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vn
I HC THI NGUYN
TRNG I HC S PHM
--------------------------



PHM TH HNG THI




NGHIN CU PHNG PHP
PHN TCH VI LNG IOT TRONG CC
I TNG MI TRNG


Chuyn ngnh: Ho Phn tch
M s: 60.44.29



L LU U N N V V N N T TH H C C S S H HO O H H C C









THI NGUYN - 2009
S ha bi Trung tm Hc liu i hc Thi Nguyn http://www.Lrc-tnu.edu.vn
I HC THI NGUYN
TRNG I HC S PHM
--------------------------



PHM TH HNG THI



NGHIN CU PHNG PHP
PHN TCH VI LNG IOT TRONG CC
I TNG MI TRNG


Chuyn ngnh: Ho Phn tch
M s: 60.44.29


L LU U N N V V N N T TH H C C S S H HO O H H C C



Ngi hng dn khoa hc: GS. TS TRN T HIU






THI NGUYN - 2009
S ha bi Trung tm Hc liu i hc Thi Nguyn http://www.Lrc-tnu.edu.vn
LI CM N

Ti xin by t lng bit n su sc n GS.TS. Trn T Hiu Trng
i hc khoa hc t nhin i hc quc gia H Ni, tn tnh hng dn,
gip ti trong sut qu trnh lm lun vn
Ti xin chn thnh cm n ThS Trn Thu Qunh khoa Ho trng
i hc bch khoa H Ni nhit tnh gip ti trong qu trnh lm
th nghim v c nhng kin ng gp qu bu gip ti hon thnh
lun vn.
Ti xin gi li cm n chn thnh ti cc thy c gio trong khoa
Ho hc trng i hc S Phm Thi Nguyn cng cc bn ng
nghip gip ti hon thnh bn lun vn ny.
Thi nguyn ngy 25 thng 9 nm 2009
Hc vin


Phm Th Hng Thi
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MC LC

M U ...................................................................................................... 1
Chng I. TNG QUAN ............................................................................. 3
1.1. Gii thiu v nguyn t iot ...................................................................... 3
1.1.1. Trng thi t nhin ca nguyn t Iot [ 1],[1

