H v tn: Phm Minh Tin Nguyn Th Th

MSSV:
MSTT:

1014220

1014212

T3 17

Th ba, ngy 20 thng 3 nm 2012

BI TNG TRNH
PHNG PHP CHUN OXY HA KH

I/ Xc nh nng chnh xc ca KMnO4 theo acid oxalic

1/ Mc ch th nghim:
Do KMnO4 l cht oxy ha mnh, d dng b kh n MnO2 v cng chnh MnO2 li l
cht xc tc tng cng cho s phn hy KMnO4 xy ra nhanh hn theo phng trnh
phn ng sau:
4KMnO4 + 2H2O 4MnO2 + 3O2 + 4KOH
V th, ta khng th dng KMnO4 lm cht gc c v phi chun li dung dch
KMnO4 bng acid oxalic bit chnh xc nng v KMnO4 s c dng lm cht
chun cho th nghim sau.
MnO4- l cht oxi ha mnh nn khng c chun trong mi trng HCl m phi
chun trong mi trng H2SO4.
2/ Nguyn tc.
- Chun KMnO4 bng dung dch H2C2O4 0, 050000 0, 000010N trong mi trng acid
n khi xut hin mu hng nht bn vng trong khong 30s.
- Phn ng chun :
2MnO4- + 5C2O42- +16H+ 2Mn2+ + 10CO2 + 8H2O
3/ Tin hnh:
- Rt 10,00mL dung dch acid oxalic 0,050000N cho vo erlen 250mL, thm vo
1,00mL dung dch H2SO4 (1:1).
- un nng n khong 80 90C .

- Chun bng cch cho tng git dung dch KMnO4, lc u cho ti khi mu hng
bin mt ri mi cho tip. Chun cho ti khi xut hin mu hng nht bn vng trong
30s th dng chun , ghi li th tch KMnO4 tiu tn.
- Lp li th nghim trn 3 ln, thu c cc gi tr sau:

V1

V2

V3

Vtb

5,70mL

5,80mL

5,75mL

5,75mL

Vpipet = (10,00 0,02)mL

VKMnO4 = 5,75 + 0,01= 5,76mL
4/Biu din kt qu:
C N KMnO4 =

C N H 2C2O4 VH 2C2O4

0,95; N KMnO4

VKMnO4

0, 050000*10, 00
= 0, 0866551N
5, 76

0,95; N H 2C2O4
= CKMnO4
CM H C O
2 2 4

2
1,96* pipet 1,96 * buret
+

*
n
*
n
V pipet

V buret

0, 000010 1, 96*0, 02 1,96*0, 05

= 0, 0866551
+
= = 0, 00087N
+
0, 050000 10, 00 * 3 5, 77 * 3

Vy nng ca KMnO4 :

C N KMnO = 0,08666 0,00087 N

4

5/ Nhn xt:
chnh xc ca qu trnh chun :
1

0,95; N KMnO4
0,95; N KMnO4

= 1

0, 00087
= 99, 00%
0, 08666

Th nghim xc nh nng chnh xc ca dung dch KMnO4 theo acid oxalic

khng cn dng cht ch th mu v bn thn dung dch KMnO4 dng oxi ha MnO4c mu tm v dng kh Mn2+ khng mu, ta s chun cho ti khi nng MnO4-
ln c th quan st c mu hng nht ca MnO4-.
Do ion MnO4- v C2O42- cng du v s cho nhn in t gia ion MnO4-(MnO4-
Mn2+: nhn 5e-), v ion C2O42- (C2O42-CO2: cho 2 e-) vi s electron khc nhau, ion
MnO4- v ion C2O42- c cu trc khc nhau, ngoi ra cn do phn ng to thnh kh

CO2 nn phn ng chun xy ra kh chm cn phi un nng 80-90 C cho

phn ng xy ra nhanh hn. Tuy nhin khng nn un si v acid oxalic s b phn
hy.
Do Mangan c nhiu s oxy ha trung gian nn ra c ng s oxy ha ca phn
ng chun ta cn phi thc hin ng h s t lng, thng thng ta thc hin
phn ng trong mi trng acid, v thng l H2SO4(1:1) v dung dch H2SO4 c tnh
oxi ha yu v tnh acid mnh thun li cho qu trnh phn ng . Ta khng th dng
HCl v c tnh kh hoc HNO3 v c tnh oxi ha mnh.
Do dung dch pemanganat khng bn, chun ca n thay i theo thi gian nn
cn phi chun li trc khi s dng.
Vic chun permanganat thng trnh s c mt ion Cl- v Fe2+ v cc ion ny s
b oxy ha ln thnh Clo hoc Fe3+, cng l l do ngi ta khng dng acid
Clohidric. Trn thc t ngi ta thng dng hn hp bo v Zymmerman, hn hp
ny bao gm H2SO4 c tc dng ngn nga s thy phn ca mui st, v s oxi ha
Fe2+ thnh Fe3+ bi oxy khng kh. Th 2, H3PO4 c tc dng to phc khng mu vi
Fe3+ v lm gim th ca cp Fe(H2PO4)2+/Fe2+ thun li cho qu trnh chun , v
Fe3+ thng c mu vng s gy nh hng n vic quan st s thay i mu sc
trong qu trnh chun . Th 3, MnSO4 c tc dng hn gim th ca cp Mn3+/Mn2+.

