ng dng ca chitosan trong hp ph kim loi nng.

Nh trn ni, trong phn t chitosan cha cc nguyn t N, O. c i

in t t do khng phn chia. Do vy m chng c kh nng to phc vi nhiu
kim loi nh: Cu, Hg, Ni, Pb, Cd, Fe Tuy nhin, tu thuc vo thnh phn cu
trc ca kim loi lm cho kh nng to phc vi chitosan cng khc nhau, v th
m kh nng hp ph ca tng kim loi ln chitosan khc nhau.
C ch chung ca s to phc gia kim loi vi chitosan c a ra
nh sau:
A2+ + 2HL = AL2 + 2H+
Bng nhiu phng php xc nh vt l v ho hc, xc nh c c
ch hp ph ca Cu nh sau:[26]
O

+ Cu
N

O
Cu

Cn vi Cd, Pb c th vit theo c ch[27]

R-NH2 + Pb2+ = R-NH2Pb2+
R-NH2 + H+
= R-NH3+
R-NH3+ + Pb2+ = R-NH2Pb2+ + H+
R-NH2Pb2+ + H2O = Pb(OH)+ + R-NH3+
V mt l thuyt th nhng c ch hp ph kim loi ln chitosan n nay
vn ang l vn xem xt nhiu phng th nghim. Nhng v thc tin th
chitosan vn ang c s dng ngy cng nhiu nhiu nc trn th gii,
chnh v th nghin cu s hp ph kim loi nng ln chitosan l cng vic rt c
ngha.

HO CHT V DNG C
1.Dng c v my mc

Dng c, my mc m chng ti s dng gm c:

-My o pH oakton ca Nht
-My quang ph hp th nguyn t SP9/800 Philip ca H Lan
-Cn phn tch ca phng th ngim phn tch
-My ct nc 2 ln ca b mn phn tch
-Bm lc ht chn khng
-Cc ct nha (ct chit pha rn ) ca Nht
-Pipet cc loi: 0.1ml; 1ml; 2ml; 5ml; 10ml
-Buret loi 25 ml
-Bnh tam gic dung tch 250ml
-Cc thu tinh chu nhit: 50ml; 100ml; 250ml; 500ml v 1000ml
-Bnh nh mc : 10ml; 25ml; 50ml; 100ml; 1000ml
2.Ho cht s dng
2.1 Dung dch chun Cu(II); Pb(II); Cd(II) 1000ppm
+> Dung dch Cu(II) 1000ppm
Cn chnh xc 0.3929g mui Cu(NO3)2.5H2O vo mt cc cn chu nhit
sch, kh. Chuyn lng cn vo bnh nh mc 100ml, sau ho tan bng 10 ml
HNO310%, lc cho tan, ri nh mc thnh 100 bi nc ct 2 ln.
+> Dung dch Pb(II) 1000ppm
Cn 0.1598g mui Pb(NO3)2, ho tan trong bnh nh mc 100ml bng
20ml HNO310%, sau dng nc ct 2 ln nh mc n vch
+> Dung dch Cd(II) 1000ppm
Cn chnh xc 0.1142 g mui CdCl2.2 H2O ho tan trong 10ml HCl 10%,
nh mc thnh 100ml bng nc ct hai ln
Cc dung dch chun trn, sau khi pha chng ti tin hnh chun li nng
theo phng php chun complexon:
Chun Cu(II): bng EDTA pH=8, ch th murexit
Chun Pb(II): bng php chun ngc EDTA, ch th ETOO
Chun Cd(II): bng chun trc tip bi EDTA, pH=10, ch th ETOO
Cc dung dch phc v o ph
- Dung dch HCl 10%

cn chnh xc 27.8g axit HCl 36% bng cc cn sch sau thm 72.2 g
nc ct hai ln
- Dung dch NH4Ac 10%; NH4Na 10%; NH4Cl 10%:
Cn mi mui vi khi lng tng ng 10g, sau ho tan chng bi 90g
nc ct hai ln(tng ng vi 90 ml) ta s thu c dung dch mong mun.
- Dung dch cc ion nh hng: Ni(II); Mn(II); Al(III); Fe(III); K(+); . c pha
thnh cc nng khc nhau vi cc mui ca chng. Khi s dng chng ti pha
long cc dung dch ny theo yu cu kho st.
Dung dch phc v phn hp ph:
- Dung dch NaOH 2M:
Cn 8g NaOH trn cn k thut, ho tan trong bnh nh mc 100ml. Sau
nh mc n vch bng nc ct hai ln
-Dung dch NH3 1M:
dng pipet ly 0.8 ml dung dch NH3 c(25%) pha, nh mc trong bnh
100ml
-Dung dch NH4Cl 1M:
Cn 5.35g mui NH4Cl chuyn hon ton vo bnh nh mc 100ml. Ho
tan v nh mc bng nc ct hai ln
-Dung dch m amoni :
Trn hai th tch bng nhau ca hai dung dch : NH 3 1M v NH4Cl 1M
chng ti thu c dung dch m mong mun. Dng my o pH kim tra li.
- Dung dch EDTA 0.1 M trong m amoni:
Cn chnh xc 3.7224g EDTA, dng m amoin trn ho tan v nh
mc trong bnh 100 ml.

KT QU V THO LUN
I iu kin ti u ca php o FAAS
1.Kho st cc iu kin o ph

 m bo cho php o t hiu qu nht th phi chn c nhng thng

s ti u cho n. Di y chng ti tin hnh chn v kho st cc iu kin v
bt k php o ph FAAS no cng phi thc hin
1.1 Chn vch o
Nh bit, qu trnh sinh ph AAS l do nhng nguyn t trng thi hi
b kch thch bi ngun sng pht tia pht x. Cc nguyn t c kh nng hp
th bc x c bc sng nht nh ng ng vi cc tia m n pht ra.
Tuy nhin qu trnh hp th ny khng xy ra vi tt c cc vch ph m
ch vi vch ph nhy, c trng.
Theo tc gi [38] th vch c trng ca Cu, Pb, Cd nh sau:
Cu
(nm)
324.8
327.4
0

Pb

nhy(ppm)
0.02
5
0.05

(nm)
217.0
283.3

Cd

nhy(ppm)
0.0
8
0.2

(nm)

nhy(ppm)

228.8

0.03

326.9

217.9
0.1
216.4
3.2
222.6
0.5
368.4
8.0
V i tng phn tch ca chng ti nng vi lng nn cn o
nhng vch c nhy cao. Cho nn chn
Nguyn t
Cu
Pb
Cd

(nm)
324.8
217.0
228.8

1.2 Khe o
Khe o nh hng trc tip n chiu cao pic ca nguyn t phn tch. Vi
cc nguyn t Cu, Pb, Cd chng ti chn khe o l 0.5nm.Vi khe o ny th tn
hiu pic nhy, n nh cao, 100% din tch pic ca vch ph s nm trong
khe o.
1.3 Cng n catt rng (HCL)

n catt rng c nhim v ch pht ra nhng tia pht x nhy ca nguyn

t phn tch. Cng dng in lm vic ca n HCL c lin quan cht ch n
vic sinh ra chm pht x v phi c t sao cho nhy cng nh n nh
cao. Thng thng cng n HCL s dng nm trong khong 6085% cng
cc i(Imax).Khng nn dng Imax v n lm vic khng n nh, d
hng, nhy, lp li km.
V nhng l do trn nn chng ti chn cng dng n lm vic ch
bng 80% Imax:
*vi Cu ( I max=12mA) nn chn cng n 10mA
*vi Pb ( I max= 15mA) nn chn cng n 12mA
*vi Cd ( I max= 12mA) nn chn cng n 10mA
1.4 Cc iu kin ghi ph
Tn hiu ca php o di dng pic nn hnh dng pic ph thuc rt nhiu
vo cc iu kin ghi ph. Cc iu kin l:
*Th ghi: thng cc nguyn t phn tch m c nhy cao th ngi ta phi
tng th ca my ghi m bo thang ghi. Cn nhng nguyn t no nhy
km th chn th ghi thp hn :
+> vi Cd c nhy cao nn chn th ghi 20mV
+> vi Cu, Pb chn th ghi 10mV
*Tc giy: thng thng chn tc 30mm/ph
*Thi gian ghi ph: chn thi gian l 5s