] ................................. 3
1.1.2. Mt s tnh cht vt l v ha hc ca Iot [1] .................................. 4
1.1.3. Vai tr ca Iot i vi sinh ha ngi [1],[2] .................................. 6
1.1.4. Tnh trng thiu Iot trn th gii v vit nam ............................... 8
1.2. Cc phng php tch v lm giu (sc k-chit) ................................. 10
1.2.1. Cc phng php sc k ................................................................ 10
1.2.1.1. Sc k bn mng ..................................................................... 11
1.2.1.2. Sc k kh ............................................................................... 12
1.2.1.3. Sc k lng hiu nng cao (HPLC) ......................................... 13
1.2.2. Phng php chit ......................................................................... 14
1.3. Mt s phng php nh lng iot ...................................................... 18
1.3.1. Phng php chun [16] ........................................................... 18
13.2. Phng php o ph hp th phn t (Phng php UV-VIS) ...... 18
1.3.3. Phng php quang ph pht x nguyn t plasma (ICP - AES)
v ph khi plasma (ICP - MS) ...................................................... 20
1.3.4. Phng php in ho ................................................................... 20
1.3.4.1. Phng php in cc chn lc ion [24] ................................. 20
1.3.4.3. Phng php cc ph dng xoay chiu (AC) .......................... 21
1.3.4.4. Phng php Von - ampe ho tan [25] .................................... 21
1.3.5. Phng php kch hot ntron (NAA) [26] ................................... 22
1.4. Mt s k thut v c ho mu xc nh iot ..................................... 22
1.4.1. K thut v c ho t .................................................................. 22
1.4.2. K thut v c ho bng l vi sng [28] ........................................ 23
1.4.3. K thut v c ho kh [28] .......................................................... 23
1.5. Kt lun phn tng quan........................................................................ 24
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Chng 2. THC NGHIM ..................................................................... 25
2.1. Dng c v thit b ................................................................................ 25
2.3. Qu trnh thc nghim .......................................................................... 27
2.3.1. Gii thiu v Fucsin baz .............................................................. 27
2.3.2. C ch tng tc gia I
2
vi cc cht mu baz hu c. ............... 27
2.3.3. Cc thc nghim kho st .............................................................. 28
2.3.3.1. nh hng ca pH n s chit ca Fucsin baz bng
cc dung mi hu c. ............................................................ 28
2.3.3.2. nh hng pH ca mi trng n s hnh thnh hp
cht lin hp ion gia fucsin baz v iot. .............................. 28
2.3.3.3. Kho st ph hp th ca hp cht fucsin baz - iot ............... 29
2.3.3.4. Kho st s ph thuc hp th quang A vo lng
dung dch HCl 2M ................................................................. 29
2.3.3.5. Kho st s ph thuc lng dung dch NaNO
2
0,1M ............ 30
2.3.3.6. nh hng ca lng thuc th fucsin baz. ......................... 30
2.3.3.7. Kho st s ph thuc hp th quang ca hp cht
mu theo thi gian. ................................................................ 31
Chng 3. KT QU TH NGHIM V BN LUN ........................... 32
3.1. Kho st nh hng ca ph n s chit thuc th fucsin baz
bng cc dung mi .......................................................................... 32
3.2. Kho st nh hng ph ca mi trng nc n s hnh thnh
hp cht mu lin hp gia fucsin baz vi iot ............................... 34
3.3. Ph hp th ca hp cht mu fucsin baz - iot .................................... 35
3.4. Kho st nh hng ca lng axit hcl ln phn ng ............................ 36
3.5. Kho st s ph thuc ca lng cht oxi ho NaNO
2
0,1M ...................... 37
3.6. nh hng ca lng thuc th ............................................................ 38
3.7. Kho st s ph thuc hp th quang ca hp cht mu theo thi gian ....... 38
3.9. Lp ng chun .................................................................................. 39
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3.10. Kho st nh hng ca mt s nguyn t. ......................................... 43
3.11. p dng nhng kt qu nghin cu c phn tch mt s
mu mi trng: t, nc, trng. ................................................. 45
3.11.1. Phn tch iot trong t. .................................................................. 45
3.11.2. Phn tch iot trong nc................................................................ 48
3.11.3. Phn tch iot trong trng ............................................................... 49
3.12. Cc quy trnh phn tch iot trong cc mu mi trng t, nc, trng. ...... 50
3.12.1. Quy trnh phn tch iot trong mu t ........................................... 50
3.12.2. Quy trnh phn tch iot trong nc ................................................ 51
3.12.3.Quy trnh phn tch iot trong trng ................................................ 51
KT LUN ................................................................................................ 60
TI LIU THAM KHO ......................................................................... 62