II/ Xc nh nng H2O2

1/ Mc ch th nghim.
Do H2O2 rt d b phn hy thnh kh O2 v H2O nn b mt dn hot tnh v nng
khng cn chnh xc na. Do ta cn xc nh li ng nng H2O2 vic s
dng hiu qu hn.
2/ Nguyn tc.
- Xc nh hm lng H2O2 qua phn ng vi cht chun KMnO4 trong mi trng
acid sulfuric.
- Phn ng chun :
Hai bn phn ng oxy ha kh
* Bn phn ng kh: MnO4- + 8H+ + 6e- Mn2+ + 4H2O
* Bn phn ng oxy ha: H2O2 - 2e- 2H+ + O2
Phn ng tng: 5H2O2 + 2MnO4- + 6H+ 2Mn2+ + 8H2O + 5O2

- im cui ca phn ng l khi cho lng d KMnO4, xut hin mu hng nht, bn
trong khong 30s.
3/ Tin hnh.
- Chun b buret vi dung dch KMnO4
- Rt 10,00 mL dung dch H2O2 vo erlen 250mL cha sn 20mL nc ct v
5,00mL H2SO4 1:1.
- Chun vi KMnO4 va xc nh li nng lc ny cho ti khi dung dch chuyn
sang mu hng nht bn trong 30s, ghi li th tch KMnO4 tiu tn.
- Lp li th nghim trn 3 ln, ta thu c cc gi tr sau:
V1

V2

V3

Vtb

9,80mL

9,80mL

9,75mL

9,78mL

Vpipet = (10,00 0,02)mL

VKMnO4= 9,78 + 0,02 = 9,80 mL
4/ Biu din kt qu.
C N H 2 O2 =

0,95; N H 2O2

C N KMnO4 VKMnO4
VH 2 O2

0,08666 * 9,80
= 0,0849268 N
10,00

0,95; N KMnO4
= CH 2O2
CKMnO

2
1, 96* pipet t 0,95;n 1 * S n;V KMnO 4

+
+
V * n

*
n
pipet
V

KMnO 4

0, 00087 1,96 *0, 02 4,30* 0, 02887

= 0, 0849268
+
= 0, 0011N
+
0, 08666 10, 00* 3 9,80* 3

Vy nng ca H2O2:

CN- H O = 0,0849 0,0011 N

2

5/ Nhn xt:
chnh xc ca qu trnh chun :
1

0,95; N H 2O2
C N H 2O2

= 1

0, 0011
= 98, 70%
0, 0849

chnh xc khng cao, c th do thao tc chun cha c chun xc.

 Kh nng oxy ha ca KMnO4 mi trng acid mnh hn mi trng kim. Mt

khc, sn phm oxy ha trong mi trng acid l Mn2+ khng mu nn d xc nh
im tng ng, cn phn ng mi trng kim xy ra rt chm, sn phm to
thnh sau phn ng l MnO2 c ta nu en nn kh xc nh im tng ng, do
ta thc hin phn ng trong mi trng acid, v chn acid H2SO4.
Chun b xong mt erlen ri chun lin, khng nn chun b cng lc nhiu mu v
H2O2 rt d b phn hy to thnh O2 v H2O.
Trong qu trnh chun khng nn lc erlen mnh v s lm cho H2O2 b phn hy.

III/ Xc nh nng Fe2+ trong mui Mohr bng K2Cr2O7- ch th Diphenylamin

1/ Mc ch th nghim:
Do mui Mohr Fe(NH4)2(SO4)26H2O lu trong khng kh s b oxy ha lm cho lng
Fe2+ b gim. Th nghim ny nhm mc ch xc nh li chnh xc nng Fe2+ c
trong mui.
2/ Nguyn tc:
- Ha tan mui Mohr ri chun trc tip Fe2+ trong mi trng H2SO4 hoc HCl cho
ti khi dung dch chuyn mu theo ch th th in cc (Ch th Diphenylamine).
- Phn ng chun :
6Fe2+ + Cr2O72- + 14H+ + 6e- 6Fe3+ + 2Cr3+ + 7H2O
3/ Tin hnh
- Chun b buret vi dung dch K2Cr2O7 0,0200000N
- Rt 10,00mL dung dch mui Morh cho vo erlen 250mL.
- Thm 1,00mL H3PO4 c + 10mL HCl (1:2) + 3-4 git ch th DPh 0,1%
- Pha long bng nc ct n khong 30mL.
- Chun bng dung dch chun K2Cr2O7 cho ti khi xut hin mu tm chm th dng, ghi
li th tch K2Cr2O7 tiu tn.
- Lp li th nghim trn 3 ln, ta thu c cc gi tr sau:

V1

V2

V3

Vtb

9,00mL

9,00mL

9,05mL

9,02mL

2+

V Fe = (10,00 0,02)mL
V K2Cr2O7 = 9,02 + 0,02 = 9,04 mL
4/ Biu din kt qu:
C N Fe2+ =

0,95; N Fe2+

CN Cr O 2 VCr O 2
2 7

2 7

V pipet

0, 0200000*9, 04
= 0, 018080 N
10, 00

0,95; N Cr O 2
2 7
= C N Fe2+ *
C N Cr O 2
2 7

0,95; N Cr O 2
2 7
= C N Fe2+ *
C N Cr O 2
2 7

0,95; N V
pipet
+
V pipet

1,96* pipet
+
V pipet * n

2

0,95; N Vburet
+
VCr2O7 2

t0,95 n 1 * sn;VCr O 2
2 7
+
V 2 * n
Cr2O7
2

0, 0000084 1,96*0, 02 4,30*0, 02887

= 0, 01808*
+
= 0, 00015 N
+
0, 0200000 10, 00* 3 9, 04* 3

Vy nng ca Fe2+:
C N Fe2+ = 0,01808 0,00015 N

5/ Nhn xt:
chnh xc ca qu trnh chun : 1

0,95; N Fe2+
CN Fe2+

= 1

0, 00015
= 99,17%
0, 01808

Do dung dch K2Cr2O7 rt bn trong nc, tc chun ca n khng thay i trong

thi gian di ngay c di nh hng ca cc yu t nh nhit , oxy hay kh cacbonic
c trong khng kh nn ta c php dng K2Cr2O7 lm cht gc xc nh nng ca
cc dung dch khc m khng cn phi chun li.
Khc vi phng php Permanganat, phng php Cromat c th tin hnh trong mi
trng acid Clohidric m khng cn dng hn hp bo v Zymmerman.
Ban u phi nh thm vi git HCl vo erlen trc khi cho thm H3PO4 ngn nga
Fe2+ chuyn thnh Fe3+ do s kh ca Fe2+ trong khng kh. Sau thm H3PO4 vo th
mu vng dung dch bin mt do to phc Fe(H2PO4)2+ khng mu. Pha long bng nc
ct sau ny mu ring ca Cr3+ khng cn mu ch th.

