MSSV: 1214360

H tn: PHM TH BCH TRM

Nguyn Duy Khanh
M s nhm thc tp: t6_25
Th 6 , ngy thng 12 nm2013
M s bnh mu kim tra:42
(Hnh thc: nh my, giy A4, font ch Times New Roman, c ch 13, l tri phi trn
di u 2 cm, cch dng 1.3.)
CHUN COMPLEXON
1. Nguyn tc chung
Da vo phn ng to phc cht ca cht cn phn tch v thuc th. N nh
lng c a s cc cation kim loi v mt s anion. Thuc th c dng nu
nht l complexon

1.

Phn ng chun :
M + Y MY
Phn ng ch th:
MIn + Y MY + In
Xc nh nng Mg2+:
Phn ng chun :
Mg+2 + Y-4 MY-2

Phn ng ch th:
MgIn- + Y MY-2 + In
Cng thc tnh sai s ca EDTA:

= () ( )2 + (

0.95,_EDTA

0.03

0.00032

)2 + ( )2

0.05

0.01 (5.00 )2 + (1.00000 )2 + (500.0)2 =0.000060 VEDTA=(0.0100000.000060)M

Bng kt qu chun :
VEDTA (mL)
Ln 1 Ln 2 Ln 3 Trung bnh
11.5

11.55

11.6

11.55

Cng thc v kt qu tnh nng Mg2+:

Nng Mg2+ (M)

0.011550.00014

 ( )
( +2)

CM(Mg+2)=

0.0100000 11.55
10.00

= 0.01155M

Cng thc v kt qu tnh sai s theo chun Student:

0.95,N_Mg+2

1.96 2
)

(+2 ) ( +2

1.960.020 2
)
3

0.01155 ( 10.00

+ (

0.000060

0.95,2,3, 2
)

)2 + (

+ (0.010000 )2 + (

4.300.05000 2
) =0.000145
11.55 3

Biu din kt qu (km sai s):

Nhn xt: (Kt qu chun , sai s, chnh xc, nguyn nhn, cch khc phc
(nu c); kin khc, kin ngh (nu c)).
+2

chnh xc= 1-

= 0.9879(98.79%). Trong qu trnh chun ta dng

khi dung dch trong erlen s chuyn t mu nho sang chm xanh chm.
pH mi trng trong qu trnh chun gim nn ta cn thm m pH=10 n

( +2 )

nh pH trong sut qu trnh chun .

Ch quan st k dng khi dd trong erlen va chuyn sang chm
xanh chm. Thao tc cn thn, chnh xc.

Vai tr ca m pH 10? Cho bit thnh phn ca h m ny?

Thc cht ca phn ng chun s gii phng ra 2H+ lm pH ca mi trng
gim nn ta cn thm pH=10(m amoniac) vo n nh pH mi trng trong
sut qu trnh chun .
-

Th nghim kt thc chun mu g? Ti sao?

MgIn- + Y MY-2 + In.
Ti im cui ca php chun c s ph hy MgIn- mu nho to thnh In
c mu xanh chm.

2. Xc nh nng Ca2+nng cao (10-2M)

Phn ng chun : Ca+2 + Y-4 CaY-2

Phn ng ch th:

Bng kt qu chun :

CaIn-2 + Y CaY-2 + In

VEDTA (mL)
Ln 1 Ln 2 Ln 3 Trung bnh
11.00 11.10 11.10

( )
( +2)

0.0100000 11.07
10.00

= 0.01107M

Cng thc tnh sai s v kt qu theo chun Student:

0.95,N_Ca+2

0.011070.00016

Cng thc tnh v kt qu nng Ca2+:

CM(Ca+2)=

11.07

Nng Ca2+ (M)

1.96 2
)

(+2 ) ( +2

1.960.020 2
)
3

0.01107 ( 10.00

Biu din kt qu (km sai s):

+ (

0.000060

0.95,2,3, 2
)

