ln in cc lm
thay di tnh cht b mt in cc cng nh- din tch tip xc gia in cc v dung dch
in gii, nh h- ng n tc phn ng in hoT
Cho nn nht thit phi lm sch 0 c my tr- c khi dng pha ch dung dch in
gii. C hai nhm ph- ng php chnh lm sch n- c l ch- ng ct v trao i ion. /-
2.4.1. Chng ntic
Chhg ct l tch cn ho tan, kh bay hi ra khi n-c. Nh ng thc t n- c
ct thu - c t cc my ct n- c th- ng phm vn khng loi ht - c
cc cn bn, nguyn nhn l trong lng my ct n- c lun c mng n- c mng ni lin
tc t bnh ch- ng ct sang bnh cha n- c ch- ng ct, cn ho tan c th theo
m lm bn n- c cat Mt khc khi ch- ng ct hi n- c bc ln. c th ko theo cc
git n- c nh, bn t binh ch- ng ct, nht l khi ct v tc nhanh. khc phc nh- de
im ny, ng- i ta dng n- c ct hai ln hoc ba ln t cc thit b ci tin, hin i t
cht l- ng f> c ct cao nht.
Cng c th t lp y b ch- ng ct n- c hai ln hay ba ln trong phng th nghim
nh= hnh 2.14 c n- c tinh khit hn.
N- c ct mt ln (hoc hai ln) cho vo bnh cu 1 bng thu tinh pyrecs c th tch
ln ( 1 - 5 lt), un nng bnh ny bng dy in tr qun hay t xung quanh bnh. Cc khp
ni u bng thu tinh nhm (khng dng ng cao su hay cht do). B ng- ng hi I- u 2 c
tc dng thu gi li cc git n= c nh t bnh 1 b cun theo hi n= c. Bnh cha n- c ct
4 phi c c nhm. Tt c cc b phn thu tinh khc phi lm bng thu tinh yens bn
ho.
C 1 lit n- c cho vo binh 1 cn cho thm 1 ml H2SO4 c Soi tinh kht phn tch
v 3 ml KMn04 3% oxy ho cc cht hu c c phn t ln. Th tch dung dch KMnCU
c th thay i tu theo sch ca ngun n- c ban u.
Phn n- c ct thu -c u tin (khong 1/5 th tch n- c trong Wnh 1) phi b i, ch dng
phn n=c ct on gia. Hng ngy phi x h phn n-c sn ca binh qua van 5 v thay
n- c mi C th dng bt grafit loi sch bi rm cho van 5 d vn.
Hnh 2.14. Dng c ch- ng ct n- c.'
1 - bnh cu; 2 -b ng- lg hi 1-u; 3 - ng sinh hn; 4 - bnh cha n- c e; 5 - van.

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.

Than hot tnh phi dng loi c bit, khng cn du vt cc tp cht hu


cd8 ch to n nh sau ; ly than hot tnh ky thut sng ly kch th- c trung binh (b ht qu
vun v qu ln), un si vi axi HF c ri li un vi S)dt HO! c cho n kh khng cn axit
Sau than - c un SI vi n- c ct, thay n- c nhiu ln cho n kh khng cn on clo
trong n- c ra. Dng n- c ct hai ln cho vo than v un n soi. sy 120 - 150c, nung
24 h trong l ng thch anh 800 - 900c c dng kh hydro i qua. un si trong n- c ct
hai ln c thm 2-3 git KOH c. Ra than bng n- c ct hai ln, sy v nung l trong l
thch anh c dng kh hydro i qua trong 24 h 800 - 900c.
Than thu - c bng eh ny s khng lm thay i dn in ring ca n= c ct hai
ln v loi b khi n- c " dc ht cc du vt ca mi cht hu C hot ng b mt (nh "
ng 5 hnh 2.5).
Bo qun n- c ct trong bnh cu bng thu tinh bn ho c nt nhm tht tt, s gi
cho n-c khng b thay i tnh cht trng vl ba ngy.
2*4,2. Lm sch nc bng nha rm on
Ph" ng php ny hin ang - dc s dng rng ri. Nha trao i ion l cc hp cht
cao phn t khng tan, c cha cc nhm Ion hydroxyl -OH v nhm hydroxon H30+ c kh
nng tham gia phn ng trao i VI cc ion khc cha trong m= c. Cc hp cht phn ly
trong f c c loi b bng cch Sc c lin tip qua cc ct catonit v anont ring bit
hoc qua ct cha ng thi c
33
cationit sn anionit. Ph~ ng php ny thu - e n~ c c dn in ring rt b, nh- ng
th= ng cn st ii vt cc tp cht hGu do chng thi ra t bn thn nha trao i ion,
l cc mosiosne cn st Sl khng c polyme ho, cc Chat xc tc tng hp, v
cc hp ht n nh cao phn t c trong nha. VI vy n=c lm sch bng phng
php ny khng dc dng trong cc nghin cu v cu to lp kp v v ng hc in
ho.
Ngoi = c ra trong mt s tr= dng hp th nghim in ho phi tim hnh trong cc
dung mi hu C nh- -du, emit (MNH2) nitril ...Cc cht ny tr= c kh dng cng phi = c
Sm sch theo nhhg ph dng php ring ph hp cho tng loi cht, tb-ng S ch-ng ct
n hay ch-ng ct phn on. Tuy nhin nhng cht qua ch- ng ct vn khng loi t
c hon ton mt s tp cht v lun cn st li mt t n~ C. Vic Sm sch cc dung mi
hu C i hi nhiu cng phu v i khi rt phc tp.
lo T% r bnh o v dung c th l nghim
Tt c cc th nghim nghin fiy v ng hc din ho phi = 0 tin hnh trong
iu Sttn tuyt i sch. Vi vy binh o v dng c thu tinh cung phi ty ra tnt sch.
ty ra = hiu qu cn bit r inh cht cc cht bn bm 'trn dng c wh= chng c th
ten <3= c trong n= c Snh hsy rb c nng, tan trong sm hay axit, c th bi xy ho bin
thinh cht d ten khng ...
rTh=dnp bnh <h vi ng c thu| thh bn phl rs bng dung d|ch hteaCO, c bng
chi Sng sch. Cc ng nh cc ch kb Sun chi hi c bng vi hay giy Sc v ra
81= c mhiu sn. Sau ngm chng vo H 2SO4 nng hay hn hp cromat nng, nh rng
phi ngm ton b b mt binh v dng c, k e ming nhm, nt m, van ...
Hn hp cromat ph ch nh sau : ho tan 15 g SCaOra? vo 100 mS n=c nng. Khi
ngui, vta Sthuy va nh t 100 ml H2SO4 c v. Hn hp c mu nu, dng
ra nhiu ln, SDi hn hop bin thinh mu Sc mi b .
Ra sch H2SO4 bng 0 c my v trng li vi b ln bng n= c t mt Sn, bai
sn ...Bnh o v dng c fi qua x S bng romat phi y n= ct ngm 12 = 18 h
Son CraO?3- hp ph c thi gian mh ra khi b mt thu inh.-Nhng qu trnh nghin
ey no nhy vi vt tp cht hOu c th khng de dng n=c my sa bnh o v
dng c thu tinh, m phi dng n-c ct hai Sn r& sau khi x l trong H2SO4 nng. Vi
H2SO4 thm = t thu inh rt tt nn bnh o v ng c thu inh phi ra k bng 0 c
nhiu ln, nu khng son HsCf st li nh h- ng n kt qu th nghim. Nu th nghim
tin hnh trong dung dch khng 0= c thi phi sy kh binh o v dng c tr= c khi dng.
Ch tr- c kh sy phi tho ri cc cc b phn ra khng & C sy cc b phn c cha
thu ngn.
trnh tp cht hOu c ln vo, khng c chm tay, s m vo cc b mt ca
binh o v dng- c thu tinh tel nhng ch s ip xc vi dung dch th nghim. Khng ~e
t nt, van, np ... lm sch ln mt bn, khngiy lc .., ch & c t chng trn mt
a hy khay thu tinh ty r sch nh chng.
Bnh o v dng c ihu tinh & c xem S ty ra i sch khi m mng n~ c c th
thm t ton b b mt, nu h a sch mng n= h s 0 li thnh - tng vng ring v
Sl nhiu vng khc khng thm = t n= c.
2.0. Pha ch dung dlch. Nt p v bi nh o
Nhiu th nghim in ho yu cu phi bit chnh xc nng dung dch nghin cu.
Mun vy I- ng cn phi - c tnh ton tr- c v phi t ho cht ln da knh ri mi cn trn
cn phn tch hay bn vi phn tch. Cn xong cn thn chuyn ho cht cn vo bnh cu nh
mc nh mt phu thu tinh sch, kho. Dng n-c ct (c sch ph hp vi yu cu th
nghim) rt/i trn phu cun ky ht ho cht vo bnh cu, khng - c st. Thm n- c
n khong 1/2 th tch cn thit, y nt nhm, lc bnh cu cho ho cht tan ht. Tip tc cho n-
c vo nh- ng phi thp hn vch nh mc 0,5 - 1 cm, y nt nhm v lc bnh mt ln na.
Cui cng cn thn thm tng git n- c ct vo bnh cu cho n khi t vch nh mc, y
nt nhm v lc bnh cu ln cht. Rt dung dch vo bnh o nlWsau :
Nu th nghim i hi phi sy kh bnh o tr-c, nh- khi lm vic vi dung dch khng n-c
chng hn, th dung dch nghin cm -c rt trc tip t bnh cu vo bnh o kh ri
bt u th nghim.
Nu th nghim khng yu cu phi sy kh bnh o tr- c th cn trng bnh o vi ba ln
bng chnh dung dch nghin c- u r mi rt dung dch vo bt u th nghim.
Khi tin hnh cc th nghim c bit cn thn c th pha ch dung dch nghin cu trc tip
ngay trong bnh o trnh tip xc gia dung dch vi khng kh trong phng thi' nghim.
2.7. Ti kt tinh mui. Lm Sch axit
i vi mt s nghin cu in ho th sch ca cc thuc th, ho cht
sn xut trong cng nghip l khng t yu cu, ngay c loi tinh khit ho hc hay tinh khit
phn tch K cng vy, v chng eon cha tap cht hOu ed d rt nh. bo nhu khi phi kt tnhl
cc mui bng n- c ct hai ln . s ln ti kt tnh c th l 1, 2 hoc 3, 4 ln tu theo yu cu ca
th nghim. Ti kt tinh tin hnh theo ph ng php ho hc v ch! dng nhng binh cha, dng
c ty ra nh- noi d mc 2.5.
Trong qu trnh thao tc ti kt tinh phi dng a thu tnh, cc thu tinh c np y cng
bng thu tnh, lc bng-tm lc thu tinh (khng dng-giy lc). Sau phi sy mui, nu c th
phi nung thm.
Mmi KC loi tinh khit phn tch u c ln tp cht hu c. Ti kt tinh cng nhiu ln
S ng tp cht ny cng t nh ng khng th no ht & c. Ch! sau khi ti kt tnh San th 4
ri nung 550c mi - c coi S ht tp cht hu c. Khi nung, lp mui trong chn nung ch!
nn dy 1 = 2 cm v phi nung trong 24h.
Mui NaSO kh ti kt tinh s cho tinh th ngm n= c NaaSCM 0H 2O nn tr- c khi nung
phi sy. Cc mui ngm n- c khi tng nhit th ng chy lng nn phi sy quay, nh- ng cn
y kn sao cho khng b ln tp cht C hc vo trong lc sy, nung.
Cc mui khng bn nh= KSs, KNO ...sau khi ti kt tnh nhiu ln trong n-c (khng
=c nng qu 60C), cn sy kh trong khng kh nhit phng. Mt s mui khc nh KI,
Nai ...nung trong quyn kh hydro trong ng thch anh 150 180c loi ht du vt ea
phn sot sinh ra trong qu trnh mui tip xc vi khng kh.
Axit H2SO4 v HC hay c dng trong cc o c in ho v nhiu tr- ng hp phi
lm sch tr= c khi dng.
Lm mcmiMCl theo hai cch 0
Cch '1 : Ch- ng hai sn axit H loai tinh khit ho hoc p sut kh quyn trong dng c tu
tinh c cc u ni mi nhm. Axit ten u dng loi dung dch n- 6 37% HCi = e pha long
theo t S 2:1 rs mi h= ng ct. N- c pha ch ln ch-ng u l ra-de ct mt sn, cho,Jn ch-ng
sau S n-e ct hai ln. Mi Sn ch- ng ch! sy on ng- ng gia (on u v on cui khng
ly). st HCl thu - c sau has ln ch- ng Sa So sch thnh phn HCI.335H20. Bo qun
axil ny trong cc ng thu tinh hn Scn u.
Cch 2 : Hoa tan kh HCl sch vo m= c sch n nng yu cu. Kh HCS sch - dc
sinh ra bng cch cho axt H2SO4 i ch- ng ct hai ln tc dng v KCS i qua ti kt inh v nung.
Lm m m rMOt bng cch ch- ng ct hai ln p sut 5 - 1 0 mmH0. on 2 ca
ln ch- n@ ct th hai cho dung dich H2SO4 06%. Bo qum trong ng thu tinh hn kn.
iit H2SO4 - c lm sch oh- vy vn cn chfe tfp cht hOu Cd lm nh h- ng n cc
kt qu o se nghin C- v ng hoc v hp phu. vs th cc dung dsch H28O4 'tr- khi dng
cn phi lim 8f ch thm bng cch in phftn tr- c nh- ii ni 2.2.2. Khng - o lm sch
H2SO4 bng than hot tnh v chng s tc dng ho hc sin nhau. .
/ .