Kho st cc iu kin nguyn t ho

1.4 Chiu cao n nguyn t ho
kho st chiu cao n NTH, chng ti lm nh sau:
Pha vo cc bnh 50 ml sao cho nng Cu, Pb, Cd tng ng l 1, 2 ,
1ppm. Thm nn HCl, CH3COONH4 . Sau thay i chiu cao n NTH , ghi
chiu cao pic thu c kt qu:

Nguyn t
H-pic
Pb
( cm)

Cu

Cd

Ln 1
Ln 2
Ln 3
TB
Ln 1
Ln 2
Ln 3
TB
Ln 1
Ln 2
Ln 3
TB

Chiu cao n NTH ( mm)

2
3
4
5
6
0.5
0.65
0.6
0.6
0.65
0.55
0.6
0.55
0.65
0.65
0.5
0.6
0.6
0.6
0.65
0.52
0.62
0.58
0.62
0.65
0.85
0.9
0.9
0.9
0.95
0.8
0.9
0.9
0.85
0.95
0.85
0.85
0.9
0.9
0.95
0.83
0.88
0.9
0.88
0.95
1.3
1.4
1.5
1.5
1.6
1.3
1.4
1.55
1.5
1.5
1.35
1.45
1.5
1.5
1.6
1.32
1.42
1.52
1.5
1.57
Bng 1: nh hng ca chiu cao n NTH

7
0.6
0.7
0.7
0.67
1.0
0.9
0.95
0.95
1.6
1.65
1.6
1.62

Theo kt qu trn thy, ti chiu cao n tng ng 6mm vi Pb; 6mm vi

Cu; 5mm vi Cd th pic thu c cao, n nh v lp li tt nn chng ti chn cc
gi tr .
2.2 Kho st thnh phn kh chy
Thnh phn v tc ca hn hp kh t to ra ngn la l yu t quyt
nh n cng on NTH mu, nh hng trc tip n kt qu ca php o.
Mun t kt qu chnh xc th phi kho st thnh phn kh nhm chn c
nhit ngn la ph hp.
Trong php o FAAS ny, hn hp kh c s dng l: khng kh +
axetilen trong thnh phn ca khng kh c gi c nh (4.75l/p). V th
xem vi t l hn hp kh no tt nht cho php o th chng ti ch thay i tc
ca kh chy(C2H2) thng qua s ch chiu cao folowmeter:
- Chun b dung dch ging phn trn, thay i chiu cao ca folowmeter. ng
thi ghi li pic thu kt qu:

Chiu cao folowmeter( mm)

18
20
21
22
23
24
Ln 1
0.7
0.6
0.6
0.6
0.65
0.7
H-pic
Ln 2
0.7
0.6
0.7
0.6
0.6
0.7
Pb
Ln 3
0.75
0.7
0.7
0.6
0.6
0.75
( cm)
TB
0.72
0.63
0.67
0.6
0.62
0.72
Ln 1
0.95
0.9
0.95
0.95
0.95
0.9
Ln 2
0.95
1.0
1.0
0.95
0.9
0.9
Cu
Ln 3
1.0
1.0
0.9
0.95
0.9
0.85
TB
0.93
0.97
0.95
0.95
0.88
Ln 1
1.75
1.7
1.6
1.65
1.55
1.5
Ln 2
1.80
1.7
1.6
1.65
1.55
1.5
Cd
Ln 3
1.75
1.7
1.65
1.6
1.6
1.55
TB
1.77
1.7
1.62
1.63
1.57
1.52
Bng 2: nh hng thnh phn kh chy
Kt qu trn cho thy:
*t l kh chy ( C2H2 ) vi Pb l 22mm(tng ng 1.12 l/ph)
vi Cu l 22mm(tng ng 1.12 l/ph)
vi Cd l 20mm(tng ng 0.93 l/ph)
th cho pic n nh nht nn chn tc kh chy ny.
3. Cc yu t nh hng n php o[18]
Trong php o ph AAS, c rt nhiu yu t nh hng. Nhng c bit
nht vn l cc yu t ho hc, chng rt phc tp v c th dn n nhng hng
nh sau:
-Lm gim cng vch ph ca nguyn t phn tch do to hp cht bn nhit,
kh ho hi v kh nguyn t ho.
-Lm tng cng vch ph do to cc hp cht d ho hi v d nguyn t ho
hay do hn ch nh hng ca s ion ho v s kch thch ph pht x ca nguyn
t phn tch.
-Tng cng vch ph khi nguyn t phn tch tn ti trong nn ca mu l
nhng hp cht d ho hi. Khi cc cht nn ny nh mt cht mang cho s
ho hi nguyn t phn tch, lm n ho hi vi hiu sut cao.
-Gim cng vch ph khi nguyn t phn tch trong nn ca mu l nhng
hp cht bn nhit, kh ho hi. Lc ny cc nguyn t nn km hm s ho hi
cc nguyn t phn tch.
Nguyn t

Chnh vi nhng tc dng trn m vic kho st nghin cu nh hng ho

hc n php o l rt cn thit.
3.1 nh hng ca thnh phn nn
Nn ca mu trong FAAS thng lm gim cng vch ph ca nguyn
t phn tch do tn ti hp cht bn nhit trong mi trng hp th, gy kh khn
cho qu trnh ho hi v nguyn t ho. loi tr chng th ngi ta thng a
vo mu cht ph gia ph hp nhm ngn cn s hnh thnh hp cht bn nhit.
Trn c s , chng ti tin hnh kho st vi mt s nn nh: NH 4Cl;
CH3COONa; CH3COONH4 v chng d ho hi v c kh nng loi b hp cht
bn nhit. Nng Cu, Pb, Cd trong cc th nghim kho st tng ng l 1; 4; 1
ppm, cn nng cc nn ph gia c thm tng dn. Kt qu c ch ra nh
sau:
3.1.1 Nn NH4Cl

Nguyn t
H-pic
Pb
( cm)

Cu

Cd

Ln 1
Ln 2
Ln 3
TB
Ln 1
Ln 2
Ln 3
TB
Ln 1
Ln 2
Ln 3
TB

3.1.2 Nn CH3COONa

Nng nn NH4Cl (%)

0
1
2
3
4
1.10
1.10
1.10
1.05
1.05
1.10
1.20
1.15
1.15
1.05
1.10
1.15
1.15
1.15
1.10
1.10
1.15
1.13
1.12
1.07
0.95
0.95
0.90
1.0
0.95
0.95
1.0
0.90
1.0
0.90
0.95
1.0
0.90
1.05
0.95
0.95
0.98
0.90
1.03
0.93
1.45
1.60
1.60
1.55
1.55
1.50
1.55
1.50
1.55
1.50
1.45
1.60
1.50
1.60
1.50
1.45
1.58
1.53
1.57
1.52
Bng 3: nh hng ca Nn NH4Cl