)2 + (

+ (0.010000 )2 + (

4.300.05774 2
) =0.00016
11.07 3

CM_+2 =(0.011070.00016) M

Nhn xt: (Kt qu chun , sai s, chnh xc, nguyn nhn, cch khc phc
(nu c); kin khc, kin ngh (nu c)).
CX=1- 0.00016/ 0.01107=0.9855 (98.55%) . Trong qu trnh chun pH trong
erlen gim ging nh Mg+2nn t cng thm pH=10 vo n nh pH mi trng
Nguyn nhn c th do sai s ca cc dng c th nghim, thao tc chun cha
chnh xc,
Cch khc phc: quan st n khi to mu trrung gian chm xanh chm th dng.
thao tc chun cn thn, chnh xc .
Mu nhn bit khi kt thc chun ? Ti sao?
Mu xanh chm r rt khi nh d mt git EDTA s c s ph hy CaIn- to thnh In
c mu xanh chm
CaIn- + Y CaY + In

So snh s i mu khi kt thc chun ca th nghim ny vi th nghim mc 1?

S i mu 2 th nghim l tng i ging nhau.

Xc nh nng Ca2+nng thp c v khng c Mg2+(5.10-4M)
Phn ng chun : CaNET( nho nht) + MgY-2 MgNET( nho m) +
CaY-2
Phn ng ch th: MgIn( nho m ) + Y MgY-2 + In(xanh chm)

Sai s EDTA (10-3M):

0.95,_EDTA

0.03

() ( )2 + (
0.000060

)2 + ( )2

0.05

=0.0000060

0.001 (50.00 )2 + (0.010000 )2 + (500.0)2

VEDTA=(0.00100000.0000060)M

Bng kt qu chun :
VEDTA (mL)
Ln 3

Trung
bnh

Nng Ca2+ (M)

4.60 4.70

4.60

4.63

0.0004630.000015

0.00 0.00

0.00

0.00

Th nghim

Ln Ln
1
2

c thm MgY2khng thm

MgY2

Cng thc tnh v kt qu nng Ca2+:

CM(Ca+2)=

( )
( +2)

0.00100000 4.63
10.00

= 0.000463M

Cng thc tnh sai s v kt qu theo chun Student:

0.95,N_Ca+2

1.96 2
)

(+2 ) ( +2

1.960.030 2
)
3

0.000463 ( 10.00

+ (

0.0000060

0.95,2,3, 2
)

)2 + (

+ (0.0010000 )2 + (

4.300.05774 2
) =0.000015
4.63 3

Biu din kt qu (km sai s): (0.0004630.000015)M

Nhn xt: (Kt qu chun , sai s, chnh xc, nguyn nhn, cch khc phc
(nu c); kin khc, kin ngh (nu c)).
CX= 96.83% .

Cho bit vai tr ca vic thm Mg2+?

V Ca+2 nng thp lm cho khong bc nhy b thu hp v im u ca
bc nhy cng ln cao, lm cho im cui nm ngoi ca bc nhy do im cui

hu nh c nh nu gi nguyn pH, lc ch th NET s i mu trc im

tng ng lm cho chun mc sai s thiu
Khi chun EDTA trc im tng ng ca php chun s c phn ng
lm chuyn t mu nho sang nho mnh v sau im tng ng khi ht Ca+2
d mt git EDTA dung dich s chuyn sang mu xanh chm.
Vy im cui ca chun l s i mu ca phc MgNET
- Hm lng Mg2+ thm vo c nh hng n kt qu chun khng?
C. Ti v: phi iu chnh lng MgY-2 thm vo erlen sao cho c cc gi tr pCacui
nm trong khong bc nhy 5.3-8.24: pCacui= 8.4 + p[

] v vy nu cho thm nhng

lng MgY-2 khc nhau s c cc gi tr pCacuoi khc nhau.

3. Xc nh cng chung ca nc
Bng kt qu chun :
VEDTA (mL)

cng ca nc

Ln 1 Ln 2 Ln 3 Trung bnh
6.50

6.55

6.60

6.55

1.3100.027

Cng thc tnh v kt qu cng :

=

(VEDTAVrng)*CEDTA*2*

1000

=(6.550.00)*0.010000*2*

1000
100

=1.31M
Cng thc tnh sai s v kt qu theo chun Student:
_=

0.95,

1.96 2
)

+ (

1.960.500

0.95,2,3, 2
)

)2 + (

0.000060

4.300.05 2
) =0.027
3

1.31 ( 100.00 3 )2 + (0.010000 )2 + ( 6.55

Biu din kt qu (km sai s):

Nhn xt: (Kt qu chun , sai s, chnh xc, nguyn nhn, cch khc phc
(nu c); kin khc, kin ngh (nu c)).
CX=97.94%. chnh xc khng cao do mc cc sai s do thao tc lm chun ,
sai s dng c, quan st s i mu cha chnh xc.