Jk IIM jflwi Si sch khf


Phn ln ee o tf c in ho phs tin hnh trong iu kin khng c mt ca xy khng
kh, v n ht 1011 in ho5 m sai lch kt qu . Ch nn cc th nghim phi tin
hnh tong quyn kh trd: nits, argon, hli. Mt s th nghim khc ch php tin hnh tong quyn
hydro. Gc kh ny th ng =c sn xut trong cng nghip VI cc schkhc nhau, Nu hm
s= dng oxy trong cc kh ny khng V- t q 0,005% th c th dng cho nhiu th nghim o c
in ho, nh Big vn phi lm sch ht tp cht h c bng cch cho kh i qua ng cha y
than hot tnh.
Khi hm 1- ng xy trong cc kh tr Sn hn con s trn th nht thit phi loi b bt bng
cch cho kh tr i qua ng thch anh di 80-100 cm, cha y xc tc, nung nng. Nu xc
tc S phoi ng = phi nung nng n 450 - 500c , nu xc tc S bt ng mn kt bm trn
sicagel hay trn t st = phi nung n 200 - 220c. Ngy nay c bi xc tc mi cho php
lm vic ngay nhit phng nh- P Chang hn, oh= sg khi ti sinh vn phi nung nng.
Hydro c th t iu ch ly trong phng th nghim bng cch in phn dung dch
NaOH 25% hay KOH 20%. Cc dung dch ny tr- c tin phi loi ht tp cht eacbooat bng
cch kt t chng nh Ba(OH)a. Sau khi lng gn v Soi b kt ta BaCOs, dung dch -c - a
vo b <n phn -dng t nh- hnh 2.16. Bnh in phn hinh h& u bng thu tSnh 40 - 50
ram. in cc bng S hay dy Ni. Mt dng in trn in cc 20 - 3 m/cm2. Din tch in
cc chn sao cho c th thng qua bnh 1,5 - 2,5 A. Oxy gii phng ti anot, qua van thu
phong 3 x ra ngoi tri.
Hai khoang a not v catot khng ngn cch gim in tr trong ca bnh nh- ng nh- th
oxy anot c th khuch tn sang bn catot v ln vo kh hydro. V vy phi kh b tp oxy
bng cch cho qua ng 6 cha xc tc. ng ny C0 th un nng tu theo tng loi xc tc .
cn phi sy kh hydro trong ct 7 tr- c khi - a vo l xc tc 6. sy kh bng CaCI 2 sch
nung tr- e. CaCI2 phi dng lai cc nh kh hydro i qua d dng v - c sy kh tt nht.
Khng nn dung loi bt nh, d b tc.

Hnh 2.16. Bnh in phn iu c hydro.