 K2Cr2O7 tuy l cht c mu nhng mu ca n khng tng phn, nn rt kh quan

st im tng ng. V vy, ta cn s dng cht ch th in cc DPh (cht ch th in
cc c c im l mu sc ca n thay i t ngt khi th in cc ca dung dch i
qua tng hoc gim ti mt gi tr xc nh c trng cho cht ch th ), chun cho n
khi dung dch c mu tm chm.

IV. Xc nh chnh xc nng Na2S2O3 0,02N theo K2Cr2O7 0,0200000N:

1.

Mc ch, phng trnh phn ng:

Na2S2O3 khng bn, d b phn hy bi CO2 trong khng kh theo phn ng:
H2CO3 +2Na2S2O3 2NaHCO3 + Na2SO3 + S
Lm thay i nng ca cht nn khi s dng cn chun li bit chnh xc nng
ca Na2S2O3.
y l php chun thay th, thay lng Cr2O72- bng lng I3- ri sau chun li
lng I3- bng Na2S2O3.
Phn ng thay th tng ng:
Phn ng chun :
2.

Th nghim, hin tng, gii thch:

Ht 10mL K2Cr2O7 0,02N cho vo erlen 250mL, thm 15mL nc ct, 3mL H2SO4 c v
5mL KI 10%, lc nh, y kn trong 10 pht phn ng hon ton, lc ny dung dch c
mu vng nu. Sau chun bng Na2S2O3 cho ti khi dung dch c mu vng rm ri
mi thm tng git h tinh bt n khi c mu xanh chm r rt l do h tinh bt bt gi
I3- to mu c trng. Tin hnh chun n khi mu xanh chm trn bin mt, dung
dch lc ny trong sut v ch c mu lc nht ca Cr3+.

3.

S liu thc nghim:

K2Cr2O7: 0,0200000 0,0000084 N

V1

V2

V3

Vtb

11,80mL

11,85mL

11,80mL

11,82mL

Vpipet = (10,00 0,02)mL

VS O
2

= 11,82 + 0,02 = 11,84 mL

4.

C N S O 2 =
2 3

Biu din kt qu:

C N Cr O 2 V pipet
2 7

VS O 2

2 3

0,95; N S O 2
2 3

0, 0200000*10, 00
= 0, 016892 N
11,84
2

0,95; N Cr O 2
2 7
= C N S O 2 *
2 3
CN Cr O 2
2 7

0,95; N Cr O 2
2 7
= C N S O 2 *
2 3
C N Cr O 2
2 7

0,95; N V
pipet
+
V pipet

1,96* pipet
+
V pipet * n

0,95; N Vburet
+

Vburet

t0,95;n 1 * sn;V
buret
+

Vburet * n
2

0, 0000084 1,96*0, 02 4,30*0, 02887

= 0, 016892*
+
= 0, 00011N
+
0, 0200000 10, 00* 3 11,84* 3

Vy nng ca S2O32- :
5.

CN- S O = 0,01689 0,00011 N

2

Nhn xt:

chnh xc ca qu trnh chun : 1

0,95; N S O 2
2

C N S O 2
2

= 1

0, 00011
= 99,35%
0, 01689

+ Th nghim ch hn ch n s tht thot I2 ra mi trng bn ngoi v I2 l cht d

bay hi, cn tin hnh y kn cc erlen v tin hnh chun nhanh. Cho KI d va
phi cng lm gim sai s chun v I2 ha tan c trong KI, gi I2 li trong dung
dch di dng I3-. Ngoi ra, cn ch trong mi trng khng kh I- b oxi ha theo
phng trnh phn ng: 4I- + O2 + 4H+ 2I2 + 2H2O
+ Khi chun phi tin hnh chun t t, cho tng git dung dch chun Na2S2O3 t

buret c thi gian cho phn ng oxi ha kh xy ra hon ton v tc phn

ng xy ra chm.
+ Phn ng c to ra Cr3+ c mu lc, c th gy nhn nh lm v im cui ca php

chun do lm vi phc ca I2 v h tinh bt, v th phi tin hnh pha long dung
dch mang i chun bng nc ct.

+ Khng th chun trc tip Na2S2O3 bng K2Cr2O7 c v Na2S2O3 l cht c tnh

kh tng i yu v nguyn t kh c s oxi ha trung gian, khi tc dng vi

K2Cr2O7 l cht oxi ha mnh s b oxi ha v nhiu trng thi vi nhiu s oxi ha
khc nhau, khng tha c iu kin ca mt phn ng chun . Do nn phi
tin hnh chun thay th, chuyn K2Cr2O7 v I3- l cht c tnh oxi ha yu hn
nn ch c th oxi ha
v
m thi. Bn cnh cn li dng c tnh
mu ca I2 m la chn h tinh bt lm cht ch th m khng cn phi tnh ton bc
nhy v iu kin pH ca mi trng phn ng i mu ch th trong khong bc
nhy. H tinh bt y khng phi l cht ch th th in cc m l cht th th c
bit ring cho ion I3- .

V. Xc nh nng Cu2+:
1. Mc ch, phng trnh phn ng:
Trong mi trng acid (pH 1-2) Cu2+ oxi ha I- to ra ta CuI v mt lng tng
ng I3-. Tin hnh chun lng I3- bng thiosunfat vi ch th h tinh bt.
Phn ng thay th:
I3- + 2S2O32- 3I- + S4O62-

Phn ng chun :

2. Tin trnh, hin tng, gii thch:

Ht 10mL dung dch Cu2+ cho vo erlen 250mL, thm 3mL H2SO4 c to mi trng
acid, thm 5mL KI 10% gi I2 trong dung dch, thm 5mL NH4SCN to ta CuSCN.
Sau lc nh, y kn v yn trong bng ti 15 pht phn ng xy ra hon ton,
lc ny trong erlen c ta mu vng nu. Sau pha long thnh 40mL bng nc ct.
Tin hnh chun bng Na2S2O3 0,02N xc nh li nng trn n khi dung dch
trong erlen c mu vng rm, sau cho vi git h tinh bt vo v chun n khi trong
erlen khng cn mu xanh chm ca h tinh bt na, h trong erlen c mu trng c nh
sa. Ngng chun v ghi nhn th tch Na2S2O3 tiu tn.
3. S liu thc nghim:
Na2S2O3 0,02368 0,00015 N
V1

V2

V3

Vtb

10,20mL

10,20mL

10,15mL

10,17mL

Vpipet = (10,00 0,02)mL

VS O
2

= 10,17 + 0,02 = 10,19 mL

4. Biu din kt qu
C N Cu 2+ =

0,95; N Cu 2+

C N S O 2 VS O 2
2 3

2 3

V pipet

0, 01689*10,19
= 0, 01721N
10, 00

0,95; N S O 2
2 3
= CN Cu 2+ *
C N S O 2
2 3

1,96* pipet
+
V pipet * n

t0,95;n 1 * sn;V
buret
+

Vburet * n

0, 00011 1,96*0, 02 4,30*0, 02887

= 0, 01721*
+
= 0, 00017N
+
0, 01689 10, 00* 3 10,19* 3

Vy nng ca Cu2+:
5.