 Cch khc phc: nhn din chnh xc mu sc dng ng thi im chuyn

mu, thao tc cn thn
Th nghim c th cho ta xc nh c hm lng chng ca nc.
- Ti sao ch th NET ch dng cho php chun complexon trong khong pH 711?
NET l mt acid n chc, c dng H3Ind, Hind, Ind c mu khc nhau ln lt
l xanh tm vi pH<7, xanh 7<pH<11 v tm pH>11. Trong khi mu ca
phc cht ca cc kim loi cn chun c mu mn. Khi chun ngi ta
da vo s thay i mu sc ti im tuowng ng, v vy chon mu sao cho s
tng phn l r nht. nh vy ta chn t mu nho(Mind) sang mu xanh Ind
l hp l , trong khong pH t 7_11
Ti sao khi xc nh Mg2+ th chun n chm xanh chm cn khi xc nh
Ca2+ th n xanh chm r rt?
Ti v khong bc nhy ca Ca+2 khong 5.3-8,24 trong khi pCacui2 4.8(nm
ngoi khong bc nhy pCa). Trong php chun ny Mg+2 c chun sau
cng ,pMgcui=6.4 suy ra pCacui= 8.4+

[ ]
[ ]

do [MgY]<[CaY] neen pCacui< 8.4

nm trong khong bc nhy ca Ca+2.

Xc nh nng Cu2+bng ch th Murexid

Phn ng chun :
Cu(NH3)4+2 + Y CuY-2 + NH3+
Phn ng ch th:
CuH2In- (cam) + Y CuY-2 + In (tm hng)
Bng kt qu chun :
VEDTA (mL)
Ln 1 Ln 2 Ln 3 Trung bnh
11.00 10.90 10.90

10.93

0.010930.00016

Cng thc tnh nng Cu2+(th s, kt qu):

CM(Cu+2)=

Nng Cu2+ (M)

( )
( +2)

0.0100000 10.93
10.00

Cng thc tnh sai s theo Student (th s, kt qu):

= 0.01093M

0.95,N_Cu+2

1.96 2
)

(+2 ) ( +2

1.960.030 2
)
3

0.01093 ( 10.00

+ (

0.95,2,3, 2
)

)2 + (

0.000060

+ (0.010000 )2 + (

4.300.05774 2
) =0.00016
10.93 3

Biu din kt qu (km sai s):

Nhn xt: (Kt qu chun , sai s, chnh xc, nguyn nhn, cch khc phc

(nu c); kin khc, kin ngh (nu c)).( 5 dng)

CX= 98.51%.Kt qu chun mc sai s nguyn nhn : do thao tc ngi
chun thiu chnh xc, sai s dng c, quan st im dng mu sc cha
chnh xc .
Cch khc phc: trong qu trnh chun phi lun quan st n mu sc, cun
n khi no thm dd NH3 vo v ta thy mu tm hoa c khng mt i. l
im cui ca php chun .
- C th s dng m pH 10 trong th nghim ny c khng? Gii thch.
Trong dd ang chun vi pH=8. Khng th s dng pH=10 v nu pH cao qu s to
hidroxit vi Cu. Lm nh hng n qu trnh chun .
-

Vai tr ca NH4Cl 1M trong th nghim?

Trong qu trnh chun EDTA c to ra H+ nn ta thm NH3 vo iu chnh
pH ca dd v vy trnh pH tng cao ta thm NH4Cl vo gn cn pH tng
cao.

4.

