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BO CO TH NGHIM

TNG TR
Ngy th nghim: 20/4/2007
H v tn: Nguyn Trung Hiu
I) C S L THUYT
Nghin cu nhng p ng ca in cc nghin cu khi p t ln n
mt in th xoay chiu bin nh c tn s thay i trong phm vi rng
(100 000 Hz 0,0015 Hz ti in th n mn).
in th xoay chiu:

U(t) = Uo. sin (t)

Trong :

l tn s gc = 2..f
f l tn s gc, Hz

Dng in xoay chiu: I(t) = Io.sin(t+) vi l gc lch pha gia U(t)


v I(t)
Tnh cht in ho ca h in cc/ dung dch c nghin cu qua mt
bnh in ho c th coi nh mt mch in bao gm cc thnh phn c bn
sau:
-

in dung lp kp, coi nh mt t in Cd

- Tng tr ca qu trnh Faraday, Zf


- in tr cha c b R, l in tr dung dch gia in cc so
snh v in cc nghin cu.
Tng tr Faraday Zf thng c phn thnh 2 cch tng ng:

Phn thnh mt in tr Rs mc ni tip vi mt gi in dung Cs

Phn thnh in tr chuyn in tch Rct v tng tr khuch tn Zw.

Nu h thng in ho tho mn s Randles th tng tr ca n tng


ng nh sau:

Cd

ZR
Rct

ZW

Hnh 1 S tng ng ca bnh in phn.


Biu din tng tr trn mt phng phc ( th Nyquist)
Tng tr ca qu trnh in cc:

Z() = U(t) / I(t)

in th xoay chiu:

U(t) = Uo. sin (t)

Trong :

l tn s gc = 2..f
f l tn s gc, Hz

Dng in xoay chiu: I(t) = Io.sin(t+) vi l gc lch pha gia U(t) v


I(t)
Z() = Z() j.Z()
Trong :

Z() l phn thc ca tng tr


Z() l phn o ca tng tr, j2 = -1

Nu h thng in ho tho mn s Randles, Ta c:


Z bnh in ho = R + 1/ {f..Cd +[1/Rct + (1-j)..- 1/2 ]}
Trong :
Z = (1-j)-1/2, l hng s Warburg
ZR() = R +{Rct +.

-1/2

} / { [.1/2.Cd +1]2 + 2.Cd2.[Rct + .

-1/2

]2}

ZR() = {. Cd. [ Rct + . -1/2 ]2 +2. Cd + . -1/2 } / { [. 1/2 . Cd + 1 ] +


2. Cd2. [ Rct + . - 1/2 ] 2 }
Khi 0 th:

ZR() = R + Rct + . -1/2


ZR() = -. -1/2 - 2.2.Cd

Biu din ZR() theo ZR() ta c:


2

ZR() = R + Rct ZR() - 2.2.Cd


y l phng trnh ng thng v c th ngoi suy n ct Z R() ti
gi tr (R + Rct -2. 2. Cd). ng thng ny ng vi khng ch khuch tn
v tng tr Warburg vi gc pha 45.
Khi :
vng tn cao phn ng ch b khng ch ng hc v Rct >> Z
ZR() = R +{ Rct/ [1+ 2.Cd2.Rct2 ] }
ZR() = - [.Cd.Rct2 ] / [ 1+ 2.Cd2.Rct2 ]
Do , ta c:

{ZR() - R - [Rct/ 2] }2 + [ZR() ] 2 = [Rct/2]2

l biu thc ca vng trn bn knh (Rct/2), ct trc ZR() ti R khi


v ti (Rct + R ) khi 0.
S biu din tng tr phc nh trn hnh 2 di y:

- Z''
Khong che dong
. hoc
.

max

Khong che khuech tan

1
Rct Cd

.
R + Rct
2

R +Rct
R +Rct

-2

Z'

Cd

Hnh 2 S biu din tng tr trn mt phng phc


Vng trn lin tip xut hin. Khi c s hp th th cn thy c na vng
trn pha di trc Z khi 0.
Ngoi cch biu din trn mt phng phc, tng tr cn c biu din
bng cc ng Bode. l cc ng biu din mi quan h Lg Z theo
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lg f hoc lg theo lg f. Ti cc min tn s cao, cc phn o ca Z bin mt


v ch cn R. tn s rt thp, ch cn R + Rct .
II) TIN HNH TH NGHIM
1) Chun b th nghim
a) Th nghim o tng tr ca thp trong axit khng c v c cht c ch:
Chun b in cc nghin cu: ct mu thp c kch thc 10x1x0,05
cm.
- Ty du m cho thp bng x phng
- Ra sch bng nc
- nh sch bng giy rp t kh n tinh
- Ra sch v trng bng nc ct
- Ty nh bng H2SO4 5-10%
- Ra sch bng nc v trng nc ct
Dung dch nghin cu: axit H2SO4 0,5M khng c v c cht c ch
urothrophin 8g/l.
b) Th nghim o tng tr ca mng sn trong dung dch NaCl 3,5%:
- in cc nghin cu: thp ph sn c gii hn din tch bng ng
nha hnh tr.
- Dung dch nghin cu: NaCl 3,5%