1 - dung dch din phn; 2 - in cc Ni; 3 - van tho phong; 4 - ng ra; 5 - ca np dung dch; 6 - l xc tc; 7 - ng cha CGa sy
kh Ha; 8 - bu thu tinh trnh dung dch ra pht ng- c vo l 6.
Ch tfo xc tc Pd nh sau: hn hp gm 20 th tch dung dch PdCla bo ho trong
n=c 4-15 th tch formalin 30%, tm vo amian sch, mn. Lm sch amian bng cch nghin
amian, ngm trong kim, ra sch. Aman tm xong, lm lnh bng n- c v cho thm tng
git dung dch NaOH c cho n khi -t m amian.'Khi trn b mt si arnian -c bm
dnh cc ht PdO mn mi sinh. Ra cn thn cho ht formalin v ion do trong n-c ra. sy kh
150c trong t sy, kh chng trong quyn hydro 400 - 500c trong 4 - 5 h lin s - c XC
tc Pd kim loi trn b mt chng.
Kh thi lung kh hydro t bnh in phn qua xuc tc Pd, oxy (tp) s tc dng vi
hydro thnh H20 dng hi v s ng- ng t trn thnh ng u ra ca S 6. u ra ca ng
phi nghing xung n- c ng- ng khng chy ng- c vo l 6.. Sau kh hydro cn phi ra
trong cc ng 4. Cc ng ny c ng knh G 15 mm xon rut g c nghing ging
nhau bt nh kh hydro i qua khng hp li thnh bt ln . u vo ng sa 4 c mt
mao qun th! hydro thnh cc bt nh. u ra ca ng ra 4 c ming 5 np dung
dch ra vo bng ng bm.
Dung dch ra S matri plombit 20% nhm Soi ht tp cht cha s ra khi kh hydro. Tp
cht ny <Sr sinh ra nu amian ch- a lm sch ht s. Ch dung dch natri ptombit nh sau
:dung dch mui chi (nh- Pb(NOs)2 hay Pb(CH3CQ);i) thm n d MaQKI c kt t ch
oxlt, ra k trn giy lc, ho tan k t bng MaOH 20% vi th tch tnllt ton sao cho dung dch
thu = e c cha 8 - 10% PbO.
Kh hydro sau khi ra en cho qua ng cha bng thu tinh (hnh 2.16 khng v) gi li
cc git nh dung dch ra bi cun theo. Khi dng cho th nghim c chnh xc rao kh hydro cn
phi lm sch thm bng raito long ng bng. u CUS thit bi S np nhm v van nhm. Khi
binh Sn phn khng Sm vic phi ng van khng kh khng St vo h. Kh hydro sinh ra v
i qua h - c l nh p sut thu inh, biu thi bng chnh Sch a hai ct dung dch trong hai
nhnh ch u Ga binh Sm phm.
iu ch xy c th vn dng 'thit bi nh~ hinh 2.16 ch! cn thay i vl Sm:
i chiu dng in vo hai cc;
Thay dung dch ra bng dung ch SCR4n04 mi tr- n kim oxy ho hp ht s sn
trong so phm.
Vn hnh thit bi Sn phin ny cn 'tun th cht chi ee srn sau :
Tr- (Sc kh cho my chy tn kim tra fi ni ng cc vi ngun in ch~a. Mi ng= e cc
t xy ra n nu P= c thit bi = c s dung ng.
L xc tc ch! ni VS h thit b| khi ton b h i thong kh hydro v ui ht khng kh. Mu
thit bi Sm vic th- dng xuyn thi hng ngy sau khi ngng Sm vic phi kho Sty u CUI
ca ht b Khi Sm vic lai phi 8ho S 6 ra , thi kh hydro 3 pht ri mi Sp l 6 vo h.
Tr= ng hp h cha y khng kh do thay dung dch, site cha ...phi thi hydro 4 5 h r
mi ni S 6 vo h.
o Khi cn sa cha thit b phi ui ht hydro kh h bng cch thi nltd qua h 5 = 6 h, sau
mi tho, lp, sa cha, o Khi binh in phn lm vic hai cc phi lun ngp trong dung
dch. Khi p sut kh hydro bn catot ln, mc dung dch h thp, in cc Ni b h khi
dung dch (do ng van cui h) th khi hai bn cc c th lt sang nhau v c ngu c gy
n7 nht l khi dng in th Sn gite hai cc. VI vy ch nn dung in th- gia haS .cc
12 - 24 V l ti a.
in phn Su dung dch s cn dn do 0= c b in phn v bc hi, tn
phi dfnh k- b sung n~ c ct hai ln vo. i vi thst b c np nhm trn ming ch u
phi nh k m np v bi tron bng m chn khng phn d ca n trnh kim ng
kt cht khng m -c na.
Uo Vl iw h t @iei!p
Vt liu in cc dng trong in ho th- ng l kim loi, hp kim, oxit kim loi, grafit,
cacbua, sunfua, nitrua ...chng l cc vt liu dn in t. Thng dng nht l cc in cc bng
kim loi c sch cao.
sch ca cc kim loi dng lm in cc ti thiu phi l 99,9% tc tp cht cho php
ti a l 10_1 %. Loi sch nht ch cha tp cht ti a l no-10 %.
Trong in ho hay dng thu ngn lm in cc, v vy cn phi bit cch lm sch n
cng nh- cc bin php an ton khi lm vic vi thu ngn. Hg dng cho th nghim vn c mt t
tp cht c hc v ho hc, nht l Hg qua s dng. Sau y l mt s pch lm sch Hg :
Lm sch fotp ch c hc cho Hg
Hg vo bn thu tinh v dy
Ra nhiu ln bng n- c, gn ht n- c v thm kh b mt Hg bng giy lc
Lc Hg vo bnh kh, ^ch bng giy lc chuyn dng, nhn, c nhiu l to.
Lm sch tap chho hc choHg Tp cht
ho hc ch yu i cc kim loi.
150 - 200 ml Hg vo bnh hai c dy
Rt thm 200 - 300 ml dung dch Hg2(N03)2 60%. N- c ho tan mui ny phi axit ho bng
HNOa tr- c :l lit H20 + 2 ml HNOa c.
Sc khng kh 18 " 20 h vo lp Hg qua mao qun thu tinh t st y bnh thi sch bi
trong thu ngn.
Hnh 2.17. Ct ra lm sch ho hc cho thu ngn.

4 - cc thu.

1 - phu, u mt c 0,5 -1 nrai; 2 - ng thu tinh c 15 - 20 mm, di 1 m; 3 - mao qun c >

2 - 3 mm, cho 60 - 80ml Hg vo tr-dc, ri cho dung dch vo


Chuyn tt c sang phu chit v chit ly Hg vo bnh kh, sch, o Ln l-t nho tng git Hg lin
tip qua cc ct ra bng n-c ct hai ln, bng H2SQ4 c, bng n-c ct hal ln, bng dung dch
HgaCNQsa 5% (trong
ba ct), cui cng l bng n- ct hai ln. Cc ct a ging nhay v kch th c v cch vn
hnh nh trnh by hnh 2.17.
i vi cc th nghim nghin cu trn cc qu trnh in cc tnh (git tflso) cn phi sy tlp
Hg trong chn khng ri mi dng.
BS in m ng Mss Sm m wi IHg
Hg rt c, nht l hi ca n. Nng hi Hg trong khng kh tng ln khi lm Hg,
chng v thnh nhiu glot nho, be mt bay hei s tng ln. Vi vy khi
s dng Hg phi dng cc dng c, thit b| dy bm, chc chn, t b h- hng , v. Cc thit b c
dng n Hg phi t trong phng iu ho nhit <% trong t ht, v Sun t trn khay hng
phng khi v. Khay hhg nn lm bng cht do cng vng". Khi rt Hg vo dng c, thit b
phi tin hnh trn bn c bit, c gd chan Hg V tng vi khng bn xung sn, hoc phi tin
hnh trn khay c bit. Phu phi dng loi c cung vut nh thnh mao qun hay dng c
chuyn dng.
Khi Hg b| vii on thu gom ngay. u tin dng ng ht nh hnh 2.18 ht gom Hg trn bn,
trn thit b|, trn sn. Cc ht Hg nb s Sch nhn thy phi dng cc tm kim loai'nh- ng, km, st
% r qut thu gom chng. Lc cc giot thu ngn si bm dnh ln Sclm toi chng t
thnh hn hng . Gt cc hn hng lng vo chu IV G, CUI cung cc tm kim Soi cng phi
bo qun ring trong ro= o. Sau C0 ra, lau chi bn, thit b, sn nh bng giy hay bng m
ri gi giy hay bng trong Hg ri ra v t gom xung y chu. Cui cung nhng ch nhim
Hg cn phi x l bng dung idh FCl3 20%, c 10 ro2 b mt phi dng 10 lt dung dfch ny,
qua 1 ngy rn roi mi ra Sf dh iai bng ri c.
Hnh 2.18. ^ng gom thu ngn red vi.
I - bng cao
su; 2 - ng thy
tinh; 3 - ming 1
ht thu ngn
ri vi.

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.

Thung ta ghi dng i theo in th 9 (Hnh3.2)


Vi qu trnh thun nghsch ta c :
1. Dng cc i catot i P.C (|oA/cm2) :
I P.C = - 2,69.1 O^Do^CoV1
trong n = s in t trao i
Do - h s khuch tn, cm2/s
Co - nng ban u ca cht o , rnol/l
rt.
vci
\ Ci
A) -- .k
(VG
W( . ti

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 ; }'

- - Cho bit qu trnh c thun nghch hay khng.


- Tnh h s khuch tn D
it 4 lc t
MittSkO^k
tu
401)1) Mil
OjO'i p
0.} O'- -\|> ^ t
tt
UP,ftcra
vi' vrottv 4 ok
: . i f t -i cht : use (ti SWJ2
' p !
0
1t . p
. . ^ Bt
PHN cc NNG
2J fJiMrg
Khi qu trnh in ee xy ra th nng cht phm hg st b mt in cc gim
xung (hnh 3-4) dn ti phn c nng :
q> = (RT/nF) lnC/Co
* (RT/nF) ta(14f)
trong :
A<p i phn c nng ;
cs C l nng cht phn hg ti b mt in cc v trong dung fch; i,
Qh l mt dng khuch tn v dng gii hn : u = - nF(D/S) Co*
5 l chiu dy lp khuch tn; - D l h s khuch tn.

2olo @M <Ms CuS4 cc nng 0,1N; 0S2N; 0.5N; 1 N


+ H2SO4 50 g/l
1JL S( i i: hnh 3.S :
Cu
1 - in cc nghin cu (W); 2 - in cc i (C); 3 - in cc so snh (R) ;
4 - Von mt in t c R > 107 Q; 5 - Bnh trung gian cha KQ bo ho ; 6 - Cu
v mao qun cha KQ bo ho; 7 - s xp ; 8 - Ngun in mt chiu; 9 - Miliampe mt mt
chiu; 10 - Bin tr; 11 Bnh o.
2.4. Trnh tth nghim :
2.4.1. Np dung dch vo bnh o
2.4.2. Cho ln lt cc mt dng (mA/cm2) = 0,1; 0,2; 0,3; 0,4; 0,5; 0,6; 0,7; 0,8; i,0; 1,2;
1,5... i qua h.
2.4.3. o sc in ng E bng von mt in t 4. Tnh <p theo cng thc:
<p = cpcalomel - E
E l gi tr o - c trn von mt in t.
2.4.4. V -ng cong phn cc (hnh 3.6); /
2.4.5. Tm igh theo - ng cong phn cc (hnh 3.6);
2.4.6. Tnh chiu dy lp khuch tn 5 ng vi cc nng cho.
Cho bit D = 10-5 cm2/s;
2.4.7. V th igh = f(C) ln hnh 3.7.
igh , .N
mA/cm2
Vl
c, N
Hnh 3.7
Gh th Gh : Sau mi ln o phi ty
sch lp ng bm trn catot (in
cc
nghin cu) bng dung dch HNOs
10%. Sau ra sch bng rs-c
my3 trng ii bng n- c ct ri tip
Cu "fowl
/ j)Aut (Lekrt: Hnh 3. V
y <iV\> f|
(c vvt hC karti' ft
. I
-l- j u

(,
% 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.