Xc nh nng Pb2+ vi ch th XO v ch th NET

Phn ng chun : Pb+2 + Y PbY-2
Phn ng ch th:
PbH2In-2 + Y PbY-2 + In
Bng kt qu chun :
Th nghim
ch th XO

VEDTA (mL)
Ln 1 Ln 2 Ln 3 Trung bnh
10.50 10.60 10.60

10.53

0.010530.00016

ch th NET 10.30 10.30 10.40

10.33

0.010330.00016

Cng thc tnh nng Pb2+(th s, kt qu):

( )
( +2)

Ch th XO :CM(Pb+2)=

Nng Pb2+ (M)

0.0100000 10.53

Ch th NET: :CM(Pb+2)= 0.01033 M

Cng thc tnh sai s theo Student (th s, kt qu):

10.00

= 0.01053M

0.95,N_Pb+2

1.96 2
)

( +2 ) ( +2

1.960.030 2
)
3

0.01053 ( 10.00

ch th XO =
2

Ch th NET

0.95,N_Pb+2

+ (

0.000060

0.95,2,3, 2
)

)2 + (

+ (0.010000 )2 + (

4.300.05774 2
)
10.53 3

=0.00016

= 0.00016

Biu din kt qu (km sai s):

Nhn xt: (Kt qu chun , sai s, chnh xc, nguyn nhn, cch khc phc

(nu c); kin khc, kin ngh (nu c)).( 6 dng)

chnh xc =98.45% (chth NET)v99.98% (ch th XO). Trong php chun
d mc sai s tha do do khi chuyn sang mu vng chanh th c nhiu mc
m nht khc nhau rt kh phn bit. khi ta chun vi ch th XO chnh xc
s cao hn do c s chuyn i mu sc r . cn khi thay th bng ch th NET
dng thi im tng ng kh nhn bit mu sc hn nn mc sai s ln hn
chnh xc km hn. Vy ta nn dng thi im chm xanh chm.
So snh s ging v khc nhau gia chun Pb2+ vi ch th XO v ch th NET?
Ging nhau: u dng xc nh nng cng mt cht, u mc nhuwngx sai
-

s ch th nht nh
Khc nhau: chun trc tip cho kt qu chnh xc hn, ch c th p dng i
vi cc kim loi phn ng nhanh vi EDTA v dng li im xc nh mu sc
l mu r rt cn i vi chun thay th bng ch th NET xc nh dng ti
khong mu sc trung gian.
Xc nh hn hp Al3+ + Fe3+
4.1. Xc nh li nng Zn2+ vi ch th XO
Phn ng chun :
Zn+2 + Y ZnY-2
Phn ng ch th:
ZnIn + Y ZnY-2 + In

Bng kt qu chun :
VEDTA (mL)
Ln 1 Ln 2 Ln 3 Trung bnh

Nng Zn2+ (M)

10.60

10.7

10.60

10.60

0.0094330.0002100

Cng thc tnh nng Zn2+(th s, kt qu):

CM(Zn+2)=

( )
(Zn 2+)

0.0100000 10.60
10.00

= 0.01060M Cng thc tnh

sai s theo Student (th s, kt qu):

0.95,_buret

= Z0.95

=(1.96*0.030)/ 3 =0.034

VEDTA=(0.010600.03400)
NEDTA=(0.010000.0001200)

s
0.0500
0.95,_V-Zn2+= 0.95, v-Pipet=t0.952 3 =4.30*
=0.01200
3

VZn2+=(10.600.1200)

NZn2+= NEDTA *VEDTA =(0.0094330.0002100)

VZn2

Nhn xt: (Kt qu chun , sai s, chnh xc, nguyn nhn, cch khc phc

(nu c); kin khc, kin ngh (nu c)).( 5 dng)

N ng Zn 2+ nh hng trc tip n kt qu tinh ton trc tip v sau nn phi chun
1 cch cn thn trnh sai s do sai s n ng Zn
4.2. Xc nh ringFe3+ vi ch th SSA
Nguyn tc:
Chunn trc tip mt th tch chnh xc ca h hp Al+3v Fe+3 bng EDTA ti pH=2
vi ch th SSA n khi mt mu hng tm. Cn un nng ti 70 phn ng xy ra tc
thi. Trong trng hp Al+3 khng b cun bi EDTA v khng cn tr qu trnh
chun Fe+3.
Phn ng chun : Fe+3 +Y-4 FeYFeIn +Y FeY- + In

Phn ng ch th:

Bng kt qu chun :
VEDTA (mL)
Ln 1 Ln 2 Ln 3 Trung bnh
5.00

5.10

5.00

5.03

Cng thc tnh nng Fe3+(th s, kt qu):

Nng Fe3+ (M)

0.005030.0000930

0.95, v-Pipet=Z0.95

= 1.96 0.007000 1.96 0.007000 =0.007900

3

VFe=(10.000.007900)
0.95, VEDTA=t0.952

s
0.0288
=4.30*
=0.720
3
3

VEDTA= (5.030.0720)
NFe= NEDTA *VEDTA =0.00503
VFe3

NFe3+=(0.005030.0000930)

Nhn xt: (Kt qu chun , sai s, chnh xc, nguyn nhn, cch khc phc

(nu c); kin khc, kin ngh (nu c)).( 5 dng)

4.3. Xc nh tng Al3++ Fe3+ vi ch th XO
Nguyn tc
Ht mt lng chnh xc dd chun EDTA cho vo mt th tch chnh xc hn hp Al+3
v Fe+3 to dd m ph=5. Sau chun dd d EDTA bng dd chun Zn+2 vi ch th XO
n khi dd chuyn t mu vng chanh sang hng tm. Khi ph hy c phc AlYv FeY
Phn ng chun :

ZnH2Y-2

ZnY-2

ZnH3Ind-3 (vng chanh) ZnInd- ( hng tm) + 3H+

Phn ng ch th:

Bng kt qu chun :
VEDTA (mL)
Ln 1 Ln 2 Ln 3 Trung bnh
15.65 15.70 15.65

+ 2H+

15.77

Nng tng
Al3+ v Fe3+ (M)
0.014870.0004000

Cng thc tnh tng nng Al3+ + Fe3+(th s, kt qu):

0.95, v-Pipet=Z0.95

= 1.96 0.007000 1.96 0.007000 =0.007900

Vhh=(10,000.007900)
NEDTA=(0.010000.0001200)

s
0.0500
0.95,_V-Zn2+= 0.95, v-Pipet=t0.952 3 =4.30*
=0.01200
3

VZn2+ =(15.770.1200)ml
VEDTA= NZn *VZn =
NEDTA

0.009433*15.77
=14.87ml
0.01

V,EDTA= V ,EDTA2 V , EDTA2 =0.3900

VEDTA=(14.870.3900)
Nhh=0.01487
0.95,_N-hh=

Nhh
Nhh
Nhh
NEDTA
Vhh
Vhh =0.0004000
NEDTA
VEDTA
Vhh

Nhh=(0.014870.0004000)
Cng thc tnh sai s theo Student (th s, kt qu):
Biu din kt qu (km sai s):
Nhn xt: (Kt qu chun , sai s, chnh xc, nguyn nhn, cch khc phc

(nu c); kin khc, kin ngh (nu c)).( 5 dng)

Trong iu kin tin hnh chun l pH = 5, ta c Al3+ v Fe3+ tn ti
di dng phc hydroxo, mun chun trc tip phi tin hnh ph v
phc hydroxo phn ng vi EDTA xy ra rt chm, khng ph hp
yu cu ca mt phn ng chun nn khng th chun trc tip.
Nn chun ngc trong trng hp ny c xem nh gii php ti u.
Vic un nng hn hp sau khi cho mt lng d chnh xc EDTA nhm
cho phn ng xy ra nhanh hn v hon ton.
Thc t chun ngc ch c th thc hin c mt khi tha iu kin:
Phc ca kim loi cho vo chun lng EDTA cn d phi km bn
hn so vi phc ca kim loi to
thnh vi EDTA trc . Ngha l trong phn gii thiu trn pKMY phi
ln hn pKNY.
4.4. Xc nh ring Al3+vi ch th XO
Nguyn tc:
-Dung dch lc ny c AlY-, FeY-, ZnY2-; cho thm NaF vo dung dch trn, s xy ra
phn ng c phng trnh: AlY + 6F- AlF63- + Y;
Lng Y4- to ra tng ng vi lng Al3+ c trong dung dch, chun li lng
Y4- bng dung dch Zn2+ n khi chuyn mu dung dch r rng t vng chanh sang
hng tm; xy ra phn ng : Zn2+ (vng chanh)+ H2Y2- In-(hng tm) + ZnY-