5
1.00
1.00
1.05
1.02
0.90
0.90
0.95
0.92
1.55
1.60
1.55
1.57

Nguyn t

Nng nn CH3COONa (%)

0
1
2
3
4
H-pic
Ln 1
1.10
1.10
1.20
1.15
1.20
Pb
Ln 2
1.10
1.10
1.25
1.20
1.30
( cm)
Ln 3
1.10
1.15
1.25
1.20
1.25
TB
1.10
1.05
1.23
1.18
1.25
Ln 1
0.95
0.95
1.00
1.05
0.95
Cu
Ln 2
0.95
0.90
1.00
1.10
0.95
Ln 3
0.95
0.90
1.00
1.05
0.90
TB
0.95
0.92
1.00
1.07
0.93
Ln 1
1.40
1.50
1.60
1.70
1.55
Cd
Ln 2
1.45
1.60
1.55
1.70
1.60
Ln 3
1.40
1.50
1.55
1.60
1.55
TB
1.42
1.53
1.57
1.67
1.57
Bng 4: nh hng ca nn CH3COONa
3.1.3 Nn CH3COONH4
Nguyn t

5
1.30
1.35
1.40
1.35
1.00
1.00
0.95
0.98
1.60
1.60
1.55
1.58

Nng nn CH3COONH4 (%)

0
1
2
3
4
5
H-pic
Ln 1
1.10
1.15
1.20
1.15
1.25
1.15
Pb
Ln 2
1.10
1.20
1.20
1.20
1.20
1.20
( cm)
Ln 3
1.10
1.15
1.20
1.15
1.15
1.20
TB
1.10
1.17
1.20
1.12
1.20
1.18
Ln 1
0.95
1.00
0.90
1.00
0.95
1.00
Cu
Ln 2
0.95
1.00
0.90
0.90
0.90
0.90
Ln 3
0.95
1.00
0.85
1.00
0.90
0.95
TB
0.95
1.00
0.88
0.97
0.92
0.95
Ln 1
1.45
1.50
1.55
1.50
1.45
1.50
Cd
Ln 2
1.45
1.50
1.55
1.50
1.40
1.50
Ln 3
1.50
1.45
1.55
1.40
1.40
1.50
TB
1.42
1.48
1.55
1.47
1.42
1.50
Bng 5: nh hng ca nn CH3COONH4
T cc s liu trn chng ti nhn thy: khi c mt cc cht nn th hu nh
pic thu c cao hn khi khng c cht nn. Tuy nhin vi nn CH 3COONH4 th
cho pic cao hn v ti nng CH3COONH4 l:

2% i vi Pb

2% i vi Cd

1% i vi Cu

th pic n nh nht nn chng ti chn nng nn ny.

3.2 nh hng ca cc loi axit trong dung dch mu
Nng cng nh loi axit trong dung dch mu lun nh hng n
cng vch ph ca nguyn t phn tch. Axit cng kh bay hi th cng lm
gim cng vch ph v c th to thnh nhng cht bn nhit vi nguyn t c
mt trong mu, cn cc axit d bay hi nh hng khng ng k v i khi lm
tng cng vch ph. Chnh v th m trong qu trnh x l mu, ngi ta
thng dng axit d bay hi nh: HCl; HNO 3.. Do vy chng ti kho st nh
hng ca nng mt s axit n php o vi nng Cu; Pb; Cd tng ng: 1;
4; 1 ppm. Kt qu c biu din bng 6
Nguyn t
H-pic
Pb
( cm)

Ln 1
Ln 2
Ln 3
TB
Ln 1
Cu
Ln 2
Ln 3
TB
Ln 1
Cd
Ln 2
Ln 3
TB
Nguyn t

H-pic
Pb
( cm)

Cu

Ln 1
Ln 2
Ln 3
TB
Ln 1
Ln 2
Ln 3
TB

0
0.50
0.50
0.50
0.50
0.75
0.75
0.75
0.75
1.30
1.30
1.30
1.30
0
0.50
0.50
0.50
0.50
0.75
0.75
0.75
0.75

1
0.70
0.70
0.70
0.70
1.10
1.10
1.10
1.10
1.70
1.70
1.65
1.68

Nng HCl (%)

2
3
0.60
0.60
0.60
0.65
0.65
0.65
0.62
0.63
0.90
0.90
0.90
0.90
0.85
0.90
0.88
0.90
1.50
1.45
1.50
1.45
1.45
1.35
1.48
1.42

4
0.55
0.60
0.60
0.58
0.95
0.95
0.90
0.93
1.50
1.40
1.50
1.47

5
0.55
0.60
0.55
0.57
0.90
0.90
0.95
0.92
1.45
1.40
1.40
1.43

1
0.60
0.70
0.70
0.67
1.20
1.15
1.20
1.18

Nng HNO3 (%)

2
3
0.70
0.70
0.70
0.65
0.75
0.65
0.72
0.67
1.00
1.05
1.00
1.05
1.00
1.05
1.00
1.05

4
0.60
0.60
0.70
0.63
1.00
0.95
1.00
0.98

5
0.60
0.60
0.65
0.62
1.00
1.00
1.10
1.03

Ln 1
Cd
Ln 2
Ln 3
TB
Nguyn t
H-pic
Pb
( cm)

Cu

Cd

Ln 1
Ln 2
Ln 3
TB
Ln 1
Ln 2
Ln 3
TB
Ln 1
Ln 2
Ln 3
TB

1.30
1.30
1.30
1.30

1.70
1.60
1.60
1.63

1.50
1.50
1.50
1.50

1.50
1.60
1.60
1.57

1.55
1.50
1.50
1.52

1.50
1.50
1.45
1.48

Nng CH3COOH (%)

0
1
2
3
4
0.50
0.65
0.60
0.65
0.65
0.50
0.65
0.60
0.65
0.55
0.50
0.70
0.60
0.60
0.60
0.50
0.67
0.60
0.63
0.60
0.75
1.00
1.00
0.95
0.95
0.75
1.00
1.00
1.00
1.00
0.75
1.00
0.90
0.95
0.90
0.75
1.00
0.97
0.97
0.95
1.30
1.60
1.55
1.60
1.45
1.30
1.60
1.50
1.55
1.45
1.30
1.55
1.50
1.55
1.50
1.30
1.58
1.52
1.57
1.47
Bng 6: nh hng cc loi axit

5
0.60
0.50
0.60
0.57
0.90
0.95
0.95
0.93
1.45
1.40
1.40
1.42

Nhn vo bng s liu chng ti thy, ti nng axit l 1% th chiu cao

pic thu c hn hn so vi cc nng khc. Trong vi axit HCl th pic cao
nht, n nh nht. V vy chn axit HCl 1% lm nn
3.3 nh hng ca cc ion khc
Trong mu phn tch, ngoi cc ion cn quan tm (Cu; Pb; Cd ) th cn c
rt nhiu ion khc. Cc ion ny c th nh hng hoc khng n php o. Tuy
nhin bit mt cch chnh xc th chng ti tin hnh kho st chng.
3.3.1 nh hng ca cation
kho st nh hng ca cation, chng ti tin hnh kho st theo tng
nhm nguyn t nh sau:
-Nhm kim loi kim
-Nhm kim loi kim th
-Nhm kim loi nng II; III
-Sau l tng cation
(Cng o vi cc bnh nh mc sao cho nng Cu; Pb; Cd tng ng
1;4;1 ppm)

3.3.1.1 nh hng nhm kim loi kim:

Mu s
Na+(ppm)
K+ (ppm)
Li+ (ppm)
H-pic
Ln 1
Pb
Ln 2
( cm)
Ln 3
TB
Ln 1
Cu
Ln 2
Ln 3
TB
Ln 1
Cd
Ln 2
Ln 3
TB

1
2
3
4
5
0
50
100
200
400
0
200
400
600
800
0
5
10
20
30
1.30
1.30
1.25
1.40
1.40
1.30
1.30
1.30
1.30
1.30
1.25
1.20
1.30
1.35
1.30
1.28
1.27
1.28
1.35
1.33
1.10
1.10
1.10
1.10
1.10
1.10
1.05
1.10
1.10
1.10
1.10
1.05
1.10
1.05
1.10
1.10
1.07
1.10
1.08
1.10
1.65
1.60
1.60
1.70
1.60
1.60
1.60
1.60
1.65
1.60
1.60
1.60
1.65
1.65
1.60
1.62
1.60
1.62
1.67
1.60
Bng 7: nh hng ca nhm kim loi kim
3.3.1.2 nh hng nhm kim koi kim th
Mu s
Mg2+(ppm)
Ca2+ (ppm)
Ba2+(ppm)
H-pic
Ln 1
Pb
Ln 2
( cm)
Ln 3
TB
Ln 1
Cu
Ln 2
Ln 3
TB
Ln 1
Cd
Ln 2
Ln 3
TB

1
2
3
4
5
0
30
50
100
150
0
30
50
100
150
0
10
20
30
40
1.25
1.30
1.30
1.20
1.30
1.30
1.25
1.30
1.30
1.30
1.30
1.35
1.20
1.35
1.30
1.28
1.30
1.27
1.28
1.30
1.00
1.00
1.00
1.10
1.00
1.05
1.00
1.00
1.10
1.05
1.05
1.00
1.05
1.05
1.00
1.03
1.00
1.02
1.08
1.02
1.60
1.65
1.60
1.70
1.55
1.60
1.65
1.55
1.75
1.60
1.55
1.60
1.60
1.70
1.55
1.58
1.63
1.58
1.72
1.57
Bng 8: nh hng ca nhm kim loi kim th
3.3.1.3 nh hng kim loi nng nhm II

6
500
1000
50
1.35
1.30
1.30
1.32
1.00
1.00
1.00
1.00
1.60
1.50
1.50
1.53

6
200
200
50
1.25
1.25
1.30
1.27
1.00
0.95
0.95
0.97
1.55
1.50
1.55
1.53

Mu s
Mn2+ (ppm)
Ni2+ (ppm)
Fe2+ (ppm)
Zn2+ ( ppm )
H-pic
Ln 1
Pb
Ln 2
( cm)
Ln 3
TB
Ln 1
Cu
Ln 2
Ln 3
TB
Ln 1
Cd
Ln 2
Ln 3
TB

1
2
3
4
5
0
1
5
10
15
0
1
5
10
15
0
1
5
10
15
0
1
5
10
15
1.30
1.30
1.20
1.25
1.20
1.30
1.20
1.20
1.25
1.20
1.25
1.30
1.30
1.30
1.30
1.28
1.27
1.23
1.27
1.23
1.10
1.05
1.00
1.10
1.05
1.10
1.05
1.00
1.10
1.05
1.05
1.05
1.00
1.10
1.10
1.08
1.05
1.00
1.10
1.07
1.60
1.60
1.60
1.60
1.55
1.60
1.60
1.60
1.55
1.60
1.60
1.60
1.60
1.60
1.55
1.60
1.60
1.60
1.58
1.57
Bng 9: nh hng kim loi nng nhm II

6
20
20
20
20
1.25
1.30
1.30
1.28
1.05
1.05
1.05
1.05
1.60
1.60
1.60
1.60

3.3.1.4 nh hng kim loi nng nhm III

Mu s
Al3+(ppm)
Fe3+ (ppm)
Cr3+ (ppm)
H-pic
Ln 1
Pb
Ln 2
( cm)
Ln 3
TB
Ln 1
Cu
Ln 2
Ln 3
TB
Ln 1
Cd
Ln 2
Ln 3
TB

1
2
3
4
5
0
10
20
30
40
0
10
20
30
40
0
10
20
30
40
1.30
1.20
1.30
1.20
1.30
1.25
1.20
1.25
1.20
1.30
1.25
1.30
1.20
1.30
1.30
1.27
1.23
1.25
1.23
1.30
1.10
1.10
1.00
1.10
1.10
1.10
1.10
1.00
1.10
1.10
1.10
1.10
1.05
1.10
1.10
1.10
1.10
1.02
1.10
1.10
1.60
1.60
1.60
1.60
1.60
1.60
1.55
1.60
1.55
1.60
1.60
1.55
1.55
1.55
1.60
1.60
1.57
1.58
1.57
1.60
Bng 10: nh hng ca kim loi nng nhm III

6
50
50
50
1.25
1.25
1.30
1.27
1.10
1.10
1.05
1.08
1.60
1.55
1.60
1.58

T s liu cc bng trn, chng ti thy cc nhm ion kim loi (vi
nng kho st) u khng nh hng n php xc nh Cu, Pb, Cd.
3.3.1.5 nh hng ca tng cation
Theo kho st trn, tng nhm cation khng nh hng n php o. Tuy
nhin khi c mt tng cc cation ny th s nh th no. V th chng ti tin hnh
kho st tng cation n php xc nh. Cc th nghim vi nng Cu; Pb; Cd
nh trn. Kt qu:
Mu s
Na+ (ppm)
K+ (ppm)
Li+ (ppm)
Mg2+(ppm)
Ca2+(ppm)
Ba2+(ppm)
Fe2+(ppm)
Zn2+(ppm)
Mn2+(ppm)
Ni2+(ppm)
Al3+(ppm)
Cr3+(ppm)
Fe3+(ppm)
H-pic
Ln 1
Pb
Ln 2
( cm)
Ln 3
TB
Ln 1
Cu
Ln 2
Ln 3
TB
Ln 1
Cd
Ln 2
Ln 3
TB

1
2
3
4
5
6
0
50
100
200
400
500
0
200
400
600
800
1000
0
5
10
20
30
50
0
30
50
100
150
200
0
30
50
100
150
200
0
10
20
30
40
50
0
10
20
30
40
50
0
10
20
30
40
50
0
10
20
30
40
50
0
10
20
30
40
50
0
10
20
30
40
50
0
10
20
30
40
50
0
10
20
30
40
50
1.30
1.25
1.20
1.30
1.30
1.30
1.25
1.25
1.20
1.30
1.20
1.30
1.25
1.20
1.25
1.20
1.25
1.25
1.27
1.23
1.22
1.27
1.25
1.28
1.00
1.00
1.00
1.00
1.10
1.10
1.00
1.05
1.00
1.10
1.05
1.10
1.05
1.05
1.00
1.05
1.05
1.05
1.02
1.03
1.00
1.05
1.07
1.08
1.55
1.50
1.60
1.60
1.60
1.50
1.55
1.50
1.60
1.50
1.60
1.55
1.55
1.55
1.55
1.60
1.60
1.55
1.55
1.52
1.58
1.57
1.60
1.53
Bng 11: nh hng ca tng cation
Nhn thy khi c mt tng cc cation th cng khng nh hng ti php

o.
3.3.2nh hng ca anion

Trong nc ngoi cc cation ra th cn c cc anion tan . Hn na trn

chng ti li dng HCl 1% lm nn nn thc t cc anion c mt trong php o vi
lng kh ln. Tu tng hm lng v tng i tng mu m chng c hay
khng gy nh hng.
Phn thc nghim ny chng ti khng kho st nh hng ca Cl - v NO3v phn trc kho st nng ca axit HCl; HNO 3 ti 5% . y chng ti
ch tin hnh kho st nhng ion: SO 42-; H2PO4-. Mu th nghim pha vi nng
Cu l 1ppm, Pb l 4 ppm, Cd l 1 ppm trong nn HCl 1% + CH 3COONH4 2%. o
v ghi chiu cao pic c s liu sau:
Mu s
SO42- (ppm)
H-pic
Ln 1
Pb
Ln 2
( cm)
Ln 3
TB
Ln 1
Cu
Ln 2
Ln 3
TB
Ln 1
Cd
Ln 2
Ln 3
TB