Hnh 3.8. - ag cong phn cc potentostatc

Nh c in cc quay m dng i s= u C ng hc to ra mt profln nng ngay


lp dung dch sat b mt in cue. Mt dng in i c inh tb0 ph g trinh :
i = n FD(Co Cs).S _1 (2)
trong Co-' nng ion tham gia phn hg in cc trong dung dch;
c 8 = nng i0 tham gia phn fihg in cc b mt in cc; s - Chiu
dy 8p khuch tn Nemst
Chiu dy lp khuch tn 5 l hm s ca tc quay co ca in cc. 8 c tnh ton
cho tng tr- ng hp trong nhng iu kin thu ng c th. i vi tr- ng hp in cc a
quay, 8 - c tnh theo ph- ng trnh Levie :
8 = 1,61 (D/v)1/3 (v/fi))1/2 (3)
trong V - nht ng hc <D = 2nf - tc gc f - tn s.
Trong tr-ng hp mt dng in gii hn khuch tn (tc khi Cs = 0), kt hp ph-
ng trnh (2) vi (3) s - c ph- ng trnh Livie (4):
id = 0,62 f CL v1/6 D2/3<a1 (4).
>
Trong id - mt dng McffnL' uA/cm2 F - s
Faraday - 96486. (up QA s/mol.
CL - nng cu t trong lng dung dch,
mol/cm3, V - nht ng hc, (cm^s C -
tc quy in cc, vng/s
Ph- ng trnh Levie (4) c th cho bit s ph thuc ca dng khuch tn id vo tc
quay in cc co v nng trong th tch dung dch CL .
33o Thc nghim, nh gi kt qu :
Kho st qu trnh oxy ho ca cu t trong dung dch nn (0,1 ..1mol/).
Nng ea h oxy ho - kh Co * 10~3 ...to-2 moS/l.
n cc nghin cu w: in cc vng,
in cc i c : in cc patn dy,
in cc so snh R: in cc calomel bo ho.
Tih hnh & :
h trng thi n nh khong 20 ph, o in th on nh cpR.
. Bt u t in th ft m hn fR khong 100 mV, ly ng cong phn cc anot.
Cui cng mt in th khng i f2 nm trong vng khuh tn gii hn, xc inh quan h
ca id v cn bc hai tc quay (oam) ca in cc v th hin bng th id - 1/2. nh gl
theo ph ng trnh (4).
Lp bng s cc gi tri f, in, id,
Sau kh nh gi, tnh D.
Gi t V s cho bit trong khi im th nghim.

B

FHUtJNG PHP TNG m SN HO


41. ii cb:
Lm quen vi ph- ng php ph tng tr in ho EIS ( Electrochemistry Impedance
Spectroscopy)
Bu th cc c tr- ng n mn Fe trong dung dch axit qua ph tng tr.
41. < s 0 thuyt:
Khi p mt th xoay chiu U(T) G tin s nh ro in cc s xut hin mt p hg 3 dng
xoay chiu S(t).
Ph ong trnh hiu in din th xoay chiu :
u(t) = Um sln{e>T > fm)
V biu din dmg xoay chiu :
I(t) - L sncttT - fi)
Trong Um 3 im 8 hin ; - 2x S tn s gc ; S tin s Hz; <p S 0C pha; t fi thi
gian.
Gia th v dng ch! sai khc nhau v ln Ga hin t v lch pha <p gla chmg
{ f> f)U f>i ).
Tnh cht in h@ ca h Bn Qtf/ung th <fro nghin cu qua mt bnh o
in ho thch hp.
tt e cc thng s quan trong (v d nh= nng Son trong dung deh 3 tnh cht in
mi ca cc mng ph hay mng th ng5 Sp kp cung nh= cc qu trnh chuyn in tch v
khuch tn) u biu th qu tng 'tr z v gc pha f>. T gi t o tng tr Z th Mt = c
tnh cht ca b mt in jq c th rt ra_ec ktlan v~cgchv nglc~a!phn-
AgW^c^rh~cc tc n mn.
Cc ph dng trnh tng rd ca h in ho Schng phi S h ph dn trinh n thun nh-
trong k thut in mt chiu . gii trc tip chng ni chung rt phc tp cho nin phi s
dng php bsn i Laplace, 2 hm ph thuc thi gian =o chuyn thnh ph thuc tm
s. T-og quan glfe th v dng cho bit gi tr tng tr ph thuc tn s Z(jffl):
2(1) = (Un/y.xpEHc^- qx) s Z ^ = z 4 j r
|Z - V(Z f + i\Tf
r * I z . cSf ; T = |Z|.sinf
Trong j = V - 1 n v o;
I z I = l gi tr tng tr
Z , Z l phn thc v phn o ca tnc tr.
Quan h gia Z v Z - c th hin trn mt phang Gaus (hnh 3.9) mi tan s c
mt tng tr t- ng ng - c ghi li v sau khi thay i nhiu ln tn s ca tn hiu xoay chiu
s thu - c mt ph tng tr. Ph ny c th biu din d- i dng ph Nyqust hay ph Bode.
Trn ph Nyquist, trc honh l Z - phn thc, cn trc tung l Z - phn o ca tng tr
Z, chng thay i theo tn s D (hnh 3.1 Oa).
Trn ph Bode th hin s thay i ca logarit tng tr z I v gc pha <p theo logarit ca
tn s co (hnh 3.1 Ob).
Ph tng tr cho bit c v s l drag lan cht-- dog cc thng tin, s liu Gg ch vlTdna
hc phan .ng cu trc b mt in cc. T cc gi t ca cc thnh phn nt> in tr R, in
dung c v ccthong^ khuch tn ...c th vch r cc gf thit v chng mt cch nh i- ng
hn. S sai khc gia cc s liu o & c v cc s liu t S t~ ng - ng m phng
(simulation) s cho bit tin cy ca php simulation. Sai s cng nh chng t s t- ng -
ng m ta m phng cng st vi thc t xy ra trong bnh o in ho.
Cc phn t quan trng nht c mt trong s t- ng ng v cu thnh tng tr " c
ch ra bng sau :
i im m> h -
49
Phn t K hiu Th hin trog t& tr
Bin tr R R
in dung . CjffiC)-1
ln cm L jooL
Warburg Zw KwiCf)^5 (a)
Hng s pha CPE Sr
Trong (a) Kw = RT/ Z2F2C0D1/2 Co ~ nng ca cu t
khudh tn D hng s khuch tn
(b) 0,5 < a < 1,0
R fth= ng biu thi in tr m ca mng ph, in tr chuyn in tch, in tr phn cc
ca qu trnh xy ra trn in cc
c in dung c mng ph, in dung lp kp,
L - in em, xut hin ch yu min tn s cao,
Zw gy ra do qu trnh in cc khng ch bi khuch tn ,
CPE (constant phas element) m t, iu chinh in dung khng l t ng gy ra do s
phn b mt dng khng ng u v b mit ktna ng nht
4oS= Nhim
o tng tr ca in tr mu, Sn dung min khi mc rini bit v khi mc ni ip hay ni
song song.
o tng tr c mt din Cc p trong dung dch axil khi c v khng c cht c eh in
mn.
Tnh ton mo bo v c cht c ch.
4.4= Tin htnih D
in Cc lm vc w : st, thp, r
in cc i c : l-lplatin, h,fhM . Harti!erftlT
Bin ce~so snh R : catemeLio-w-(GE)
Bung dch nghin c= : HgSOr-^S-M ftct- I fv
Cht c ch ^---------"'"''' ~
Tn s f
Bin xoay chiu um:
Thi gian o : 5, 15, 30, v 60 ph sau khi nhng in cc.
Th nghim - c tin hnh binh o c sc kh Hz tr= c khi o 30 ph; khng khuy.
in ec nghin cu c mi VI giy nhm c ht 800; ra sch bng 81 c ct;
Sau cnT
Sau khi o trong dung dch H2SO4 khng c cht c ch, thay dung dfeh v o trong
dung dch c cht c ch.
Qu trnh o s dng phn mm E1S v khi x l s liu dung phn mm SM ca hng
Zahner iektrk. Trinh t o s = c ch dn khi lm th nghim.
fe,
4.5. nh gi v tho lun kt qu
Lp s t- ng - ng ca h l in tr mu v in dung mu. Dng Fitting
Program nhn - c gi tr c th ca chng.
Lp s t- ng - ng ca h in cc Fe IH2SO4 . Cc phn t xut hin trong
s t- ng - ng t- ng ng vi cc thng s ca in cc.
Xem xt s thay i theo thi gian ca cc i I- ng khi c v khng c cht c
ch: Rp - in tr phn cc; Cik - in dung lp kp.
Tnh mc bo v s % ca cht c ch
s = 100 (R ,1 - Rp.o) / R ,1 ,
P P %
Trong s l mc bo v hay kh nng bo v, %
Rp.1 l in tr phn cc kh c cht c ch,
Rp.o l in tr phn cc khi khng c cht c ch.
Ch : Sau y l s t- ng - ng ca h in cc Fe IH2SO4 mt cch n
gin , c th dng tham kho. ~~ """
I w>f\
1 \
Rn (in tr dung dich)
Ac.
Cc ph tng tr c th th hin
dng Bode hay dng Nyquist. I IJJ
t Ure
-) Qp = -J-
npM. t