2+

CN- Cu = 0,01721 0,00017 N

Nhn xt:

chnh xc ca qu trnh chun :

0,95; N Fe2+
CN Fe2+

= 1

0, 00017
= 99, 01%
0, 01721

V I2 l cht d bay hi v t tan trong nc nn ta cn phi cho KI vo, th nht l v

KI trong dung dch s phn ly hon ton thnh I-, I- ny s tc dng vi I2 to thnh I3-, c
tc dng gi I2 li trong dung dch. Th hai, I3- l cht phn cc nn s tan tt trong dung
mi phn cc l nc.Trong qu trnh chun khng c lc mnh erlen v s lm iod
bay hi.
Thm H2SO4 m c to mi trng acid c pH~ 2-3, mi trng ny th Cu2+
oxy ha I- to thnh kt ta CuI v mt ng lng I3-. Phn ng xy ra chm, cn nhiu
thi gian phn ng xy ra hon ton. Nu phn ng thc hin trong mi trng acid
mnh s xy ra phn ng ph oxy ha iodua oxi khng kh. V iod nhy sng v phn
ng to kt ta(phn ng d th) nn cn phi y kn erlen v trong ti 15 pht to
iu kin chophn ng xy ra.

VI. Xc nh nng ClO- trong nc Javel:

1. Mc ch, phng trnh phn ng:
Hm lng ClO- trong nc ty ra thng mi thng tham gia phn ng oxi ha kh
vi cht kh l cht mu hay vt bn trn vi. Theo thi gian, hot tnh ca nc Javel c
th gim nu bo qun khng tt. Nn cn xc nh hm lng ca OCl- nh gi hot

tnh thc t ca sn phm. Xc nh bng phng php iod cho OCl- bng phn ng vi
lng d tc nhn kh I- sau chun lng tng ng I2 sinh ra bng Na2S2O3
bng ch th h tinh bt.
Phn ng thay th: ClO- + 2I- + 2H3O+ I2 + Cl- + 3H2O
Phn ng chun : I3- + 2S2O32- 3I- + S4O622. Tin trnh, hin tng, gii thch:
Ht 10mL dung dch ClO- cho vo erlen 250mL, cho thm 20mL nc ct v 5mL KI
10% lc ny dung dch c mu vng nu m ca I3-. Thm 2mL HCl 1:1, lc u to mi
trng acid cho phn ng. Tin hnh chun vi Na2S2O30,02N n khi dung dch c
mu vng nht. Ri sau cho ch th h tinh bt vo c mu xanh tm, tip tc chun
n khi mt mu xanh tm v dung dch trong erlen trong sut khng mu. Tin hnh th
nghim 3 ln ly kt qu trung bnh.
3. S liu thc nghim:
Na2S2O3 0,02368 0,00015 N
V1

V2

V3

Vtb

8,30mL

8,40mL

8,35mL

8,35mL

Vpipet = (10,00 0,02)mL

VS O
2

= 8,35 + 0,016 = 8,37 mL

4. Biu din kt qu.

C N ClO =

0,95; N ClO

C N S O 2 VS O 2
2 3

2 3

V pipet

0, 01689*8,37
= 0, 01414 N
10, 00

0,95; N S O 2
2 3
= C N ClO *
C N S O 2
2 3

1,96* pipet
+
V pipet * n

2
t0,95;n 1 * sn;VS O 2
2 3
+
V 2 * n

S2O3

0, 00011 1,96*0, 02 4,30*0, 05000

= 0, 01414*
+
= 0, 00023N
+
0, 01689 10, 00* 3 8,37 * 3

Vy nng ca Cu2+:

CN-ClO- = 0,01414 0,00023N

5.

Nhn xt:

Trc khi chun phi y kn ming erlen gim lng iod bay hi ra khi

h. V iod d bay hi, lm tht thot lng I2 c trong h nn chun b dung dch
xong l tin hnh chun ngay ch khng nn lu kt qu s b sai s nhiu gia
ln chun trc v ln chun sau. Khi tin hnh chun ch c lc nh erlen
gim lng I2 bay hi ra khi h, gim sai s ng tic.
Khng nn cho ch th h tinh bt vo lc u v h tinh bt s hp th mt phn

I2, nhng li gii hp ph chm(do cu trc c trng ca h tinh bt), dn n l

khi ta cho d Na2S2O3 th mu xanh vn cha bin mt sai s tha ln. V vy,
ta chun cho n khi dung dch chuyn sang mu vng rm (tc l trong dung dch
lc ny cn t I2) th mi cho ch th h tinh bt vo nhm hn ch sai s.

VII/ Xc nh nng chnh xc ca Na2S2O3 0,01N theo K2Cr2O7 .

1.