1
0
1.20
1.20
1.25
1.22
1.05
1.05
1.05
1.05
1.60
1.60
1.60
1.60

Mu s
H2PO42H-pic
Ln 1
Pb
Ln 2
( cm)
Ln 3
TB
Ln 1
Cu
Ln 2
Ln 3
TB
Ln 1
Cd
Ln 2

1
0
1.25
1.30
1.25
1.27
1.00
1.00
0.95
0.98
1.55
1.55

2
3
4
50
100
150
1.20
1.20
1.20
1.20
1.20
1.20
1.20
1.20
1.20
1.20
1.20
1.20
1.00
1.00
1.05
1.05
0.95
1.05
1.00
0.95
1.05
1.02
0.97
1.05
1.60
1.60
1.60
1.55
1.60
1.60
1.55
1.55
1.70
1.57
1.58
1.63
Bng 12: nh hng ca ion SO42
2
50
1.20
1.20
1.25
1.22
0.95
0.95
0.90
0.93
1.55
1.55

3
100
1.20
1.20
1.20
1.20
0.95
0.95
0.95
0.95
1.60
1.50

4
150
1.20
1.20
1.25
1.22
0.90
0.90
0.90
0.90
1.60
1.60

5
200
1.15
1.15
1.20
1.17
1.00
1.00
1.05
1.02
1.60
1.60
1.65
1.62

6
300
1.20
1.20
1.20
1.20
1.00
1.00
1.00
1.00
1.60
1.60
1.60
1.60

5
200
1.20
1.20
1.20
1.20
0.95
1.00
0.95
0.97
1.60
1.60

6
300
1.30
1.20
1.20
1.23
0.95
1.00
1.00
0.98
1.60
1.55

Ln 3
TB

1.60
1.57

1.55
1.50
1.60
1.55
1.53
1.60
Bng 13: nh hng ion H2PO42

1.55
1.58

1.55
1.57

Mu s
SO42- (ppm)
H2PO42-(ppm)
H-pic
Ln 1
Pb
Ln 2
( cm)
Ln 3
TB
Ln 1
Cu
Ln 2
Ln 3
TB
Ln 1
Cd
Ln 2
Ln 3
TB

1
2
3
4
5
6
0
50
100
150
200
300
0
50
100
150
200
300
1.20
1.25
1.25
1.25
1.30
1.30
1.25
1.20
1.25
1.30
1.20
1.25
1.20
1.30
1.30
1.30
1.20
1.25
1.22
1.25
1.27
1.28
1.23
1.27
1.00
0.95
0.95
0.90
1.00
1.00
1.00
0.95
0.95
1.00
0.95
1.00
1.00
1.00
0.95
1.00
0.95
0.95
1.00
0.97
0.95
0.97
0.97
0.98
1.55
1.60
1.60
1.55
1.50
1.50
1.60
1.60
1.55
1.55
1.50
1.50
1.55
1.60
1.60
1.55
1.60
1.50
1.57
1.60
1.58
1.55
1.53
1.50
Bng 14: nh hng ca tng anion
Nh vy, vi kt qu trn th cc anion H 2PO42; SO42- tng ng vi nng
trn khng nh hng n cng vch ph ca ba nguyn t.
3.3.3nh hng tng cation v anion
Nhm nh gi mt cch tng qut, chng ti tin hnh kho st nh hng
ca tng cc ion n chiu cao vch ph ca Cu; Pb; Cd(cc mu vn c pha
vi nng v nn nh cc th nghim trn)
Mu s
Na+ (ppm)
K+ (ppm)
Li+ (ppm)
Mg2+(ppm)
Ca2+(ppm)
Ba2+(ppm)
Fe2+(ppm)
Zn2+(ppm)
Mn2+(ppm)
Ni2+(ppm)

1
0
0
0
0
0
0
0
0
0
0

2
50
200
5
30
30
10
10
10
10
10

3
100
400
10
50
50
20
20
20
20
20

4
200
600
20
100
100
30
30
30
30
30

5
400
800
30
150
150
40
40
40
40
40

6
500
1000
50
200
200
50
50
50
50
50

Al3+(ppm)
Cr3+(ppm)
Fe3+(ppm)
SO42- (ppm)
H2PO42-(ppm)
H-pic
Ln 1
Pb
Ln 2
( cm)
Ln 3
TB
Ln 1
Cu
Ln 2
Ln 3
TB
Ln 1
Cd
Ln 2
Ln 3
TB

0
10
20
30
40
50
0
10
20
30
40
50
0
10
20
30
40
50
0
50
100
150
200
300
0
50
100
150
200
300
1.30
1.30
1.30
1.30
1.30
1.35
1.30
1.30
1.20
1.30
1.30
1.35
1.25
1.20
1.25
1.25
1.30
1.30
1.28
1.27
1.28
1.28
1.30
1.33
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.00
1.05
1.00
1.00
0.95
0.95
1.05
1.05
1.00
1.00
0.98
0.98
1.02
1.03
1.55
1.55
1.55
1.55
1.50
1.50
1.55
1.50
1.60
1.60
1.60
1.50
1.50
1.50
1.60
1.60
1.60
1.55
1.53
1.52
1.58
1.58
1.57
1.52
Bng 15: nh hng ca tng ion
Kt qu trn chng t rng cc ion trong vng nng kho st khng nh
hng n php xc nh Cu; Pb; Cd. Hn na, trong mu thc th hm lng ca
cc ion trn nh hn hm lng m chng ti kho st rt nhiu nn c th
khng nh chc chn rng chng khng nh hng. y l mt u im ni bt
ca php o so vi cc phng php khc.
Qua phn thc nghim trn chng ti c th tng kt cc iu kin ti u
o ph ca Cu; Pb; Cd nh sau:
iu kin
Vch o (nm)
Khe o (mm)
Cng n HCL(mA)
Chiu cao n NTH(mm)
Tc giy(mm/ph)
Th ghi (mV)
Thi gian ghi ph (s)
Thnh phn
Khng kh (l/ph)
kh
Axetilen(l/ph)
Tc dn mu (ml/ph)
Thnh phn nn
HCl (%)

Cu
324.8
0.5
10
6
30
10
5
4.75
1.12
5
1

Nguyn t
Pb
217.0
0.5
12
6
30
10
5
4.75
1.12
5
1

Cd
228.8
0.5
10
5
30
20
5
4.75
0.93
5
1

NH4Ac(%)
2
1
Bng 16: tng kt cc iu kin o ph

4 nh gi chung v php o FAAS

4.1 Khong tuyn tnh ca Cu, Pb, Cd
xc nh khong tuyn tnh ca 3 nguyn t trn chng ti pha cc dy
mu chun ca tng nguyn t (trong nn HCl; NH 4Ac) sao cho nng tng dn.
Sau o, ghi li chiu cao pic (mi nng o 3 ln v ly kt qu trung bnh )
thu c kt qu:
4.1.1 Khong tuyn tnh ca Pb
CPb(ppm) 0.5
1
3
5
6
7
8
Hpic(cm) 0.20 0.33 0.90 1.45 1.75 2.00 2.25