'>' 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

/\

Dng c-th nghim gm hi-nhnh-IA) v (B) =*c ni vi nhau bng phn


nhm (C).
Nhnh (A) - c chia nh, nhnh (B) c tc dng thit lp cn bng p sut kh
hydro thot ra trong nhnh (A).
6.3. Chun b th nghim :
- Mu st th nghim : ct mt ming st c din tch khong 8-10 cm2, sau khi gia cng
sch (nh- bi 5) em i cn - c trng I- ng mi-
- Chun b dung dch v ra dng c th nghim nh- bi 5.
6.4. Tin hnh th nghim :
Sau khi chun b y dung dch nghin cu, mu st v dng c o th tin
hnh nh- sau : y dung dch nghin cu vo nhnh (A) ri cho mu st vo v y ngay
nhnh () bng nhnh (B). Sau dng dng c th nghim li nh- hnh v. Ghi ngay thi
gian (TI) khi cho mu st vo dung dch nhnh (A). Sau khi kh hydro thot ra trong nhnh
(A) y - c dng dch sang nhnh (B) t 3 ml tr ln th dng th nghim. Ghi th tch
hydro thot ra, ly mu st ra v ghl ngay thi gian ngng th nghim (T2) .
Mu st - c ra sch bng n- c th- ng, ri n n- c ct, lau kh, lau li bng r-
u hoc axeton v em i cn - c gi tri (m2).
6.5. Cc s liu thu c:
" gim trng - ng mu st Am = mi m2 (g)
Th tch kh hydro thot ra V (ml)
- Din tch mu th nghim S (cm2)
- Thi gian th nghim x = ta - Tt (h)
Da vo cc s liu th nghim thu - c tnh tc n mn
- Theo ph ng php trng l ng, tc n mn Kg bng :
Kg m s A T g/cm2h
- Theo ph- ng php th tch tc n mn K bng :
Kv = AV/S.AT ml/cm2h
Hoc chuyn sang th nguyn trng I- ng th:
Ko = 28 Kr/12000 g/cmh 28
S - ng I- ng gam ca st (g)
12 000 cm3 l th tch ca 1 gam kh hydro nhit v p sut bnh th= ng. Hoc
chuyn qua n v in :
Ki = Kg.26,8 / 28 A/cm3
26,8 : s Faraday (l din I" ng cn thit ho tan 1 ng S- ng gam km lo), Ah.
Nhng kt qu n st ra:
a. Tc n mn ca st trong dung dch H2SO41N c xc nh bng ph- ng php
trng S- ng v ph- dng php th tch.
b. So snh tc n mn ca st trong cc dung dch trn - c xc nh qua 3
ph-ng php (ph-ng php in ho, ph~ ng php trng l-nga ph-ng php th tch).
c. Kh nng c th xy ra sai s ca cc ph- dng php xc nh tc n mn trn.
BS
STH NG CA HM LO I
7.1o Mue i l %
o Nghin cu hin b dng th ng ea h Km lo ung ch thng qua h Fe trong cc
dung dch khc nhau lam v d.
o Lm quen vi dng dng cong phn cc cng mS> cc trng thi c tr- ng ca h Kim So
i t ng /dung dch .
?o2 s 8 thuyt:
Nhiu kim loi v hp kim (trong c F v hp kisn ca F) b th ng trong cc
iu kin thch hp v c og dng cong phn cc rt c tr= ng , d nhn bit. Bt u
in th n mn, cho tng in th din cc v pha d ng thi mt dng in cng s 'tng
thao trong giai on u tin, kh n mt gi tr in th no th mt dng bt u gim
v in n gi tri rt nh (mt vai mA/cm2), khi Sm the t n in th phng din ea thi
dng 3fS ting Sn. - ng cong phn cc ca kim toi th dng = c m t trn hnh 3.13.
Mt iz thot H otam thu ng
dng in >...... .. boat tnh -. . . .-. gu th ng
2
(m/cm ) %- .-.
-5^ .
0
3#^
7
Tm
fT +<p, V

Hnh 3.13. - d&g cong phn cc potendostatc ca kim loi b th ng.

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

Ch : pH cc dung fch l 3,5.


hSht phng (xm v ghi If I)
Mt ng n eatot 2 /drn2.
Thi gian ti0 phn 20 pht.
& Sm (>&n) Hnh 3.14:
u

Hnh 3.14: S in phn


u Ngun in mt chiu, N B ng ngt in, R in tr iu
chnh, mA miliampe k, - Cc bnh in phn.

B1, B2S B3a B4 - Bn bmh in phn mc ni tip, c anot bng km v cato c


bng thp c in tch gn bng nhau, v ghi y s liu vo bng 1.
Cato tr= c khi in phn phi iy sch du m trong kim, hot ho b mt trong
axit nh mi th nghim khc.
Rt dung dch 1 vo bnh B1, dung dch 2 vo B2, dung dch 3voB3,
dung dch 4 vo B4, sao cho catot ngp su bng nhau trong cc bnh.
Ni in v iu chnh cc in tr R - c dng in trn mA t gi tr mong
mun. Gi tr ny phi tnh tr- c da trn phn din tch thc t b ngp trong dung dch
ca catot v mt dng in Dc cho (2 A/dm 2). Ghi thi gian bt u ni in v in
phn trong 20 pht Ngt in, ly 4 cato ra, ra sch d- i vi n- c, sy kh. nh gi
hnh thc v cht I- ng kt ta theo cc mc:
- Nhn mt v soi knh hin vi xem lp kt ta sng hay ti, nhn hay sn si, tinh th mn
hay th, gai, cy.
- Un catot 90 (bn knh un 4 mm) quanh trc thp c () 8 mm ri quan st :
lp ph c b rn, nt, bong ... nh- th no. Ghi kt qu vo bng 1
Bng 1 s liu v kt qu th*?ghrn i nhit :...
Catot Dung dch De, ' Din tch Dng in, Nhn xt
s s A/dm2 catot, mA Thi gian in
dm2 phn, ph
1 1 2
2 2 2
3 3 2
4 4 2
Phn hai: o - ng cong phn cc - I ln I t cho 4 dung d ch trn nh b nh o in ho
ba cc v my t nh in t c phn mn
t-ngthch.
Bnh o in ho 3 cc: cc Sm vic w bng Pt (cn bit din tch ca n), in cc
i c bng dy Pt, in cc so snh R l in cc calomel, c gi tr
in th coi nh khng i fcaiomei = 0,244V.

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.

Bi ny chn nhm AI lm th nghim. AI c in th rt m <p = -. 1,67


V nn rt hot ng, trong khng kh hay trong dung dch oxy ho trn mt AI lun sinh ra
mng oxit AI2O3 hay AI2O3.H2O mng c 4 - 5 nm. c mng pha oxit dy c vi chc
n vi trm pm phi oxy ho anot cho b mt nhm.
Dung dch oxy ho anot nhm c hai loi:
1" Loi dung dch oxy ho khng ho tan mng oxit, cho mng kn, st, khng l
xp, khng dn in, mng rt mng cch in tt, th- ng dng trong ch to t in
hay trong k thut in v in t. Cc dung dch ny th- ng l axit yu nh- axit boric, axit
tartaric, axt citric ... Chiu dy 5 ca mng t l vi in th E (V) catrinh in phn : =
aE
trong a - h s t l, bng 1,4.10'7cmA/
2- Loi dung dch oxy ho c ho tan mng oxt, cho mng c nhiu s xp, mng
dy (1 - 500pm). Cc dung dch ny th-ng l axit cromic, axit photphorie, axit oxalic, v
thng dng nht l axit sunfuric...
9.2. Qu tr nh h an@t nhm trong H2S04 Phn hg
tng ca qu trinh oxy ho ano i l :
2Ai "8= 3H2O > S2O3 + 6H* + 6e Khi thng dng in qua
h, trn bin gii kim lo - dung d ch u tin to thnh lp mng mng barie kn, st, c
chiu dy trong gii hn 0,01 0,1 pm. in phn tip lp ny cng khng dy thnn ln =
c, bi v mt ngoi ca n b
ho tan cc b v bin thnh mng xp :
203 + 6H* - 2AS3* + 3H20
Mng xp c dy dn tn theo thi gian in phn, cn mng kn barie vn
gi nguyn chiu dy ni trn (hnh 3.16)
9.3. T nh cht mng oxit
Mng AI2O3 xp, hp ph tt, d b hydrat h. VI vy tng kh nng b v ho
mng c th x S trong hi n- c hay n- c mng hyrat ho MA, bt kn l xp, hay x
S trong dung dch cht c ch n mn nh- crmat hoc tm du vo l xp. Nh tnh hp
ph ca s xp m c th nhum mu cho mang tng tnh trang sc cho nhm.
Mng S2O3 gn bm tt vi mn AI, n hi km, rm nt khi un, gp
mu.
io tr mng AS2Qs rt Sn, nm dim th dng ch qu trinh xy ho Mh ca,
fh ng > 12 V, v c th dng A2O3 mh= mt mng cch dim.
@A K]i h, cdMuDfj 3
v hl )
1,5 Si 3
sl 3
o
m)j&8m inm
Dung dch H2SO4 200 g/s Bnh
in phn (cc) 2S0 m Miu
nhm 40x50 mm
htm hay tetradoruacacboir)
hay xng,5 Sit ng h amp

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.

C(Wn2* ( Vi. .Ci a.c a ) / v .


Vi
- th tch dung dch EDT, mi
v2- - th tch dung dch Zn2+ . ml
th tch uog dich Mn2* . ml
Ci - nng dung dch EDTA, mo/l
Ca - nngdung dch Zn2\ mol/l.