Mc ch th nghim:

Do chun ca dung dch Na2S2O3 c th b thay i do nh hng ca:

+ Kh cacbonic (Na2S2O3 + CO2 + H2O NaHCO3 + NaHSO3 + S), nng ca dung
dch thiosulfat tng ln do cc ion hidrosunfit hnh thnh phn ng vi iod theo
phng trnh: HSO3- + I2 + H2O HSO4- + 2HI
+ Oxy khng kh ( 2Na2S2O3 + O2 2Na2SO4 + 2S) nng ca dung dch Na2S2O3
gim
chun ca dung dch Na2S2O3 b thay i. Do ta cn chun li xc nh
chnh xc nng ca dung dch Na2S2O3.
2. Nguyn tc:
- Ly mt th tnh chnh xc dung dch chun K2Cr2O7 cho phn ng vi lng d
dung dch KI trong mi trng acid to ra I3- Tin hnh chun trc tip lng I3- trn bng dung dch Na2S2O3 vi ch th h tinh
bt.
Thc cht y chnh l php chun thay th
- Phn ng thay th tng ng:
Cr2O72- + 6I- + 14H+ 2Cr3+ + 3I2 + 7H2O
3I2 + 3I- 3I3-

- Phn ng chun :

I3- + 2S2O32- 3I- + S4O62-

3. Tin hnh:

- Chun b buret vi dung dch chun Na2S2O3.

- Rt 10,00mL dung dch K2Cr2O7 0,0100000 0,0000040 N cho vo erlen 250mL.
- Thm 15mL nc ct + 3mL H2SO4 c + 5mL KI 10%, lc nh.
- y kn v yn 10 pht kh hon ton K2Cr2O7
- Chun t t tng git cho ti khi xut hin mu vng rm ri cho thm vi git dung
dch h tinh bt cho ti khi dung dch c mu xanh chm r rt, va thm va lc u.
- Tip tc chun bng dung dch Na2S2O3 cho ti khi mu xanh chm bin mt, ghi li
th tch Na2S2O3 tiu tn.
- Lp li th nghim trn 3 ln, ta thu c cc gi tr sau:
V1

V2

V3

Vtb

10,20mL

10,15mL

10,15mL

10,17mL

Vpipet = (10,00 0,02)mL

VS O
2

4.

= 10,17+0,02=10,19mL

Biu din kt qu:

C N S O 2 =
2 3

0,95; N S O 2
2 3

V Cr 2O7
V

C N Cr O 2
2 7

pipet

10, 00 *0, 0100000

= 0, 0098135N
10,19

0,95; N Cr O 2
2 7
= C N S O 2
2 3
CN Cr O 2
2 7

0,95; N Cr O 2
2 7
= C N S O 2
2 3
C N Cr O 2
2 7

0,95; N V
pipet
+
V pipet

0,95; N Vburet
+
V buret

1, 96* pipet t 0,95;n 1 * S n;

V buret
+
+
V pipet * n V * n
buret

0, 0000040 1,96 *0, 02 4,30 * 0, 02887

= 0, 0098135
+
= 0, 000073N
+
0, 0100000 10, 00 * 3 10,19 * 3

Vy nng ca Na2S2O3:

C N S O 2 = 0, 009814 0, 000073 N
2 3

5. Nhn xt
chnh xc ca qu trnh chun :
1

0,95; N S O 2
2 3

C N S O 2

=1

2 3

0, 000073
= 99, 26%
0, 009814

chnh xc cao hn so vi 2 phng php permanganat v phng php

bicromat.
Cht kh dng trong phng php Iode lun l thiosulfate phn ng mang

tnh nh lng v lu l Na2S2O3 lun lun nm trn buret do Na2S2O3 d b

phn hy trong mi trng acid .
Na2S2O3 l mt cht kh tng i yu trong nguyn t c tnh kh l S c

s oxy ha trung gian l +2. trng thi oxy ha ny, S c th b kh v 0 hay

-2, cng c th b oxy ha ln +2,5 (Na2S4O6) hay +4, +6. Cc qu trnh ny
din ra ty thuc rt nhiu vo iu kin phn ng v thng khng t lng.
Trong khi , K2Cr2O7 l cht oxy ha kh mnh, s oxy ha Na2S2O3 v nhiu
s oxy ha khc nhau nu ta chun trc tip K2Cr2O7 bng Na2S2O3 th phn
ng chun s khng tha iu kin. V vy, ngi ta chuyn ha K2Cr2O7
thnh cht c tnh oxy ha yu hn l KI3( 3I2 + 3I- I3-) c th oxy ha t
lng Na2S2O3 thnh Na2S4O6.
Ta khng cho ch th h tinh bt vo lc bt u chun m ch cho khi dung

dch chuyn sang mu vng rm (iod trong dung dch gn ht) v khi cho h
tinh bt vo dung dch cha KI3 , ion I3- s chui vo cu trc xon ca phn t
h tinh bt lm cho cu trc ny c mu. S mt mu nhanh hay chm cn ty
thuc vo lng d Na2S2O3 v mc thm nhp ca I3- vo cu trc ca h
tinh bt, nu cho h tinh bt vo lc u, khi lng I3- cn rt nhiu th n s
xm nhp vo su cu trc h tinh bt cn dng mt lng d ln Na2S2O3
mi c th lm mt mu dung dch sai s tha kh ln.
I2 khng phn cc nn t tan trong nc vy nn vic cho KI vo to thnh phc

I3- phn cc d tan hn gip cho qu trnh chun thun li hn.

Cr3+ c mu xanh lc, d gy nhm ln vi mu ca ch th h tinh bt khi cho

vo dung dch nn ta cho nc ct vo pha long dung dch nhm hn ch

iu ny.
Nn ch n thao tc chun , ta khng nn lc mnh erlen trnh cho I2

bay hi.

VIII. Xc nh hm lng oxygen ha tan trong nc (DO) bng phng php

Winkler
1. Mc ch th nghim:

Xc nh lng oxy ha tan trong nc

2. Nguyn tc:

- Phng php da trn c s phn ng m Mn ho tr 2 trong mi trng kim

(dung dch c cho vo trong mu nc trong cng hn hp vi dung dch KI) b O 2
trong mu nc xy ho n hp cht Mn ho tr 4, s ng lng ca hp cht Mn ho
tr 2 lc c kt hp vi tt c O2 ho tan.
Mn2+ + 2OH- = Mn(OH)2
4Mn(OH)2 + O2 = 4MnO(OH) + 2H2O
4MnO(OH) + O2 + 2H2O = 4MnO(OH)2
- S ng lng ca Mn ho tr 4 c to thnh dng kt ta mu vng nu bng s
ng lng xy ho tan trong nc. Khi thm axit H2SO4 vo trong mu, hp cht Mn
ho tr 4 hay ni khc i l s ng lng ca O2 ho tan, chnh bng s ng lng I2
c trong mu nc.
MnO(OH)2 + 4H+ + 3I- Mn2+ + 3H2O + I3I3- sinh ra d dng nh lng bng dung dch chun Na2S2O3.
I3- + 2S2O32- 3I- + S4O623. Tin hnh:
a. C nh mu nc
-Cho nc y bnh nh mc 500mL
- Lp tc cho vo 2mL MnCl2 +2mL dung dch KI/ NaOH (lu l cm u pipet ht cc
dung dch xung di mt thong ca cht lng), y nt chai li sao cho khng c bt
kh, o u xut hin kt ta trng ri chuyn sang mu vng nu.
b. X l mu
- yn bnh nh mc trong mt gi
- Thm 6mL H2SO4 c, o u kt ta vng nu tan ht, dung dch lc ny c mu
vng ca I2
c. Phn tch mu:
- Dng pipet rt 100mL mu cho vo erlen 250mL
- Chun bng Na2S2O3 (0,009814 0,00073)N n khi dung dch chuyn sang mu
vng nht th thm vo 3 git h tinh bt dung dch chuyn sang mu xanh tm. Tip
tc chun cho n khi mu xanh ny bin mt, ghi li th tch Na2S2O3 tiu tn
- Lp li cc bc trn 3 ln, ta thu c cc gi tr sau:

V1

V2

V3

7,65 mL

7,60mL

7,65mL

Vtb
7,63 mL

Vng ong = 100,0 0,025 mL

Vtb = 7,63 + 0,01 = 7,64 mL
Cc bc xc nh th tch gn ng ca bnh nh mc 250mL cha mu nc:
- Np dung dch nc vo bnh ti y trn
- y np li ui phn dung dch do np chim ch
- B np ra, nh du mc dung dch trong bnh
- Rt b phn dung dch trn vch nh mc
- Np dung dch nc vo buret. Qua buret, cho nc vo bnh nh mc cho n vch
mc nh du. Ghi li th tch V* tiu tn
V*= 16,20mL
V dung dch mu = V danh nh + V*
4. Biu din kt qu:
mgO2 / L =
mgO2 / L =

VNa2 S2O3 CN Na2 S2O3

Vmu

Vbdm + V * V1
8 1000
Vbdm

7, 64 0, 009814 500, 0 + 16, 20 4, 00

8 1000 = 6,112505mg / L
100, 0
500, 0

Vi V1 = VMnCl 2 + VKI / NaOH = 2, 00 + 2, 00 = 4, 00mL

V 1 = 1,96* pipet

VMnCl2

2
2

pipet
0, 002
0, 002

+ 1,96*
= 0, 020
+ 1,96*
= 1,96*
VKI / NaOH
2, 00
2, 00

t A=Vbm + V * V1 = 500, 0 + 16, 20 4, 00 = 512, 2mL

2

4,30* S3,V buret V 1

A = 1,96 bm +

+
Vbm
V 3
V1

0, 05 4,30*0, 02887 0, 020

= 1,96
+
= 0, 0050
+
500, 0 16, 20 3 4, 00

 0,05;mg O2

0,95; N Na2 S2O 3

= mgO2 / L
C N Na S O
2 2 3

0,95; N Na2 S2O 3

= mg O2 / L
CN Na S O
2 2 3

0,95; N Vmau 0,95; N Vburet A 2

+
+
+
Vmau
Vtb
A

1, 96* V ongdong
+

Vongdong

2

t0,95;n 1 * sn;V buret

+
Vburet * n

A 2
+
A

0, 000073 1,96*0, 025 4,30*0, 002887 0, 0050

= 6,112505*
+
+
+

7, 64* 3
0, 009814 100, 0
500, 0
= 0, 0072 g

Vy:

mg O2 / L = 6,1125 0,0072 g

5/Nhn xt:
chnh xc ca qu trnh chun :
1

0,95;mgO2 / L
mgO2 / L

= 1

0, 0072
= 99,88%
6,1125

Hn ch ca phng php ny l khng p dng trc tip vi nhng mu nc c

cht oxy ha v n c kh nng oxy ha anion I- hoc cc cht kh (H2S). Mt s ci
bin ca phng php Winkler gip hn ch cc nhc im v phm vi p dng. V
d : phng php ci bin azide c thm KF loi b nh hng ca ion nitite v Fe3+,
phng php ci bin permanganat loi b nh hng ca ion Fe2+. Nhc im th
hai ca phng php ny l chnh xc thng thay i, ph thuc nhiu vo kinh
nghim v k thut thu mu.
Bn cnh , phng php ny c u im l c chnh xc rt cao nn thng
c s dng trong phng th nghim. Dng c cn thit cho phng php ny cng
kh n gin v r tin.
Do phn ng gia Mn(OH)2 vi oxygen din ra kh chm nn ta cn mu nc
c nh ch mt 1h lng oxygen c trong dung dch phn ng ht.
Trong giai on c nh v x l mu nc phi ht sc cn thn, khng oxy
khng kh ha tan vo dung dch (tt nhin khng th hon ton trnh c iu ny
nhng cng hn ch c th kt qu cng chnh xc), c bit lu qu trnh thm
MnCl2 v KI/NaOH vo mu, phi cm u ca pipet vo trong dung dch.