9
2.5

10
2.60

0
Bng 17: khong tuyn tnh ca Pb
3.0

2.5

chiu cao pic (cm)

2.0

1.5

1.0

0.5

0.0
0

10

nng
(ppm)

hnh 1: khong tuyn tnh ca Pb

Hnh v trn cho thy khong tuyn tnh ca Pb nm trong on t 0.59
ppm. V th trong tt c cc th nghim phi pha, iu chnh sao cho nng Pb
nm trong khong tuyn tnh .
4.1.2 Khong tuyn tnh ca Cu

CCu(ppm)
Hpic (cm)

0.1
0.10

0.5
1.0
2.0
3.0
4.0
0.40
0.80
1.60
2.45
3.30
Bng 18: khong tuyn tnh ca Cu

4.5
3.70

5.0
4.00

Y Axis Title

X Axis Title

hnh 2: khong tuyn tnh ca Cu

Vy khong tuyn tnh ca Cu l 0.14.5 ppm
4.1.3 Khong tuyn tnh ca Cd
CCd(ppm)
Hpic(cm)

0.1
0.20

0.2
0.5
1
1.8
0.35
0.80
1.55
2.70
Bng 19: khong tuyn tnh ca Cd

2.0
3.00

2.5
3.50

4.0
3.5

chiu cao pic(cm)

3.0
2.5
2.0
1.5
1.0
0.5
0.0
0.0

0.5

1.0

1.5

2.0

2.5

nng
(ppm)

hnh 3: khong tuyn tnh ca Cd

Khong tun theo quy lut tuyn tnh l 0.12.0 ppm
4.2 Lp phng trnh ng chun ca Cu; Pb; Cd
lp phng trnh ng chun cho tng nguyn t chng ti da vo
chiu cao pic thu c ng vi nhng nng pha trong dy mu chun ( s
liu phn 4.1). Sau thc hin cc php ton thng k v hi quy tm ra cc
thng s.
Phng trnh ng chun :
Y = (b b) x + (a a)
Trong :
b ; a: l h s tng quan hi quy
a = t(n-1, P)*Sa
b = t(n-1,P)*Sb
t : chun student, vi P = 0.95
Sa; Sb l sai chun ca a v b
Vy chng ti c bng kt qu sau:
Nguyn
t

Sa

Cu

0.8288

-0.0304

0.0143

Pb

0.2723

0.0802

0.0221

Cd

1.4677

0.0655

0.0098

Sb
0.004
9
0.003
6
0.007
5

2.45

0.0351

0.0121

2.36

0.0523

0.0085

2.57

0.0252

0.0193

Bng 20: bng ng chun ca Cu, Pb, Cd

Phng trnh ng chun l:
+> ca Cu :

y = ( 0.8288 0.0121)x

+ ( -0.0304 0.0351)

+> ca Pb :

y = ( 0.2723 0.0085)x + ( 0.0802 0.0523)

+> ca Cd :

y = ( 1.4677 0.0193)x

+ ( 0.0655 0.0252)

4.3 Gii hn pht hin , gii hn nh lng ca Cu, Pb, Cd

Theo l thuyt thng k th :
-Gii hn pht hin (LOD) ca mt nguyn t l nng thp nht ca nguyn t
m h thng phn tch cn cho tn hiu khc c ngha vi tn hiu mu trng
hay ca nn
-Gii hn nh lng (LOQ) l nng cht phn tch ng vi tn hiu phn tch.
Cng thc tnh LOD v LOQ nh sau:
LOD =

3 Sy

LOQ =

10 S y
b

Kt qu:

Cu
Pb
Cd

Sy
LOD(ppm)
LOQ(ppm)
0.0178
0.064
0.215
0.0249
0.274
0.914
0.0118
0.024
0.081
Bng 21: gii hn pht hin v nh lng ca ca Cu, Pb, Cd

4.4 Sai s v lp li ca php o

4.4.1 Sai s ca php o FAAS trong xc nh Cu, Pb, Cd
nh gi sai s ca php o i vi Cu, Pb, Cd chng ti tin hnh pha
3 mu chun ca 3 nguyn t nm trong ng chun. Sau o ph ca chng,
mi mu o lp li 10 ln v tnh sai s ca mi ln o theo cng thc:

X% =

Trong :

( H1 H 2 )
100
H2

X: sai s phn trm tng i

H1: gi tr chiu cao pic o c
H2: gi tr chiu cao pic tnh theo ng chun
Kt qu nh sau:
Nguyn t
Nng (ppm)
H2(cm)
Ln o
1
2
3
4
5
6
7
8
9
10
TB

Cu
2.0
1.63

Pb
5.0
1.44

Cd
1.0
1.53

H1
X(%)
H1
X(%)
H1
X(%)
1.65
1.23
1.45
0.69
1.55
1.3
1.65
1.23
1.45
0.69
1.55
1.3
1.60
1.84
1.45
0.69
1.55
1.3
1.55
4.9
1.40
2.78
1.50
1.96
1.60
1.84
1.40
2.78
1.55
1.3
1.60
1.84
1.45
0.69
1.50
1.96
1.60
1.84
1.40
2.78
1.60
4.58
1.65
1.23
1.45
0.69
1.55
1.3
1.65
1.23
1.40
2.78
1.55
1.3
1.60
1.84
1.45
0.69
1.50
1.96
1.62
1.9
1.43
1.52
1.54
1.8
Bng 22: sai s ca php o i vi Cu,Pb, Cd
Cc kt qu bng trn cho thy: sai s ca php o i vi 3 nguyn t
tng i nh v u thp hn mc sai s cho php ca php o xc nh cht
lng vt (15%).
4.4.2 lp li ca php o
nh gi lp li ca php o, chng ti thc hin bng cch: o lp
li mt mu ca mi nguyn t ( Cu, Pb, Cd) nhiu ln ( khong 10 ln). Sau
tnh ton cc gi tr phng sai mu(S2) v h s bin ng (CV%) theo cng thc:
S

(H
=

CV (%) =

Trong :

H tb ) 2

n 1

S
100
H tb

Hi: chiu cao pic o c (cm)

Htb: chiu cao trung bnh ca n ln o
n : s ln o
S : lch chun ca mu , v
S = S2

Sau khi tin hnh x l thng k chng ti c bng sau:

Phng sai(S2)
lch chun(S)
CV(%)
0.0011
0.0333
2.07
0.0007
0.0263
1.84
0.0011
0.0333
2.1
Bng 23: lp li ca php o
Nh vy chng ta thy rng phng sai (hay lch chun) v h s bin
thin (CV) ca mu kh nh, iu ny chng t lp li ca php o tt.
Tm li, thng qua cc bc nh gi chung (khong tuyn tnh, lp
li, sai s..) chng ti nhn thy phng php ph FAAS l phng php phn
tch n nh,lp li tt ng thi c chnh xc cao hon ton ph hp cho vic
xc nh vi lng Cu; Pb; Cd trong nc.
Nguyn t
Cu
Pb
Cd

II. Kho st cc iu kin tch, lm giu Cu, Pb, Cd ln chitosan

K thut tch, lm giu Cu, Pb, Cd ln chitosan c th thc hin hai iu
kin:iu kin tnh hoc iu kin ng tu tng yu cu c th. kho st cc
iu kin ti u hp ph ca chitosan th chng ti tin hnh nghin cu trong
iu kin tnh (lc dung dch phn tch vi mt lng chitosan trong cc bnh
nn ). Kh nng hp ph s c nh gi qua thng s q gi l dung lng hp
ph (mg/g):

q=

C0 C
V
a

Vi :
q: lng cht b hp ph trn khi lng cht hp ph (mg/g)
C0: nng ban u ca cht phn tch (mg/l)
C: nng cht phn tch khi t cn bng hp ph(mg/l)
a: lng cht hp ph (g)

q cng ln th kh nng hp ph ion kim loi trn chitosan cng tt.