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 :

Hnh 3.18. S in phn ch to Mn2 ! bnh in phn; 2 -


mot titan; 3 - catot ch hay grafte 4 - von mt;
5 - ampemet; 6 - bin tr; 7 - ngun mt chiu; 8 - culong met.
Thi gian 1 h 3 h
Tr= ng hp in phn nhit cao, bnh in phn 1 - c t trong my iu
nhit.
Trong qu trnh in phn, c 20 pht o in th mt sn . Th nghim ch 2 nhit
cao nn n c bc hi nhiu, cn ch b sung thm n- c ct.
Sau mt thi gian in phn 1 h ch 1 , sn phm nm trong bc anot - c
mang ra nhanh bng n- c , sau ra trong n= c ct n khi ch Ca 2 vo n- c
khng thy mu sa, mang sy sn phm 60c, cn sn phm.
ch 2, kt ta bm cht trn anot Mang anot i ra, sy, co MnOa, mang MnOa
i cn. Cng c th cn in cc tr- c v sau in phn tnh s= ng Mn02 kt ta.
Trong c hai tr- ng hp, phn tch nng MnS3 cn li sau qu trnh in phn
1.S. Yu eM b&@ e V G* ton
- GII thiu ngn l thuyt iu ch Mn02;
- S . th nghim v m t cng vic;
- Bng s liu thc nghim;
Bng s liu thc nghim

Hiu sut dng in (H) - c tnh tho cng thc:

- Tnh hiu sut dng in v hiu s nng MnS04 u v sui in phn;


- So snh kt qu v sn phm ca hai ch in phn;
- M t s thay i in th theo thi giam.
H " lOOei.h/ 2.mi , %
1, S2 = = ng S- ng irs ho sa Cu v M0O2
m* - khi l= dng Cu kt ta trn oatot ca cuSong met no
m2 = khi S ng ft/lnOa kt ta trn anot binh in phn.
Bi 11
SPH THUC CA HIU sr DNG EN
HYPOCLORIT V CLORAT VO THI GIAN DN PHN
11.1. C SI thuyt
Ph- ng php in ho sn xut NaCIO v NaCI3 da trn nguyn tc in phn
dung dch NaCI trong thng in phn khng c mng ngn.
Trn catot hydro phng in: 2H+ + 2e - H2 (1)
Trn anot ion Ch phng in : 2 Ch - 2e Cl2 (2)
Phn t do ho tan trong n- c b thu phn thnhaxit kh phn ly HCIO :
c2 + H'20 4 HCIO + HCI (3)
Khi trong thng in phn to thnh OH~ th HCIO s b trung ho :
HCIO + OH- CIO- + H2'O (4)
Bi vy ngoi ion Ch v OH, trong dung dch cn xut hin ion CIO - o So snh in
th phng in ca CIO - v Ch thy rng : nu trong dung dch c nng CIO - - ng
i ln, n s = u tin phng in :
6 CIO - + 3H20 - e - 2C03- + H* + 4Ch + 3/2 Oa (5) lon dorat to thnh ng thi vi
s thot oxy. Giai on u oxy thot ra t, nng CIO - rt nh v s phng in ca ion
CIO - hu nh- khng xy ra. Dn dn nng CIO - tng dn ln, chng phng in cng
vi oxy thot ra theo ph ng trnh (5). Cui cng nng CIO - t n mt gi tri cn
bng no

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.

m ti yB- ng CIO - sinh ra bng 1= ng cso - phng in, S nng


hypoclort n nh.
A rS h- ng ca thi gian n s to thnh hypocorit v corat natr v oxy - c -
a r a hlnh 3.1 8 (-ng Vetter)."
trng hi n nh hiu sut dng in cc i theo oxy hot tnh l 66,67%, cn
tiu tn in th thot oxy S 33,3%. T" dng quan ch ng khi trn anot ch c qu trnh
(2) v (3) xy ra v khng mt qu trnh no khc nh h- ng n nng n nh e
hpocSorii
Ngoi con = ng in ho, clorat cn = to thnh theo con & ng ho
hc:
Cl~ + 2HCSO - CIOs- + 2H* + 2CS- ' (6)
Hiu sut dng in dora cao vl c phn ng (6) xy ra, bi vl hiu sut dng
in cc i to thnh ciorat theo con - ng in ho ch! t - c 67,7%.
Hiu sut dng in to thnh hypodort v clora cn ph thuc vo nhiu yu
t nb- : nng dng 'dch, mt dng in ano, nhit dung ch, bn cht in
cc... (xem gio trnh).
C cc phn tog ph nh hog n hiu sut dng in to thnh hypociorit v
dorat:
-CIO - v CIOs' bi kh atot bi hydro
CIO- * 2H CS" 4- HsO (7)
CIOs- * 8H -> ;Ot -fr 3H20 (8)
naftn nga phn tog ph ny nghB ta ch vo ung'ch 0,2% SCCrOa.
Chnh s to thnh clorat bng con = ng ho hc theo (6) cng lm gSm
hiu sut dng din ca hypodorii
- Oxy phng in trn anot:
4H- - 4 -> Ga HV 2H2O (9)
Khi h nghim, giai oan cui cho thm mt 8= ng HCS mnh th mt phm
cso - si chuyn thnh HC1 :
CIO- + MCI -> HCiO Q- (10)
S xut hin mt Sdng mi HCSO lm tng ng qu trnh h hc t
thnh clorat Nng CIO - gim nn s t thnh clorat theo con " ng in ho nn
O2 t thot ra.
11.2= Mae i h Sh nghim
Bng con -drsg thc nghim nghin cu qu trnh xy ra khi in phn dung
dch NaCI iu ch NaCIOv NaCIOs kho st s thay oi nng (v hiu sut dng
in) a sn phm theo thi gian.
Ill Tin hnh th nghim.
fill hui b ung (S : Dng sv c ct v mui tinh pha dung dch NaCS c
nng 270 g/l v Na2Cr4. .
. Bts phn: in phn nhit th-mg, mt dng in 500
A/dm2. Trong binh in phn treo mt anot grafit v hai catt thp hai bn. Sd
in phn nh= hnh 3.18. Tin hnh in phn trong 4h. C 30 ph mt sn in
th thng v phn tch nong NaCIO v MCls, ghi cc kt qua vo bng sau : '
- .
Thi in L-ng phn Nng , g/l Hiu sut, % Ghi ch
gian, the, tch,
h V ml CIO- CIO3- CIO- CIO3-

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* .

Hnh 3.20 (a)

Trn th (a) v (b) chia 3 vng:


1. Vng ng vi iu kin kt ta kim loi dng rn;
2. Vng ng vi iu kin kt ta kim loi dng sa thch;
3. Vng ng v iu kin kt ta kim loi dng bt.
- ng QK biu din dng in chuyn (Dch) ph thuc vo GW*;
- ng OP biu.din dng in gii hn (Bgh) ph thuc vo *&* .
Cng thc xc nh dng in gii hn : Dgt, = c .Co+
K l h s ph thuc vo bn cht ion phng in; Con2* l nng on Cu2+.
12== Chym fe nghim o Chun b s , Sp s
th nghim (theo hnh 1.1) o Chun b hai dung dch in
phn :
Dune dlehl Duro dih 2
CUS04.5H20 20 g/s 30 g/l
H2SO4 50 g/l 50g/f
Th tidh dung dch 1 lit 1 lit
Nhit
ng, trung ho, ra Kt cp h nghim
1 Th t Thinh 1 Nhit , ThM ly- cl|g
th bt 1 Him SB Ma x
phn dung 1 Be, 1 e, giam, f
nghim e 1 Ego ng in,
pt 1 %\
1 m

A/dm2
1 r 1
________ 1_________ 1
Chun b in cc: anot Cu : 40 X 30 X 1(mm)
catot Cu hoc l: 40 X 30 X 1 (mm)
- c khi th nghim ph gia cng sch tu m v mng oxit.
Dng c th nghim : Cc thu tinh loi 500 m v 250 ml
B in cc != i Ft (dng fi phn tch)
Ngu chfnh s= u8 ampe met, in tr con chy
tUo Th Bighim:
12oo1a t t ng (so snh G t. ng kt a ng n catoty
Vi ch De ln S d bng 1; 5; 10 Nm2
Thi gian in phn 15 - 20 ph
HLoo Pm lh ^ h) ft@mg rag Cn chnh xc mt S
ng bt ng mu ti khong 0,5 4. 1 gam, ho tan vo 10 ml HO, gia nhit on 4 " 50c .
Thm 1=2 git HNO3 cho bt ng d tan. Sau ph long dung dich n 50 ml bng n- c
cat
Phn tch s= eg xy cha trong bt ng bng ph= ng php in phn : dng b l= i
Pt ( bit tr= c trng l rsg) tin hnh in phin vi De = 0,2 = 0,3 A/m2 trong khong 10
pht ri thm mt t n=c ct vo dung dch v in phn tip xem ng cn bm ln phn
in cc ml ngp thm hay khng? Nu cn, in phn tip ri li thm n= c v lm si
nh trn cho n khi khng cm ng bm ln in cc. Ra, sy, cn v tnh != mg ng kt
ta ln in cc catot
L-ngbt . Trng 1 -ngcat tPt, g L-ng
Nhn xt bt ng phn Gi Ga Ga G oxy, IOOG02 OOG01
ng em tch, Gbt Gte
r
phn tch g %

G: trng I- ng Ctot Pt sau phi phn tch Ga = G : trng 1-ng ng


B Bski: Nhn xt, gii thch, Ikt lun ca sinh vin.
B 13
IN PHN I CH KM KIM LO ITQUNG
Th nghim iu ch km bng ph- ng php in phn t dung dch sunfat vi in
cc anot ho tan, hoc khng ho tan l mt m hnh thu gn ca sn xut cng nghip.
Ph- ng php ny - c p dng rng ri v rt hp l, thun li v r. N gm cc b- c :
hoa tan qung tinh; tinh ch dung dch v in phn thu km kim loi.
13.1. Ho tan tinh qung km :
Tinh qung km l qung -c lm sch v thiu kt to thnh hp cht km
d tan trong axit sunfuric. Th nghim ny dng tinh qung ch sn.
Cn mt I- ng tinh qung km : 10 hoc 20 gam
Chun b dung dch ho tan : H2SO4 50 g/l
Ho tan tinh qung km vi t l th tch : rn/lng = 1/10-1-14;
Gia nhit n 40 - 50 c. Khuy lin tc.
Thi gian ho tan 30 pht;
Lc; thu - c dung dch cha km v b khng tan:
B khng tan : ra ht axt, sy kh 110 c trong 15 -- 20 ph, ngui, cn, tnh s
% tinh qung ho tan. Ghi vo bng 1.
Dung dch thu - c: o pH, o th tch, phn tch nng on Zn2\ Ghi vo bng 1.
Bng 1 L- ng tinh qung ho tan v dung dch sa ho tan
% 1- ng qung pH dung dch
L= ag rit B khng tan tan, Th cli dung Nng OI
qung ho G , lOOCGi- dch V, ZE2*
tan Gi, g ' I Gl/G, 1 g/1
10
hoc
2

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 :

Hinh 3.22 . S in phn


1 - Ngun in mt chiu; 2 - in 1- ng k; 3 - B in phn
R - Bin tr; V - Yonmet; - ampemet.