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DANH MC CC BNG

Bng 1.1: c im v cc hng s vt l ca Iot ....................................... 5
Bng 1.2: S phn b hm lng iot trong mi trng t nc v
khng kh [7] .............................................................................. 8
Bng 1.3: Phn loi mc ri lon thiu Iot ........................................... 10
Bng 3.1: Gi tr A ca dch chit Fucsin Baz bng CHCl
3
cc pH
khc nhau ca dung dch nc .................................................. 32
Bng 3.2: Gi tr A ca dch chit fucsin baz bng CH
2
Cl
2
cc pH
khc nhau ca dung dch nc .................................................. 33
Bng 3.3: Gi tr A ca dch chit fucsin baz bng 1,2 - dicloetan
(C
2
H
4
Cl
2
) cc gi tr pH khc nhau ca dung dch nc......... 33
Bng 3.4: Gi tr A ca dch chit hp cht mu Fucsin baz - Iot
trong Clorofom cc pH khc nhau trong mi trng nc ..... 34
Bng 3.5: Gi tr A ca dch chit hp cht mu lin hp Fucsin baz -
Iot trong diclometan t mi trng nc cc gi tr pH
khc nhau .................................................................................. 35
Bng 3.6: Gi tr A ca dch chit hp cht mu lin hp Fucsin
baz - iot trong 1, 2 - dicloetan cc pH khc nhau ca
mi trng nc ...................................................................... 35
Bng 3.7: S ph thuc hp th quang (A) vo nng HCl ............... 37
Bng 3.8: Gi tr A ca dch chit hp cht mu Fucsin baz - iot bng
1,2 - dicloetan ph thuc vo lng cht oxi ho NaNO
2
.......... 37
Bng 3.9: Kt qu kho st nh hng ca lng thuc th Fucsin
baz .......................................................................................... 38
Bng 3.10: S ph thuc gi tr A vo nng iot ...................................... 40
Bng 3.11: S ph thuc gi tr A vo nng iot ...................................... 41
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Bng 3.12: Kt qu kho st nh hng ca Br
-
.......................................... 44
Bng 3.13: Kt qu kho st nh hng ca

3
ClO ....................................... 44
Bng 3.14: Kt qu kho st nh hng ca Cl
-
........................................... 45
Bng 3.15: Kt qu kho st nh hng ca CN
-
........................................ 45
Bng 3.16: Kt qu kho st nh hng ca S
2-
.......................................... 45
Bng 3.17: Kt qu kho st nh hng ca Fe
3+
........................................ 45
Bng 3.18: Kt qu xc nh iot khi x l mu bng phng php kim
chy, phng php ha tan bng Axit ....................................... 47
Bng 3.19: Kt qu xc nh iot trong mu nc khi c cn mu v khi
x l bng HNO
3
37% .............................................................. 48
Bng 3.20: Kt qu phn tch iot di ng trong mu t.............................. 51
Bng 3.21: Kt qu phn tch iot trong mu nc ....................................... 52
Bng 3.22: Kt qu phn tch iot trong mu trng vt .................................. 52
Bng 3.23: Kt qu phn tch iot trong cc mu t i Thi Nguyn ....... 53
Bng 3.24: Kt qu phn tch iot trong cc mu t vn v t rung
H Ni v Thi Nguyn ......................................................... 54
Bng 3.25: Kt qu phn tch iot trong mt s mu nc khu vc
Thi Nguyn v H Ni ............................................................ 55
Bng 3.26: Kt qu phn tch iot trong mt s mu trng H Ni ............ 57
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DANH MC CC HNH

Hnh 3.1: Ph hp th ca hp cht mu Fucsin baz - iot cc nng
iot khc nhau c chit bng diclometan. ........................... 36
Hnh 3.2: nh hng ca thi gian n bn mu ca hp cht mu
lin hp Fucsin -baz -iot (dung mi chit l CHCl
3
) ................ 39
Hnh 3.3: ng chun xc nh iot bng thuc th fucsin baz ............... 40
Hnh 3.4: ng chun xc nh iot bng thuc th fucsin baz ............... 41
Hnh 3.5: ng chun xc nh iot bng phng php thm ................... 43