- cc erlen chun xc nh nng tng 2 ion trn ngui, sau tip tc cho
thm 5mL dung dch bo ha NaF, un si 2 pht phn ng to phc xy ra hon
ton, ngui ri cho thm 3 git ch th XO vo, lc u, lc ny dung dch c mu
vng chanh, tin hnh chun bng Zn2+ dung dch chuyn t mu vng chanh sang

Bng kt qu chun :
VEDTA (mL)
Ln 1 Ln 2 Ln 3 Trung bnh
10.90 10.85 10.90

10.88

Nng Al3+ (M)

0.10270.0001600

Cng thc tnh tng nng Al3+(th s, kt qu):

s
0.95, v-Pipet=t0.952 3 =0.12

Cng thc tnh sai s theo Student (th s, kt qu):

VZn2+ =(10.880.1200)
NZn2+=(0.0094330.0002100)

0.95, v-Pipet=Z0.95

= 1.96 0.007000 1.96 0.007000 =0.007900

3

Vhh=(10.000.007900)
NAl3+=

NZn2 *VZn2 0.009433*10.88

=
=0.1027
Vhh
10.00

0.95,N-Al3+=

NAl 3
NAl 3
NAl 3
VZn2
Vhh
Zn2 =0.0001600
VZn2
Vhh
NZn2

NAl3+=(0.10270.0001600)
Nhn xt: (Kt qu chun , sai s, chnh xc, nguyn nhn, cch khc phc

(nu c); kin khc, kin ngh (nu c)).( 5 dng)

Do nhm c kh nng to phc hidroxo khbn, s kh to phc vi EDTA,
khng ph hp vi phng php chun trc tip. Mc khc,c th do khong bc
nhy ca Al3+ kh hp hoc khng c mt ch th no c kh nng to ra pAl cui nm
trong khong bc nhy nn nhn chung chun Al3+ bng phng php trc tip l
mt iu ht sc kh khn. Trong trng hp ny, chun ngc hay chun thay th
l phng php ti u nht
-Ti sao phi un nng dung dch khi chun Fe3+ bng SSA, Al3+ c nh
hng n kt qu chun khng? Gii thch. V phn ng chun ti pH bao
nhiu?

Vic un nng s gip cho phn ng thay th xy ra nhanh v hon ton hn. Vic
cho cht ch th vo hn hp nh phn thc hin nhit thng, tr trng hp
bt buc mi tin hnh s dng ch th khi hn hp nng. Nhit cao c th ph
hy ch th
-

Ti sao phi un nng dung dch khi chun xc nh tng Al3+ v Fe3+? V li
phi ngui mi thm XO?
Do chi th Xo khng bn vi nhit nn nu thm vao luc con nong thi Xo se b phn

hy
Cho bit vai tr ca NaF trong th nghim mc 7.4? : Bng vic cho NaF vo
Al3+ to phc vi F- bn hn phc to vi EDTA.
NHN XT CHUNG(nu c, 10 dng):
-

Chun complexom l phng php phn tch nh lng dng xc nh

nng ca cc hu ht cc ion kim loi ni chung, tr kim loi kim. EDTA phn ng
to phc bn vi hu
ht cc kim loi theo t l 1:1 nn rt thun li trong vic tnh ton kt qu chun .
Phng php chun complexom c nhiu u im trong vic xc nh hm lng
cc ion kim loi trong dung dch. Tuy nhin phng php ny hn ch trong vic xc
nh hn hp cc kim loi khng tinh khit (v EDTA phn ng hu ht vi cc kim
loi nn tnh chon lc khng cao). Do ngi ta c th nng cao tnh chon lc bng
vic s dng cht che

 KIM TRA 2:
Xc nh nng Fe3+ vi ch th SSA
MSSV:1214145
H tn: Nguyn Duy Khanh
M s nhm thc tp: t6_25
Th 6 , ngy 6 thng 12 nm 2013
M s bnh mu kim tra:13

Nng EDTA dng chun :0.01

Bng kt qu chun :
VEDTA (mL)
Ln 1 Ln 2 Ln 3 Trung bnh
9.90

9.85

9.90

9.88

Nng Fe3+ (M)

0.009880.000320