IX. Xc nh nng K2Cr2O7 bng Fe2+ vi ch th ferroin:

1. Mc ch, phng trnh phn ng:
p dng phng php bicromat xc nh nng K2Cr2O7 bng Fe2+ vi ch th
ferroin.

 y K2Cr2O7 c chun trc tip t Fe2+ c nng chnh xc pha t cht

gc l mui Mohr vi s c mt ca ch th ferroin l ch th th in cc nn cn tnh
ton bc nhy phn ng:

Phng trnh phn ng:

E = 0,56V
Khong bc nhy 0,89-1,31, ch th ferroin c E0In=1,06 nm trong khong bc nhy.
Vy tin hnh s dng ch th ny l ph hp chun cho n khi chuyn t mu xanh
chm sang nu.
2. Tin trnh, hin tng, gii thch:
Cho 10mL dung dch K2Cr2O7 vo erlen, thm 5mL H2SO4(1:1) thy dung dch chuyn t
mu vng ti sang mu vng t hi ti, sau nh 2-3 git ch th ferroin vo. Khi
chun th nghim ny cn tin hnh chun tht chm v lc mnh erlen phn ng to
phc xy ra hon ton. Khi cho ch th vo to phc c mu vng cam hi ti, chun
s chuyn sang mu xanh l cy, sau chuyn sang mu xanh dng, khi chuyn sang
mu xanh dng hi ti, lc ny gn n im cui, cn ngng cho Fe2+, ly erlen ra
v tin hnh lc u mnh, thy mu xanh ti s chuyn li sang mu xanh dng trong,
li tip tc cho Fe2+ vo tng git mt, tin hnh chun n khi dung dch c mu
nu nh mu ch th ferroin, bn khng bin mt trong 1 pht l ngng chun v ghi
nhn th tch ca Fe2+. Tin hnh th nghim 3 ln ly kt qu trung bnh.
3. S liu thc nghim:
Fe2+: 0,020000 0,000010 N
V1

V2

V3

Vtb

12,40mL

12,40mL

12,45mL

12,42mL

V K2Cr2O7 = (10,00 0,02)mL

2+

V Fe = 12,42 + 0,02 = 12,44 mL

4.

Biu din kt qu:

C N Cr O 2 =
2 7

C N Fe2+ VFe2+
V pipet

0, 0200000*12, 44
= 0, 024880 N
10, 00

 0,95; N Cr O 2
2 7

2+
= CN Cr O 2 * 0,95; N Fe
2 7
C
N Fe2+

1,96* pipet
+

V pipet * n

2
t0,95;n 1 * sn;VCr O 2
2 7
+
V 2 * n
Cr2O7

0, 0000025 1,96*0, 02 4,30*0, 02887

= 0, 024880*
+
= 0, 00015 N
+
0, 0200000 10, 00* 3 12, 44* 3

Vy nng ca Fe2+:

C N Fe2+ = 0,02488 0,00015 N

5. Nhn xt:
chnh xc :

0,95; N K Cr O
2

2 7

C N K2Cr2O7

= 1

0, 00015
= 99, 40%
0, 02488

Trong iu kin th nghim gp phi sai lch gia 2 ln chun nhanh khi erlen

cn nng v lc ta ngui. C th gii thch hin tng ny v khi ta pha dung

dch H2SO4 c vo th s sinh ra 1 lng nhit kh ln, lng nhit ny s thc y
phn ng chun cng nh phn ng ch th nn nu ta chun lin th th tch thu
c s ln hn vic mt lc mi chun.
Ta nn chun chm vi tc va phi th s chnh xc hn so vi vic chun

nhanh v nh th phn ng s xy ra c hon ton v gip ta d nhn bit im

cui. Ti im cui ny s xut hin mu nu thng hin ra v bin mt kh lu
do ta phi lc k kim chng mu nu bn hay cha.
Khng nn cho vo dung dch H2SO4 qu c v nu cho dung dch qu c,

H2SO4 khng cn ng vai tr to mi trng na m tr thnh cht oxi ha, kh

Fe2+ thnh Fe3+ gy sai s kh ln.
NHN XT CHUNG:
Phng php permanganat:
KMnO4 l mt cht oxy ha mnh c s dng rng ri trong php chun , u
im ca phng php ny l phn ng t xc tc nn xy ra nhanh dn v vic xc
nh im cui da vo mu ca ion MnO4- nn hn ch c nh hng ca cht ch
th v khng cn tnh trc khong bc nhy. Nhc im ca phng php ny
cng chnh l do tnh oxy ha ca KMnO4 qu mnh nn n oxy ha c giy v bi
trong khng kh nn kh pha dung dch chun v kh bo qun. Khi dng phng
php permanganat ta cng khng th s dng acid HCl khi c mt Fe2+ nn ta thng
s dng H2SO4.
Phng php bicromat:

Mc d l mt cht oxy ha km hn KMnO4 nhng th ca K2Cr2O7 vn kh cao nn

c th dng thay th phng php permanganat trong bt k php chun no m
phng php permanganat c th dng c. Ngoi ra n cn c u im l mt cht
chun gc n nh trong iu kin thng nn khi s dng khng cn phi nh phn
li.Khng nh phng php permanganat, n c th s dng HCl to mi trng
acid m khng s c phn ng ph. Phng php phi s dng cht ch th th in
cc nn ta phi tnh ton khong bc nhy th la chn ch th ph hp.
Phng php thiosulfat:
Khng ging nh 2 phng php permanganat v bicromat ch cho php chun cc
cht kh th phng php thiosulfat cho php chun cc cht c th cao hn cp
I2/I- v ta chun vi phc I3- (phn ng c trng ca phng php thiosulfat). Ty
thuc vo th oxy ha kh ca cht m ta dng php chun thay th hoc
chun ngc.
Cc phng php oxi ha kh c chnh xc cao, lp li tt, nhiu phng php
thc hin rt nhanh; nhiu phng php a dng, do c th s dng rng ri trong
kim tra, phn tch sn xut. S chun oxi ha c th thc hin nhiu mi trng v
i khi khng cn n ch th xc nh im cui ca php chun . Cn phi bit
c bn cht phn ng c th xc nh ng c ch th hay xc nh c tc
khi tin hnh chun phn ng chun t hiu qu cao nht.

H v tn: Phm Minh Tin

MSSV: 1014220
M s dung dch kim tra s 10
Kim tra nng K2Cr2O7 bng Fe2+ vi ch th ferroin

Tin hnh:
- Thm nc vo n vch mc ca bnh nh mc.
- Rt 10,00mL dung dch K2Cr2O7 cn xc nh nng cho vo erlen 250mL.
- Thm 5mL H2SO4 (1:1) + 3 git ch th ferroin.
- Chun vi dung dch Fe2+ 0,020000 0,000010 N cho ti khi mu thay i t xanh
chm sang nu bn trong 1 pht, ghi li th tch Fe2+ tiu tn.