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1
M U

Cc nguyn t vi lng c vai tr quan trng i vi sc khe con
ngi, chng c trong thnh phn ca cc enzym, iu khin s hot ng ca
cc c th sng, cho nn cc nguyn t vi lng khng nhng duy tr s sng
m cn m bo cho s pht trin ca con ngi c v th cht ln tr tu.
Iot l nguyn t vi lng rt cn cho s pht trin ca c th nh qu
trnh tng hp hocmon tuyn gip, duy tr thn nhit, pht trin xng, qu
trnh bit ha v pht trin ca no cng nh h thn kinh ca bo thai.
Thiu iot s gy hin tng tuyn gip khng lng hocmon cn
thit, dn n nng hocmon trong mu thp gy tn thng no v cc c
quan khc trong c th. Hin tng ny c gi l ri lon Thiu iot.
Theo thng k ca t chc y t th gii (WHO). Hin ti trn ton cu c
khong 1,5 t ngi sng trong cc vng thiu iot v c nguy c mc cc
chng bnh thiu iot, trong c hn 20 triu ngi mc chng bnh n n.
Vit Nam cng nm trong vng thiu iot. theo s liu iu tra quc gia
v tnh trng thiu Iot nm 1992 cho thy c ti 84% dn s Vit Nam trong
tnh trng thiu iot: trong 16% thiu nng, 45% thiu va v 23% thiu
nh, khong 10% tr em nc ta b bnh bu c.
Mi trng (kh quyn, thy quyn, a quyn) v lng thc, thc
phm l ngun cung cp Iot cho con ngi.
Hng ngy khu phn iot a vo c th di 100g th s xy ra hin
tng thiu iot. Bu c v cc bnh ri lon do thiu iot l nhng bnh nan
gii. Gii php phng chng hin tng ri lon thiu iot l trn ln iot vo
mui n cho nhn dn dng hng ngy. i vi nhng bnh nhn nng dng
mui iot khng t c kt qu mong mun, ngi ta phi iu tr bng bin
php tch cc hn nh tim hay cho ung du thc vt c gn iot (Lipiodol)
hoc cc vin nn c hm lng iot cao theo ch nh ca bc s iu tr.

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2
Khi phn tch mi trng hay cc ngun nc, lng thc v thc
phm ca mt vng a l, ngi ta thy hm lng ca iot trong cc i
tng ny c lin quan n t l nhng ngi mc bnh bu c.
Bnh bu c sinh ra khng phi ch do hm lng iot trong cc i
tng khng kh, nc ung, lng thc v thc phm thp m cn do cc
yu t vi lng khc na. Chng hn hm lng canxi trong t, trong nc
qu cao, do tp qun sinh hot n ung ca cc dn tc, do c a ca tng
ngi v.v V th cho nn mt s ni mc d hm lng iot trong lng
thc, thc phm cao nh: Hi Phng, Thi Bnh vn c t l ngi mc
bnh bu c ng k.
nh gi vi lng iot trong t, nc, lng thc v thc phm cn
phi nghin cu tm c phng php phn tch c nhy, lp li v
chnh xc cao, nh cc phng php phn tch quang hc hin i (AAS,
AES,) phng php ng hc xc tc, phng php in ha hin i (Von
-ampe ha tan, hp ph,) phng php sc k lng hiu nng cao (HPLC),
phng php phng x, phng php kch hot Ntron.
Song cc phng php ny i hi phi c thit b chuyn dng, t
tin, cha ph hp vi a s cc phng th nghim hin c nc ta.
Xut pht t nhng l do trn, trong lun vn ny chng ti t cho
mnh nhim v nghin cu tm mt phng php phn tch iot n gin c
th p dng cho cc phng th nghim c s, l phng php trc quang
UV-VIS da trn phn ng to phc mu ca iot vi mt thuc th hu c.
tng nhy ca phng php chng ti s kt hp vi phng php chit
tch v lm giu iot ng thi loi tr nh hng ca lng thuc th d.