Bng 2 : Bng kt qu tM nghim


Nng Zn2+ iu kin in phn
Th trong dung dch, g/
Din tc
t
Tr- c Sau in phn in catot
phn Vd De in th 1 ml A/m2 V c TM gian h dm2
1 1 1
1
1' 1I 1 ___________1___________
Tip bng trn
Km loi km catot, G Nng 1-
Hiu sut ng tiu in 1- ag
Gi Ga 1 1 G = Ga - Gi dng iE th ring thng qna dung
H% kWh/kfe dch A/lit

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.

Kt lun : Nhn xt, gii thch, kt Sun ca sinh vin.


BI14 ^
O KH NJ^NG PHN B CA DNG DCH M^YlN
jV r
14.1. Mcch^ngha
Kh nng phn bo (KNPB) ca dung dch m l mt ch s cho bit dung dch y c
th cho lp m dy u n mc no trn b mt vt m. KNPB ca dung dch ph
thuc yo phn h dng Mnjn catot v vo cch bini nh/h no ca hiu
Sdng Min H theo mt M dngn Dc.
Phn b dtktg in li ph thuc vo tnh cht v mc bin i ca in th catot
A theo mt dng in (tc phn cc catot), vo dn in ca dung dch v vo
cc yu t hnh hc (hnh dng, kch thtc v v tr fcfong i ca cc cc trong b m).
Phn b dng in dic biu th bng t s:
Dg/Dx = k [ 1 - '(<px-g)/Ex ' (1)
Trong D - mt dng in catot
- in tli catot
g,x - ch phn catot gn v xa anot E = DR in th ri trong dung dch
gia anot v catot k = lx/lg t s khong cch gia hai phn catot gn v xa anot, cng
bng k = Rx/Rg t s in tr dung dch ti cc khong cch khc nhau.
Tr-ng hp <px <py = 0 , theo (1) th Dg/x - k = lg , ta c phn b dng in
s cp; n ch ph thuc vo cc thng s hnh hc.
Tr-ng hp x-g >0 th Dg/Dx < k, ta c phn b dng in th cp. Vy
phn b dng in th cp lun ng u hn phn b dng in s
cp, do 06 s can thip ca phn cc (yu t in ho).
. Tc tng qu trnh catot dwbc th hin bng mt dng in catot Dc.
Mhrng ring tc m (hay tc tng trng Kng m lp m) Sl ph thuc vo
c mt dng din Dc v hiu sut dng in H , cho nn phn bMm Q- s phs :
mjmx - Dg.Hg/ Dx.Hx (2)
M bn thn H li cng ph thuc kh phc p vo D (ng bin, nghch bin hay khng i).
V vy phn b kim loi (hay dy ng u ca Sp m) ph thuc ng thi vo rt nhiu
yu t, : hnh dng v kch th- c vt m, cch b tr cc cc trong b m, dn in ca
dung dch, phn cc in cc trong dung dch, cch bin i ca H theo D ...Cho nn khi
thay i mt thnh phn no ca dung dch hay mt ch m no ...s c th nh
htng ng thi n mt hay nhiu'yu t ni trn, lm cho phn b kim loi bin i kh m
Hng fc te.
nh gi mt dung dch c kh nhg phn b(PB) tt hay xu, tc c kh
nng cho phn b kim loi ng u nhiu hay t, ng- i ta dng cng thc:
PB = 100 [k - mg/mx] / k ,% . ' (3)
Theo (3) th PB cng ln khi rrmx > 1 , tc khi m0 5TX . Vy dng dch no
c tr s PB cng ln th c khnng cho lp m dy u mi ni trn catot.
C nhiu cch o kh nng phn b PB , th nghim ny o PB theo ph- ng
php Fild cho hai dung dch m km n v phc.
14.2. Nguyn tic phng php Fild
Dng binh in phn c bit (hnh 3.23) uc ngn thnh 2 khariQ, c mt khe h
pha anot. not t st vch . Hai catot c kch re bng nhay v t va kht trong 2
khoang ea bnh. Ctot X t xa anot gp i so v catot g to ra t s khong cch : k =
Sx/le = 2. Cn ref5c v sau khi m hai catot s bt trng t^ng kim Soi m ln mi catot, t
tnh ra t s mj/sTfe. Ap ng cng thc (3) tnh ra PB. .

catot

Hnh 3.23 Bmh Fild o kh nng phn b

H4Jo H@ Gig vi teg SM Ira M


Chun bi hai dung dch m km thnh phn v ch m nh= sau IMI
dung dh pha i lit. af ttP . ;
Dung |ch s g/i
hnh phn v dh phc
n 12 15
240 - 26
.20 = 25
1
QlnO 5, = 7,5
^ NHTCI f 9
I,_____ Afelnf __ __________________ __________1______ _______________........... . .
HsBOs miMH
Gelatin /fw,km'c
Anot: tm qfe ! pHkh thfce to bng vch A ca binh : 1 ci.
'*'*-* 3,5kht
Catot: bng thp l hay ng l c kch th c va - 4,5
trong cc khoang ca
rln nhm 0 phng
1 phng
1
bnh in phn : 4 ci.
Dung dch ty du m ho hc 1 f OEC 50 g/i : 0,5 = 1 if
Dung dch ty nh cho thp H2SO4 60g/l : '0,51st
Dung dch ty nh cho ng HNO3 1:4 : 0,25 0,5 lit
B ngun mt chiu : chinh t, bin tr, ampemet ...mc thnh s in
phn nt^hsnh 1.1 * tong bnh in phn chinh l bnh Fid ni trn.
Dy in, cp mu, cc hu tinh, th^oc o chiu di, cn phn tch ...
v /
14.4. Tin hnh th I nghim
Lp anot km lm sch vo bnh, cn catot chun b nh- sau :
Ct mu theo kch th- c nh;
Mi nhn mu trn my hoc nh giy nhm;
Ty du m trong dung dch 110 EC 40 - 70c, 5ph;
Ra, quan st nu thy b mt thm rn/c u i ty sch; t khng s tay
vo mu na;
Tay nh 30 s trong cc dung dch Hng ng trn;
Ra sch;
Sy kh;
Cn cc catot trn cn phn tch bit trng l^ng ban u, ghi vo bng 1; o din
tch s m ca catot (tnh mt mt) ri tnh dng in I cn i qua mch (s ch trn
ampemet);
Treo 2 catot 1 v 2 vo v tr X v g nlttt hnh v sao cho k = 2. Rt dung dch m km
n (dung dch 1) vo binh n mc tnh ton tr- c. ng in. iu chnh bin
tr - c dng in I mong mun;
M 1 h; M xong ngt in, ly 2 catot ra, ra sch, thm kh bng giy lc, sy kh,
ngui;
jCn li bit trng ft&Jng sau khi m. Ghi cc kt qu vo bang 1;
Dung phu rt dung dch 1 t bnh in phn vo chai sau dng li. Ra sch bnh
in phn.
Treo 2 catot 3 v 4 vo bnh in phn, rt dung dch phc (dung dch 2) vo ri tip
tuc cng vic nh- lm vi cc catot 1 v 2. , r _ - M
-te m

Ctot Trng mu, g LMmg km kt ta &


1. L Ghi ch
SO
Tr- c m Sau ma Dung dich 1 Dung (ch 2
m
1
2
Lm_________ iO>
3 m
Vt 4 m
MJ L
r r ....................- J

Kt lun gi v cht I"ng lp m, v kh nng phn b PB, v ohnb kim loi ca 2


dung dch ny. fwtc tf t mat
tn CMC m j fmt
Bng 2 : Kt qu h mghim KNPS umg dch m km m v phc.____________
Dung dch Mx .Nhn xt
14< Cm m
- Phn bit KMPB ca dung dch vi phn b dng in v phn b kim lot.
- A nh h~ ng ca mt dng in De n hiu sut dng in H% th- ng xy ra theo
my cch. Cch no lm cho phn b tt hn.
- Kt qu o ca anh ch cho bit dung dch no GO KNPB tt hn9 c phn b kim Soi u
hn? Ti sao ? *
- c kt qu th nghim c chnh xc, trong qu trinh th ogtim phi c bit S- u
nhOhg im no ?

/)
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. __

Bng BiM th (mi m m 20 ph)


Catot s, nghim
t, Dc, Trong 1- ong catot. g H, Nhn xt
cm2 c /m2 Tr-c m Sau m Hiu s %
Sl . 0,2 Phng 10
LK 1 . phng

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

Kt qu th nghim : vi mi pin o 3 ln v ly gi tr trung bnh :


S pin Ln1 .Ln 2 Ln 3
& WF :
A
frOT uf\ tiff

17.1.2. Tr nh t tin hnh o:
Dng mt milivon met c in tr trong ln (r > 10 o) o in th hai u cc ca
pin. in th ny VI mt sai s nht nh c th coi nh- l sut in ng ca pin. Tht vy
E thng th- ng ca pin G 1,5 V . Nu dng milivon mt c in tr trong 10s Q th dng
in I i qua mch o s l :
I = v/r = 1,5/10 = 1,5.10-A (rtnh)
V vy dng in i trong mch o coi nh bng 0 , ngha l :
V o = pin.