S liu thc nghim:

Fe2+: 0,020000 0,000010 N
V1

V2

V3

Vtb

10,50mL

10,55mL

10,55mL

10,53mL

V K2Cr2O7 = (10,00 0,02)mL

2+

V Fe = 10,53 + 0,02 = 10,55mL

Biu din kt qu:

C N Cr O 2 =

C N Fe2+ VFe2+
V pipet

2 7

0,95; N Cr O 2
2 7

0, 0200000*10,55
= 0, 021100 N
10, 00

2+
= CN Cr O 2 * 0,95; N Fe
2 7
C
N Fe2+

2+
= C N Cr O 2 * 0,95; N Fe
2 7
C
N Fe2+

0,95; N Vpipet
+
V pipet

1,96* pipet
+

V pipet * n

2
t0,95;n 1 * sn;VCr O 2
2 7
+
V 2 * n
Cr2O7
2

0,95; N Vburet
+
VCr2O72

0, 0000025 1,96*0, 02 4,30*0, 02887

= 0, 02110*
+
= 0, 00015 N
+
0, 0200000 10, 00* 3 10,55* 3

Vy nng ca Fe2+:
C N Fe2+ = 0,02110 0,00015 N

Nhn xt:
chnh xc :
1

0,95; N K Cr O
2

2 7

C N K2Cr2O7

= 1

0, 00015
= 99, 29%
0, 02110

Li dng nhit khi cho thm H2SO4 vo phn ng chun din ra nhanh v hon
ton hn, v th lm n u th chun b erlen n , chun ngay khng lu trnh
sai s.
Phn ng chuyn mu rt phc tp, khi chun phi chun tht chm vi tng git
dung dch Fe2+, tin hnh lc erlen tht mnh v u sao cho dung dch trong erlen xoay
xoy trn u. Khi thy dung dch chuyn sang mu xanh ti th ngng cho Fe3+ vo, ly
erlen ra v lc tht mnh dung dch s chuyn li sang mu xanh ti hn v lc ny
gn i n im cui . Phn ng ny rt d c sai s do thao tc chun , ch yu do lc
khng k v chun qu nhanh
Phng php ny l phng php bicromat, phng php ny c th dng K2Cr2O7
xc nh lng Fe3+ v dng Fe3+ xc nh li nng K2Cr2O7 u c. Phng
php ny c nhc im l bicromat phn ng chm vi nhiu cht kh nn dung dch
bicromat i khi khng th dng chun trc tip c m phi dng phng php
chun ngc, im i mu kh nhn bit nn phi dng cht ch th in cc.
bicromat c tnh oxi ha yu hn permanganat nn lng cht c th dng chun t
hn, nhng c u im l bicromat c th iu ch c nng chnh xc v bn, kh
b kh bi cc cht hu c trong nc v trong mi trng.

H v tn: Nguyn Th Th
MSSV:

1014212

M s dung dch kim tra s: 8

Kim tra nng K2Cr2O7 bng Fe2+ vi ch th ferroin

Tin hnh:
- Thm nc vo n vch mc ca bnh nh mc.
- Rt 10,00mL dung dch K2Cr2O7 cn xc nh nng cho vo erlen 250mL.
- Thm 5mL H2SO4 (1:1) + 3 git ch th ferroin.
- Chun vi dung dch Fe2+ 0.020000 0.000010 N cho ti khi mu thay i t
xanh chm sang nu bn trong 1 pht, ghi li th tch Fe2+ tiu tn.

S liu thc nghim:

Fe2+: 0,0200000 0,0000025 N
V1

V2

V3

Vtb

10,75mL

10,75mL

10,80mL

10,77mL

V K2Cr2O7 = (10,00 0,02)mL

2+

V Fe = 10,77 + 0,02 = 10,79mL

2/ Biu din kt qu:

C N K 2 Cr2 O7 =

0,95; N K2Cr2O7

C N Fe 2+ V
V pipet

2+
Fe = 0,0200000 * 10,79 = 0,0215800 N
10,00

2+
= CN K2Cr2O7 0,95; N Fe
C
N Fe2+

0,95; N V pipet
+
V pipet

0,95; N Vburet
+
V buret

2
2
0,95; N Fe 2+ 1,96* pipet t 0,95; n 1 * S n;V Cr 2O 72

= C N K 2Cr2O7
+
+
C
V pipet * n

n
2 *
2+
N Fe
V Cr 2O 7

0, 0000025 1,96*0, 02 4, 30*0, 02887

= 0, 0215800
+
= 0, 00015N
+
0, 0200000 10, 00 * 3 10, 79* 3

Vy nng ca K2Cr2O7:

C N K 2 Cr 2 O7 = 0,02158 0,00015 N

Nhn xt:
chnh xc:

0,95; N K 2 Cr 2 O 7

C N K 2Cr 2O 7

= 1

0, 00015
= 99,30%
0, 02158

Li dng nhit khi cho thm H2SO4 vo phn ng chun din ra nhanh v
hon ton hn, v th lm n u th chun b erlen n , chun ngay khng lu
trnh sai s.
Phn ng chuyn mu rt phc tp, khi chun phi chun tht chm vi tng
git dung dch Fe2+, tin hnh lc erlen tht mnh v u sao cho dung dch trong erlen
xoay xoy trn u. Khi thy dung dch chuyn sang mu xanh ti th ngng cho Fe3+
vo, ly erlen ra v lc tht mnh dung dch s chuyn li sang mu xanh ti hn v
lc ny gn i n im cui . Phn ng ny rt d c sai s do thao tc chun ,
ch yu do lc khng k v chun qu nhanh
Phng php ny l phng php bicromat, phng php ny c th dng
K2Cr2O7 xc nh lng Fe3+ v dng Fe3+ xc nh li nng K2Cr2O7 u
c. Phng php ny c nhc im l bicromat phn ng chm vi nhiu cht kh
nn dung dch bicromat i khi khng th dng chun trc tip c m phi
dng phng php chun ngc, im i mu kh nhn bit nn phi dng cht
ch th in cc. bicromat c tnh oxi ha yu hn permanganat nn lng cht c th
dng chun t hn, nhng c u im l bicromat c th iu ch c nng
chnh xc v bn, kh b kh bi cc cht hu c trong nc v trong mi trng.