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3
Chng I
TNG QUAN

1.1. GII THIU V NGUYN T IOT
1.1.1. Trng thi t nhin ca nguyn t Iot [1], [1

]
Nguyn nhn con ngi mc bnh thiu ht iot l do mi trng thiu
iot. Qu trnh chuyn ho iot t mi trng vo ngi l qua ng thc n,
nc ung. Chu trnh c m t bng s sau:




















Con ng- i
Vt nui Cy trng
t N- c

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4
Nh vy c th khng nh mt iu l t vng no giu iot th
nc vng cng c hm lng iot cao, cy trng vt nui nhng
vng cng cha hm lng iot cao. Cui cng con ngi s dng ngun
nc, lng thc, thc phm c hm lng iot cao th s trnh c s
thiu ht iot.
Iot tn Hy Lp Iodes, ngha l tm, sau ny hip hi quc t v ha l
thuyt v ng dng gi l Iodine, l nguyn t ha hc, k hiu l I, nguyn
t s l 53.
Iot l nguyn t vi lng rt cn cho s sng ca cc sinh vt.
Iot l nguyn t t hot ng nht, c m in thp nht trong cc
halogen. Ging nh cc nguyn t nhm VIIA (h halogen), iot t do thng
dng phn t c cng thc I
2
.
Iot c th thu c dng tinh khit bng cch un nng hn hp KI
vi CuSO
4
. Iot c th iu ch t ngun to b, rong bin v mt s loi cy
khc, do chng c kh nng hp th v tch t iot trong c th. iu ch iot
t ngun nguyn liu ny, ngi ta ly rong bin kh, t thnh tro ri ha
tan tro vo nc. sau lc ly dung dch, c dung dch n khi mui kt tinh
lng xung (mui kt tinh l cc mui clorua, sunfat). Gn ly phn nc
trong (c mui ca iot). Dng kh clo hay MnO
2
v H
2
SO
4
oxi ha I
-
trong
dung dch thnh I
2
.Cho I
2
thng hoa ta s thu c iot. Ngun nguyn liu
chnh iu ch I
2
l nc ging khoan du m.
Hi iot gy kh chu cho mt v mng nhy, khi tip xc vi thi gian
ko di = 8 gi trong bu khng kh c nng I
2
1mg/m
3
.
Khi thao tc nu dy iot vo da c th gy bng.
1.1.2. Mt s tnh cht vt l v ha hc ca Iot [1]
Iot tinh khit c mu tm xm. iot c tnh thng hoa, hi iot c mu tm,
mi kh chu v gp lnh s kt tinh li (khng qua th lng).

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5
Bng 1.1. Trnh by mt s c im v cc hng s vt l ca Iot.
Bng 1.1: c im v cc hng s vt l ca Iot
Tinh th Iot Cu to trc giao
Tnh cht vt l
Trng thi Rn
im nng chy 113,7 K (236,66
0
F)
im si 184,3

K (363,7
0
F)
Th tch phn t 1.10
- 6
m
3
/mol
Nhit bay hi (I
2
) 41,57 kJ/mol
Nhit nng chy (I
2
) 15,52 kJ/mol
m in 2,66 (thang Pauling)
Nhit dung ring 54,41J/ kgK ( 25
0
C)
dn in 1,310
7
O/mk
dn nhit 449W/mk (300
0
K)
I
2
khng c T tnh
Nng lng ion ho 1. 1008,4 kJ/mol
2. 1845,9 kJ/mol
3. 3180 kJ/mol
Cc ng v n nh nht ca iot
ISO Thi gian bn r DM DE (Mev) DP
127
I ~ 100% Rt n nh
129
I Tng hp 1,57.10
7
nm | - 0,194
129
Xe
131
I Tng hp 8,0207 ngy | - 0,194
131
Xe
128
I Tng hp 25 pht