1. Kho st nh hng ca pH n kh nng hp ph ca chitosan
pH l mt trong nhng yu t rt quan trng n nh hng mnh n kh
nng hp ph ca chitosan.
kho st pH chng ti lm nh sau:
-Cn 18 mu chitosan, mi mu 0.2g cho vo 18 bnh nn
-Pha 50ml cc dung dch Cu(II); Pb(II); Cd(II) vi nng l 100 ppm. Sau
chnh pH ca cc dung dch bng OH- v H+
-Lc cc mu trong 2h tc 1 trn my lc, sau lc, ra dung dch, thu ly
phn dch lc nh mc trong bnh 100ml ri xc nh lng ion cn li nh php
o ph FAAS. Kt qu nh sau:
pH
100

Cu
C(ppm
)
54.8

100

C0(ppm)
3.
0
4.
0
4.
5
5.
0
5.
5
6.
0

q(mg/g) C0(ppm)

Pb
C(ppm q(mg/g) C0(ppm)
)
8
23
100

Cd
C(ppm
)
44.66

q(mg/g)

11.3

100

0.4

24.9

100

9.5

22.63

100

50.55

12.36

100

25

100

3.5

24.13

100

56.45

10.89

100

4.45

23.89

100

24.5

100

47.6

13.1

100

0.85

24.79

100

1.5

24.63

100

53.5

11.63

100

1.3

24.68

100

2.25

24.43

100

24.02

19.0

Bng 24: nh hng pH n kh nng hp ph

13.84

27
Pb

q(mg/g)

25
23
21

Cu

19
17
15
13

Cd

11
9
7
5
2

pH

Hnh 4: nh hng ca pH n kh nng hp ph ca chitosan

T s liu ca bng v hnh v chng ti thy: ti gi tr pH= 4.5 vi Cu,
5.5 vi Pb v 6.0 vi Cd th q ln nht nht tc kh nng hp ph ln chitosan l
tt nht nn chn nhng gi tr pH ny cho cc nghin cu v sau.
2. nh hng ca thi gian lc n kh nng hp ph Cu, Pb, Cd ln
chitosan
i vi Cu: cn 7 mu chitosan, mi mu 0.2g chitosan cho vo 7 bnh
nn. Pha 7 dung dch Cu(II) vi th tch 50ml, nng 100ppm v chnh pH v
4.5 ri lc trn my lc tc 1. C sau mt khong thi gian kho st th ly ra
lc, nh mc phn dch lc trong bnh 100ml xc nh lng Cu(II) d.
i vi Pb v Cd lm tng t nh trn nhng pH ca Pb l 5.5; pH ca
Cd l 6.0 cc kt qu c ch ra trn bng 25 v hnh 5:
Thi
gian(ph)
20
40
60
90
120
150
180

Co
100
100
100
100
100
100
100

Cu
C
19.67
10.96
11.23
10.96
10.79
10.96
10.90

q
20.1
22.26
22.19
22.26
22.30
22.26
22.28

Co
100
100
100
100
100
100
100

Pb
C
29.44
25.24
21.04
16.6
14.04
14.04
14.12

q
17.64
18.69
19.74
20.85
21.49
21.49
21.47

Co
100
100
100
100
100
100
100

Cd
C
34.72
33.33
34.72
33.88
34.72
34.7
34.72

q
1632
16.67
16.32
16.53
16.53
16.33
16.53

Bng 25: nh hng thi gian lc n kh nng hp phu

24

Cu

22
Pb

20
18

Cd

16
14
12
10
10

30

50

70

90

110

130

150

170

190

Hnh 5: nh hng ca thi gian lc n kh nng hp ph ca

chitosan
Nhn xt: t cc s liu trn chng ti thy rng dung lng hp ph q ca
chitosan ph thuc vo thi gian v vo tng kim loi hp ph. Nhn chung thi
gian t cn bng hp ph ca Cd v Cu tng i nhanh (ch sau 20 v 40 pht )
trong khi thi gian t cn bng ca Pb li lu hn, khong 150 pht.
3.Kho st nh hng ca nng Cu(II); Pb(II) v Cd(II) n kh nng hp
ph ca chitosan
3.1 nh hng ca nng Cu(II) n kh nng hp ph ca chitosan
Chun b 6 bnh nn (c nh th t), mi bnh cha 0.2g chitosan. a
lng Cu(II) vo sao cho nng thay i t 40400ppm v pH =4.5 ri lc trong
1h. Sau khi lc xong, lc dung dch v thu dch lc nh mc 100ml ,o ph xc
nh lng Cu(II) cn li. Kt qu ch ra nh sau:
C0(ppm)
40
80
100
160
200
400

C(ppm)
q(mg/g)
10
2.77
19.31
5.49
23.63
15.84
36.04
28.95
42.76
106.9
73.28
Bng 26: nh hng ca nng Cu(II)

C/q
0.143
0.232
0.440
0.677
1.459

80
70
60
q(mg/g)

50
40
30
20
10
0
0

20

40

60

80

100

120

nng Cu cn li

Hnh 7:s ph thuc kh nng hp ph ca chitosan vo nng Cu(II)

Nhn vo hnh v chng ti thy rng, khi nng Cu(II) tng th kh nng
hp ph ca chitosan cng tng ln v n mt gi tr nng no s t bo
ho.
Thc cht hnh biu din 7 c bit l ng hp ph ng nhit
langmuir. tm c dung lng hp ph cc i ca Cu(II) (tc lng Cu(II)
ti a hp ph trn mt lng chitosan ) chng ti tnh ton bng thc nghim
nh sau:
Theo phng trnh langmuir
C
q = qmax
1 +bC

Trong :
q: dung lng hp ph (mg/g)
qmax: dung lng hp ph cc i(mg/g)
b: h s
C: nng cht phn tch khi t cn bng (mg/l)

V ta c:

C
1
bC
=
+
q
qmax
qmax

V th biu din s ph thuc ca C vo C/q th l ng thng:

1.6
1.4

y = 0.0121x + 0.2039
R2 = 0.974

1.2
1
0.8
0.6
0.4
0.2
0
0

20

40

60

80

100

120

Hnh 8: xc nh dung lng hp ph cc i ca Cu

Khi , qmax c tnh l : qmax= 1/tg
Vy: qmax ca Cu l 82.65mg trn mt gam chitosan.
3.2 nh hng ca nng Pb(II) n kh nng hp ph ca chitosan
Tin hnh tng t nh phn Cu, nng Pb(II) thay i t 40 1000ppm,
pH = 5.5. Lc trong 2h tc 1. Kt qu bng sau:
C0(ppm)
40
80
100
200
400

C (ppm)

q(mg/g)

C/q

5.57
8.61
0.647
13.12
16.72
0.785
19.15
24.68
0.776
64.95
33.76
1.924
193.73
51.57
3.757
Bng 27: nh hng ca nng Pb(II)

q(mg/g)