Chun b bnh in ha: cc thy tinh gm 3 in cc:

- in cc nghin cu (nh trn)


- in cc so snh: SCE
- in cc ph: li Pt
2) Tin hnh th nghim:
Mc in cc theo s h 3 in cc
1
3

1)

in cc nghin cu

2)

in cc ph

3)

in cc so snh

4)

Bnh o

5)

Galvanostat / Potentiostat c kt ni my tnh

t cc thng s u vo: khong tn s (5000 Hz n 0,05Hz); bin


th (10mV quanh in th mch h); Din tch mu (1cm2).
o ph tng tr nh phn mm Gamry ca M.

III) KT QU V NHN XT
1) Tng tr ca thp trong axit H 2SO4 khng c v c cht c ch
urothropin
Mu thp c ngm vo dung dch axit v o ngay sau khi ngm. Kt
qu c a ra th hnh 3.

Hnh 3 Tng tr ca thp trong axit H2SO4 0,5M khng c v c cht c ch

Ph Nyquist ca thp trong dung dch axit H2SO4 c v khng c c ch


u c dng 1 cung trn v phn tn s thp c thy s hp ph (c ph quay
ngc li v pha tn s cao).
T ph Nyquist v tnh cht ca h Fe/H 2SO4, c th xy dng m hnh
tng ng ca h nh sau:
Clk

Rp
Hnh 4 S tng ng ca in cc st trong axit H2SO4

Trong : R : in tr dung dch


RP : in tr phn cc
Clk : in dung lp kp
S hp ph trong 2 dung dch ny khc nhau.
Trong dung dch axit H2SO4 c s hp ph H2 kh sinh ra catot khi
thp b ha tan trong dung dch axit hp ph trn b mt thp.
Trong dung dch axit H2SO4 c cht c ch c hp ph mt phn kh H 2
sinh ra catot khi thp b ha tan v mt phn l hp ph cht c ch ln b
mt in cc. S hp ph ny lm ngn cn s ha tan st, hay lm gim
tc ha tan st trong mi trng axit.
T ph c th thy, in tr ca dung dch rt thp, gn nh bng 0.
in tr phn cc trong dung dch axit l:

Rp,0 = 11,1

in tr phn cc trong dung dch axit c cht c ch:

Rp,1 = 16,7

Tc n mn ca thp t l nghch vi in tr phn cc, v th c th


tnh c hiu qu bo v ca cht c ch thng qua in tr phn cc:
S = 100 (Rp,1 Rp,0)/Rp,1 , %
S= 100 (16,7-11,1)/16,7 = 33,5%
T kt qu tnh ton ny c th thy hiu qu bo v ca urothrophin i
vi thp trong axit H2SO4 0,5M thi im ban u ch t 33,5%.
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2) Tng tr ca mng sn

Hnh 5 Ph Nyquist ca mng sn trong dung dch NaCl 3,5% sau 35 ngy

Ph Nyquist cho thy, ph tng tr ca mng sn c hnh bn cung, in


tr ca dung dch gn nh bng 0, trong khi in tr ca mng sn rt ln.
iu chng t qu trnh n mn kim loi bn di lp sn vn cha xy ra
khi mu thp c sn ngm trong dung dch NaCl 3,5% sau 35 ngy.
iu ny cng thy r khi quan st ph Bode v ph tng tr ca mng
sn theo tn s.

Hnh 6 Ph Bode ca h sn trong dung dch NaCl 3,5%


Trn rng: lg Modun theo tn s
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Hnh 7 Tng tr ca h sn trong dung dch NaCl 3,5% theo tn s


Tr rng: trc thc theo lgf

V cha c qu trnh n mn kim loi di lp sn nn s tng


ng ca h nh sau:
R

Cc

Rc
Hnh 8 S tng ng ca mng sn trong dung dch NaCl 3,5%

Trong : R : in tr dung dch


Rc : in tr ca mng
Cc : in dung ca mng