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6
Iot cng ging nh Cl
2
, Br
2
n c th to nhiu hp cht vi cc
nguyn t ha hc, nhng n t hot ng hn so vi cc nguyn t khc
trong nhm VIIA v iot c tnh cht hi ging vi kim loi.
Iot tan trong cc dung mi hu c: Nu dung mi hu c l cc hp
cht khng cha oxi nh CHCl
3
, CCl
4
, CS
2
, C
6
H
6
, etxng... to thnh dung
dch mu tm; nu dung mi hu c trong phn t c cha oxi nh ru, te,
xton... to thnh dung dch mu nu.
Iot ha tan t trong nc ( 25
o
C tan ca I
2
trong nc l 0,34 g I
2
/l)
to ra dung dch mu vng. Iot tan nhiu trong dung dch nc c cha I
-
v
c phn ng I
2
+I
-
= I
3
-
, dung dch I
3
-
c mu nu v c tnh cht ca mt hn
hp gm I
2
v I
-
.
Iot c phn ng vi dung dch tinh bt long to dung dch mu xanh,
mu xanh s bin mt khi un nng dung dch, nhng ngui mu xanh s
xut hin tr li. dung dch tinh bt long c dng lm ch th nhn bit
v chun iot
Hp cht ca iot thng gp l cc mui natri v kali: NaI, KI,
NaIO
3
, KIO
3
,...
1.1.3. Vai tr ca Iot i vi sinh ha ngi [1],[2]
i vi con ngi iot l nguyn t vi lng cc k quan trng. Trong
c th ngi, iot ch chim 4.10
-5
% trng lng c th (15-23mg), nhng n
ng vai tr quan trng cho s pht trin ca c th c v th cht ln tr tu.
Trn 75% iot trong c th tp trung tuyn gip, phn cn li c phn b
trong cc m tuyn v, dch tiu ha, thn, nc bt. Iot tn ti dng I
-
hoc
gn vi protein vn chuyn lu thng trong c th.
Chc nng quan trng nht ca iot l tham gia to hocmon T3 (triiotothyronin)
v T4 (thyroxin). Hocmon tuyn gip ng vai tr quan trng trong vic iu
ha pht trin c th, hot ng ca hocmon tuyn gip rt cn cho s pht

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7
trin bnh thng ca no, lm tng qu trnh bit ha ca t bo no v tham
gia vo chc nng ca no b. Chnh v vy cc hocmon tuyn gip T3 v T4
rt cn cho s pht trin chc nng ca no v h thng thn kinh. Khng
iot to hocmon tuyn gip s gy ra ri lon ni tit, cc ri lon ny c
biu hin thnh cc chng bnh n n, thiu nng tuyn gip v bnh bu
c [3], [4], [5], [6].
Bnh n n xy ra trong qu trnh pht trin ca bo thai, thiu iot
gy ra hin tng sy thai lin tip, thai cht lu hoc a tr sinh ra b n
n do no b tn thng vnh vin, thn kinh, tr tu v th cht chm pht
trin, c th gy ra cm, ic, ln, kh nng t duy hc tp km v.v...
Thiu nng tuyn gip do c th khng nhn hocmon tuyn gip do
lng hocmon tuyn gip trong mu thp, sinh ra bnh vi nhng biu hin
chm chp, l , bun ng, da kh v to bn.
Bnh bu c l hin tng tuyn gip to hn bnh thng, lng
hocmon tuyn gip trong mu thp, sinh ra nhiu hocmon kch thch tuyn
gip lm cho tuyn gip phnh to thnh bu.
Theo khuyn ngh ca t chc y t mi ngy ngi trng thnh cn
150g iot, ph n c thai 175g, ph n cho con b 200g. Liu lng ln
ti 1000 g iot/ ngy c th coi l an ton.
Iot c trong thc phm tn ti nhiu dng khc nhau nh: I
-
, dng iot
v c t do, dng hu c...
Iot c dng lm thuc kh trng, dung dch iot trong cn c nng
3% dng kh trng vt thng.
Cc ng v ca iot c s dng nhiu trong ha hu c, ngnh y.
ng v
128
I dng trong y t to nh v xt nghim hot ng ca tuyn
gip, ng v
131
I c dng iu tr ung th tuyn gip.