60
50
40
30
20
10
0
0

50

100

150

200

250

nng Pb(II) cn li

Hnh 9: s ph thuc kh nng hp ph ca chitosan vo nng Pb

tm qmax ca Pb chng ti cng thc hin nh phn trn :

y = 0.0167x + 0.5859
R2 = 0.9876

4.5
4
3.5
3
2.5
2
1.5
1
0.5
0
0

50

100

150

200

250

hnh 10: xc nh dung lng hp ph cc i ca Pb

T tnh c qmax = 59.9 mg/g.
3.3 nh hng cu nng Cd(II) n kh nng hp ph ca chitosan
Lm hon ton tng t ging nh trn, nng Cd(II) a vo t 20
600 ppm, pH dung dch l 6, lc trong 1h.
C0(ppm)
20
40
80
160
300
600

C(ppm)
q(mg/g)
13.22
1.7
17.11
5.7
28.59
12.9
67.9
23.0
174.4
31.9
472.4
31.9
Bng 28: nh hng ca nng Cd(II)

35
30

q(mg/g)

25
20
15
10
5
0
0

100

200

300

400

500

nng Cd cn li

Hnh 11: s ph thuc kh nng hp ph ca chitosan vo nng

Cd(II)
Vy khi tng nng ca Cd(II) th kh nng hp ph ca chitosan cng
tng ln v n mt nng nht nh th kh nng hp ph t bo ho. Dung
lng hp ph bo ho ca chitosan i vi Cd l 31.9mg/g
4. Kho st kh nng ra gii Cu(II); Pb(II); Cd(II) bi dung dch EDTA
Ra gii cc ion kim loi Cu; Pb; Cd sau khi tch, lm giu chng ln
chitosan l mt cng vic quan trng nhm xc nh, nh gi nng trong
mu nc. Cng vic ny cng thun li hn khi chng ti tin hnh theo k thut
ng( thut ng ny c gii thch trong phn tng quan).
kho st kh nng ra gii Cu; Pb; Cd khi chitosan, chng ti lm nh
sau:
-Trc ht pha dung dch EDTA 0.1M trong m NH4+/NH3
-Chun b 3 ct nha SPE trong c cha 0.5g
-Pha cc dung dch: Cu(II) 20ppm; Pb(II) 20 ppm; Cd(II) 20 ppm (th tch 50 ml);
pH ln lt l 4.5; 5.5; 6.0
Sau cho 3 dung dch ny chy qua 3 ct SPE trn, chy xong dng
nc ct ra ct khong 3 ln. Tin hnh ra gii bng dung dch EDTA 0.1M
(pH=9) theo tng phn on, mi phn on 5ml. Thu phn chy ra v nh mc
thnh 10 ml, ly ra xc nh lng kim loi bng php o ph FAAS. Kt qu

Nguyn t
Lng ban
u(mg)
Phn on
0
1
2
3
4

Cu

Pb

Cd

Phn
Lng
Phn trm
Lng
trm
Lng
gii
gii
gii
gii
gii
hp(mg)
hp(%H) hp(mg) hp(%H hp(mg)
)
0
0
0
0
0
0.8323
83.23
0.915
91.5
0.86
0.101
10.1
0.083
8.3
0.122
0.032
3.2
0
0
0.013
0
0
0
0
0
Bng 29: kh nng gii hp Cu; Pb; Cd bi EDTA

Phn
trm gii
hp(%H)
0
86
12.2
1.3
0

100
80

%H

60
40
20
0
-20

ph
n on

Hnh 12: kh nng gii hp ca EDTA

T cc s liu trn chng ti thy: dng EDTA 0.1M trong pH = 9 ra gii
kh tt Cu; Pb; Cd khi chitosan v ch vi phn on u (5 ml) th % ra gii
ca chng u kh cao (trn 80%), nn c th thy rng EDTA l mt tc nhn ra
gii thch hp
5. Hiu sut thu hi Cu; Pb; Cd
Hiu sut thu hi ca Cu; Pb; Cd chnh l phn trm khi lng tng
nguyn t thu c sau khi cho chng hp ph trn chitosan v c ra gii bng
EDTA:
Hth(%) = [mgh/mo] x 100
Trong :

mgh: khi lng kim loi gii hp c (mg)

mo : khi lng kim loi ban u (mg)
nh gi v xc nh hiu sut thu hi ca Cu; Pb; Cd chng ti tin
hnh nh sau:
-Chun b 6 ct nha, mi ct cha 0.5g chitosan
-Pha 6 dung dch vi th tch 50 ml, mi dung dch cha hn hp 3 nguyn t Cu;
Pb; Cd c nng ln lt l: 5; 5; 10 ppm. Sau cho 6 dung dch ny chy qua
6 ct nha trn tc 1.2ml/ph. Sau khi chy xong, tin hnh gii hp cc ct
bi 20 ml EDTA 0.1M (pH=9) v nh mc vo bnh 25 ml. o ph xc nh
nng ca chng. Kt qu nh sau:
Cu
Pb
Cd
m0(mg) mgh(mg) %Hth m0(mg) mgh(mg) %Hth m0(mg) mgh(mg) %Hth
0.25
0.252
100.7
0.25
0.231
92.3
0.5
0.48
96.1
0.25
0.251
100.3
0.25
0.237
94.8
0.5
0.509
101.8
0.25
0.229
91.4
0.25
0.232
92.4
0.5
0.434
87.8
0.25
0.244
97.6
0.25
0.245
98
0.5
0.466
93.2
0.25
0.256
102.4
0.25
0.238
95.3
0.5
0.719
94.4
0.25
0.249
99.8
0.25
0.236
94.4
0.5
0.476
95.3
Bng 30: Hiu sut thu hi Cu; Pb; Cd
Nhn xt: qua bng s liu 30, chng ti thy rng hiu sut thu hi Cu; Pb;
Cd kh cao, chng t s kt hp gia phng php ph hp th nguyn t vi s
tch lm giu chng ln vt liu hp ph chitosan l hng nghin cu kh quan
trong phn tch ho hc.
6. H s lm giu Cu; Pb; Cd
Trong nc, thng nng cc ion kim loi rt nh v nm di gii hn
pht hin ca php o nn thc t ngi ta phi tch, lm giu chng trn mt vt
liu no . Sau khi hp thu kim loi trn vt liu th tin hnh ra gii chng
bng mt th tch nht nh ca cht ph hp v th tch ny nh hn th tch mu
thc rt nhiu, v vy nng cc kim loi ny ln hn nhiu ln so vi thc t v
tu thuc vo h s lm giu mu.
Nhm xc nh h s lm giu Cu; Pb; Cd ln chitosan chng ti x l nh
sau:
-Pha 3 mu dung dch Cu(II); Pb(II); Cd(II) (mi dung dch c th tch l 1 lit v
nng 1ppm). Chnh pH ca chng tng ng : 4.5 vi Cu; 5.5 vi Pb v 6.0 vi

Cd. Tip theo cho 3 dung dch chy qua 3 ct nha cha chitosan (0.5g) vi
tc 1.2ml/ph. Ra gii bng EDTA 0.1M (20 ml), thu v nh mc trong bnh
25 ml xc nh nng theo php o FAAS. Kt qu :
Nguyn t
Cu
Pb
Cd

V-u(ml)
m0(mg)
mgh(mg)
% thu hi
H s lm giu
1000
1
0.961
96
40
1000
1
0.979
97.9
40
1000
1
0.993
99.3
40
Bng 31: h s lm giu ca Cu; Pb; Cd
Vy qua bng s liu trn thy rng h s lm giu cc kim loi Cu; Pb; Cd
l rt cao, c ngha nng ca chng ln gp 40 ln so vi ban u. iu ny c
ngha ln i vi thc t phn tch .