17JL B@ iin tr trong ca pin


17.2.1. in tr trong ca pin ph thuc vo nhiu yu t: kch th-c, vt liu ch
to, nhit , pin c hay
mi.
Theo nh lut Om
E ca pin bng :
'E
IR + Sr Trong I - t
dng in i qua ngun R - in tr mch
ngoi, r- in tr trong
F rtb
t
o . t-X CA X
OOA)
c
i)
n
c.
T rt ra r: 1
r = (E- IR)/ (E- )/S
tb
17.2,2. @ @ xem hnh 3.25

,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.

Cho pin phng


in, c 30 pht o mt gi tr I v V.

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

Hnh 3.27. S o dng 1- ng ac quy.


AQ - sc quy cn xc nh ong 1- ng; V - von m; A - arnpe met; R in tr
Ngn th nht phng v dng 1 " 0.5;
Ngn th hai phng vi dng I = 1 A; I 1\
Ngn th ba phng vi dng 8 = 2A.
C sau 15 pht o gi t V v I ca mi ngn ri ghi vo bng sau cho n khi in
th ca mi ngn gim xung n 1 s8 V th ngng phng.
Thi im _ Maim I = 5 A _. ___Nem .I= J LA ... Ngm ;=2........
V 1 I V' I.

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

Ph lc 2 Ty g cho st thp, gang


H 2SO 4 150 - 200 g/l
Urotropin 40-50g/1
Nhit 15 -45c
Thi gian Q10 n kh ht g

m 9

IPSf If 3 li 5i ft} dh in Bc MBE


Thnh phn (g/) v ch ng v hp kim ng Nhm v hp kim nh..
H2SO4 900-920
HNO3 440 - 450
NaQ 5-10 25-35
NaOH 125 -150
Nhit , c 15-30 50-60
Thi gian', pht d- i 10 0,5-1

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"

Pi Ifc Qffiam Sn giffia t rmg (g/m3) v Bung (% irfHBg


IffiOTBg) eia mt s ast v Mm hmg png
Nguyn t H oxy ha kh H oxy ho -kh
T trng, g/cm3 HO HNQs H2SO4 " KOH NaOH
Nhm AI o Al3+ + 3e - 1,66
1,000 0,360
3
0,3296 0,261 0,197 0,159
1,010AI + 6F- o A1F
+
- +3e
2,364. 2,164 1*731 -2,07 1,295 1,04
Bc 1,020Ag <=> Ag + e4,388 3*982 3*241 + 0,7992,38
+ 0,222 + 0,344 1*94
1,030Ag + CT <=> AgQ 6,433 +e 5*784 4*746 + 0,6013*48
+ 0,74 2*84
1,0402Ag + 20H" <=> Ag20 + H20 + 2e
8,490 7,530 6*237 4*58 3,74
1,050Agio + 20H- o10,52
2AgO + H20 + 2e 9,259 7,704 5*66 4,65
1,0602AgO + 20H" o Ag
12,51 2 3 + H 2 0 + 2e
10,97 9*129 6*74 5*56
1,070 14,50 12,65 10,56 7*82 6*47
1,080 16,47 14*31 11,96 *9 7J
1,0902Ct o a2 + 2e
Qo + 1,359
18,43 15*95 13*36 9,96 8J8
1,100 20,39 17,58 14,73 11,03 9*19
1,110a2 + 40H- o 2Q0~
+ 0,40
22,23 + 2H20 + 2e19*19 16,08 12,08 10,10
1,120ao- + 20H- <I> ao2- + H20*79 + 0,66
24*25 20 + 2e 17*43 13,14 11,01
<=> aoj- + H2O ++ 2
1,130ao2- + 20H- 26,20 22*38 18,76 + 0,3314*19 11*92
1,140a2 + 6H20 <=> 28,182a3- +12H 23*94+ lOe 20,13 + 1,4715*22 12,83
a04- + 2H+ +25*48
1,150a3" + BbO o 30*14 2e 21*38 +1,1916*26 13,73
1,160aor + 20H-32,14 o ao4- + H2o + 2e 27*00 22,62 + 0,36 173 14,64
a- + 80H- <x>36,23
1,170 34,18 28*51 23*95 + 0,5618*32 15*54
Coban 1,180Co . Co3+ + 3e
aor + 4H Q + 8e
Co <=> Co2+2 +30,00
2e 25,21 +0,3319,35 -16,44
1,190 38,32 31,47 26,47 -0,28 20*37 17*34
1,200 - 32,94 27,72 21*38 18,25
1,250Co + 20H- => CO(OH)2 + 2e 40,58 33*82 - 0,7326*34 22*82
-
Caimi 1,300Cd C2+ + 2 C + 4CN- o [Cd(CN) 48,42 ]2- + 2e Cd39*68
4 + 20H- -0,40231,15
-1,09 27*41
1,350 - 56,95 45*26 35,82 32,10
o Cdoh + 2e -0,82
1,400 - 66*97 50*50 40*37 36,99
1,450 79,43 55*45 44,79. 42,07
1,500 - 96*73 60,17 49*10 47,33
ng 1,600 2 -
Cu o Cu * + 2e Cu o Cu* + e - 69,09 + 0337
- -
1,700 - - 77*63 -
+ 0,521
- - 87*69 - -
1,800 2+
Cu* o Cu + e + 0,153
Cu + 2CN" [Q(CN)2]- + e -0,43
Cu + cr o CeCl + e + 0337

Grom Cr2+ Cr3* + e -0,41


Cr o Cr3* + 3e 0,74
2Q3* + 7HO o Q2Q72- + 14H* + e + 1,33
Ist
F2+ 0 Fe3* + e + 0,771
Fe 0 Fe3* + 3e -0,037
Fe 0 Fe2+ + 2e -0,440
Fe + 20H 0 Fe(OH)2 + 2e - 0,877
KaM K > K* + e -2,92

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

Thu ngn Hg 0 Hg2* + 2e 4 0 850


2Hg 0 Hg22^ 4 2 4-0/792
Hg + 20 0 Hgada + 2e 4-0,336
Hg -- 20H- 0 HgO + HaO + 2e + 0,098
Hg + HaG 0 HgO + 2H* + 2e + 0,926
Hg + SO42- 0 HgSQ4 4- 2e + 0,614

lot 21- 0 la + 2e 4 0,536


la + 40H- 0 210- 4- HaO 4- 2e 4 0,45
IQr 4- 40H- 0 IQs- + 2HaO + 4e 4 0,14
r 4 3H20 0 IOs: + 6H; + 6s 4 1,08

i*: Li 0 Li* + -3,02

Mage Mg 0 Mg2* + 2e -2,37


Mg -5- 20H- 0 Mg(OH)a + 2e -2,60

Mangan Ma2+ 0 ME3* + e +1,51


Mn 0 Mn2* + 2 -1,19
Mn2+ 4- 2HaG 0 MmGa + 4H* + 2e 4 1,23
MaQ42- 0 MmG4" 4- 4 0,56
MfflOa 4= 40H- 0 MaOr 4- 2Ha + 3e Of\
B4 A 5W
Ml2* 4= 4HaO 0 MffiOr 4= gH* 4= 5e JLI] if

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

Qxy 2HaO 0 Oa + 4H* 4- 4e +1,229


40H- 0 Oa + 2HaO 4- 4e + 0,401
HaOa 0 O2 + 2H* + 2e + 0,682
HQa + OH- 0 O2 + HaO + 2e -0,076
O2 4 HiO 03 =1 2W 4 2 + 2,07
2 4= 20H 03 4 BbO 4 2 4 l924
Ch Pb <=> Pb2+ 4 2e -0,126
Pb 4 30H <=> HPbOf + H20 4 2e - 0,54
Pb2H f 2H2C Pb02 + 4H* 4 2e 4 1,455
PbSC + 2H20 O Pb02 4 4H+ 4 SO f-+ 2e 4 1,68
X,
Pb + S4 <=> PbS04 + 2e , - 0,356
2
-
Thic Sn <=> Sn2+ + 2e - 0,140
Sir* <=> Sn4* + 2e 4 0,15
Sn <=> ... So4* + 4e 4 0,01
SO 2- 4 0,29
L-u : 4 5H2 ,0 2S42- + 10H* + 8e
hunh Sz 2- + 10 0H- - 2S42- + 5H20 + 8e U, /o + 201
O. 4 -
2S0 2
<=> SzOg2- 4 2e

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

1. G.T. Bacvalov, A.V. Turcovskaia. Rukovodstvo k laboratom-m rabotam po


corrosi i galvanostegy. Metallurgia. Moskva. 1965.
2. N.T. Kudriavsev, P.MT Viacheslavov. Praktikum . po prikladni eclectrokhimi .
Khimia. Leningrat. 1973.
3. B.B. Damaskin, O.A. Petti, B.I. Podlochenko... Praktikum po electtokhimi. V-ssaia
skola. Moskva. 1991.
4. C.M.A. Brett, A.M.O. Brett. Electrochemistry. Principles , Methods and Applications.
Oxford. 1993.
5. G.A.Ottewill, F.G Walsh. Electrode Potential Measurments. Trans. Inst. Metal Finish".
1992,70 (3), 141 - 143
6. T.G. Nevell, F.G Walsh. Reference Electrodes. Trans. Inst. Metal Finish 1992 70(3). 144-
147.
7. Trn Minh Hong. Cng ngh m in . Khoa hc v K thut. H ni. 1998.
(l 4 M&CGSP 'H* (jf / ; rwi<j
c cd&n; f/ JL _ 4 . JL /f ^
HL amM\42;i. (hm M / f y
Ma fm A^J45
\t rvm yh 5Jtti - X J

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