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8
1.1.4. Tnh trng thiu Iot trn th gii v Vit Nam
Trong mi trng iot phn b khng ng u. Hm lng gn ng
ca iot trong cc thnh phn mi trng c trnh by trong bng 1.2.
Bng 1.2: S phn b hm lng iot trong mi trng t nc
v khng kh [7]
Mi trng Nng (ppm) %I
Khng kh 0,002 2.10
-8
- 2.10
-7

Nc sng 0,001 10
- 7
Nc bin 0,01 10
-6
- 10
-5
Than bn 3,4 3,4.10
-4

t 1,8 1,8. 10
-4
Khong 0,3 3.10
-5

Nhng khu vc t lin cng xa i dng cng c nguy c thiu ht iot
ln. S thiu ht iot nghim trng xy ra trn min ni cao, cng c khi xy
ra vng hay b l lt hoc ng bng c cc sng ln.
Vng tun hon ca iot trong mi trng c th m t nh sau: iot d b
ra tri t t i vo cc ngun nc ri ra bin. T nc bin iot theo nc
bc hi i vo khng kh. Mt phn iot c tr li t, nc theo ma,
lng iot c b sung theo ma khng , v vy t v nc nhiu vng
lun thiu iot, c bit l cc vng ni cao. Cc sn phm nng nghip nh
lng thc, thc phm, cc gia sc chn nui... cc vng ny cng mang
du n thiu iot. Con ngi sinh sng bng cc loi sn phm cng chu
hu qu thiu iot, mc chng bnh chung l bu c.
* Trn th gii, theo nh gi ca WHO v UNICEF c khong 29%
dn s th gii (1570 triu ngi) c nguy c thiu iot, trong t nht c 655
triu ngi b tn thng no; 11,2 triu ngi b n n [8], [9].

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9
Hin nay c 110 nc c vn thiu iot cc vng M La tinh,
Chu u, vng Andit v Himalaya ni m iot b si mn bi ma v bng.
Ti Trung Quc nm 1978 c lng ti 80% ngi dn mc bnh bu
c, 11% b n n. Ti vng ni Jawa (indonexia) lng iot trung bnh thp,
c ti 70% ngi b mc bnh bu c (1972).



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10
* Vit Nam s thiu ht iot mc trm trng. Nm 1993, UNICEF
v bnh vin ni tit trung ng tin hnh kho st ti mt s im ngu
nhin trn ton quc bng cch khm bu c v xc nh lng iot niu,
kt qu cho thy 94% dn s b thiu iot [10]. Cng theo s liu ca
UNICEF [11] nm 1993 v t l bu c v lng iot niu c thng k
trn bn .
A
=
T l bu c (%)
B Iot niu (g/dl)

Da theo kt qu kho st cho thy, cc tnh Lao Cai, Sn La, Cao Bng,
Yn Bi, Ngh An l nhng tnh c s ngi mc bnh bu c cao. nh gi
mc thiu iot theo iot niu c trnh by trong bng 1.3.
Bng 1.3: Phn loi mc ri lon thiu Iot
Iot niu (g / dl)
Mc ri lon thiu iot
< 2 Nng
2 - 4,9 Trung bnh
5 - 9,9 Nh
> 10

1.2. CC PHNG PHP TCH V LM GIU (SC K - CHIT)
1.2.1. Cc phng php sc k
Nguyn tc ca phng php sc k [12] l qu trnh tch lin tc tng
phn hn hp cc cht do s phn b khng ng u ca chng gia pha tnh
v pha ng khi cho pha ng i xuyn qua pha tnh.
Cht lng v hiu qu tch c biu din bng phng trnh Van-
Demter, chiu cao a l thuyt ca mt ct H ph thuc vo tc pha ng.

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11
CU
U
B
A H + + =

Trong : A: H s khuych tn xoy ca cc phn t cht
B: H s khuych tn phn t
C: Tc trao i gia 2 pha
U: Tc tuyn tnh ca pha ng
Chiu cao H cng nh th hiu qu tch cng ln. Tng s a l thuyt
ca mt ct tch n c tnh bng chiu di l ca ct (c nh) chia cho chiu
cao a l thuyt H.
=
l
n
H

Phng php sc k c phn chia nh sau:
- Theo c ch tch (hp ph, phn b, trao i ion)
- Theo s phn loi cc pha trong sc k (lng - lng, lng - kh, lng - rn).
- Theo cng c s dng tin hnh (sc k bn mng, sc k kh, sc
k lng hiu nng cao).
1.2.1.1. Sc k bn mng
Qu trnh tch hp cht bng sc k bn mng xy ra khi cho pha ng
di chuyn qua pha tnh. Cht hp ph trong pha tnh sc k bn mng c
ri thnh mt lp mng trn tm knh hoc tm kim loi. Cc cu t c
dch chuyn trn lp mng theo hng pha ng vi tc khc nhau. Kt
qu thu c mt sc trn lp mng [12].
Cc i lng c trng cho sc k lp mng l:
* H s di chuyn R
f
: l t s ca khong cch t tuyn xut pht ti
tm vt sc k (I) v khong cch t tuyn xut pht ti tuyn dung mi (I
o
):
0
=
f
I
R
I
O sR s 1

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12
Gi tr R
f
c trng cho s tng tc gia hot cht - dung mi -
cht hp th. nh gi kh nng tch cc vt trn sc ta dng 2 i
lng sau:
+ AR
f
l hiu gi tr R
f
ca 2 cu t ln cn nhau.
+ K l h s tch c tnh bng t s h s phn b ca 2 cu t A
(K
A
) v B (K
B
):
A
B
K
K
K
=
* Cht hp ph (pha tnh) c s dng trong sc k bn mng gm
silicagen, oxit nhm, xenlul, tinh bt, nha trao i ion.
* Dung mi (pha ng) dng chy sc k bn mng, thng l dung
mi hu c hay hn hp dung mi hu c, chng hn nh heptan; CHCl
3

hoc hn hp heptan - clorofom, propanol - CHCl
3
- benzylamin [13], [14].
nc ta sc k bn mng c p dng nhiu trong phn tch mi
trng, nhng cha c cng trnh no p dng cho vic tch iot [13].
Trn th gii, phng php sc k lp mng c p dng trong
nhiu lnh vc nghin cu, v cng c s dng trong phn tch iot [13].
1.2.1.2. Sc k kh
L qu trnh tch cc cht trong ct tch trng thi kh, cht mang
mu l cht kh. V vy ch c th tch c hn hp cc kh, nu l hn hp
cht lng hay cht rn th phi ho kh . Thng ch tch c cc cht rn
d ho kh ( = 250
0
C) [12]. Trong sc k kh, pha tnh l cht rn, cn pha
ng l mt cht kh hay hn hp kh. Cht kh ny mang kh cn phn tch
vo ct thc hin qu trnh tch, n chuyn ng lin tc trong sut qu
trnh tch vi tc xc nh. Pha tnh ng vai tr chnh trong vic to nn
tng tc cn thit tch cc cu t khi nhau. S thay i pha tnh v cc

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13
thng s lm vic s nh hng n tng tc gia kh mang, cht mang rn
v cu t cn tch. Kh mang dng trong sc k thng l N
2
, H
2,
He
phn tch lng vt, kh mang phi tinh khit (99,99%). Vt liu lm ct trong
sc k kh c th lm bng kim loi hay thu tinh.
Phng php sc k kh l mt trong nhng phng php hin nay
c s dng nhiu trong phn tch mi trng, n c thi gian phn tch
nhanh, nhy cao, hiu qu tt. Bonner v cc cng s dng mui grafit
c din tch b mt ring 100m
2
/g lm cht nhi ct. Dng ct ny pht hin
c cc kh c c cha lu hunh nh: SO
2
, H
2
S, (CH
3
)
2
Svi hm lng
ch my chc ppb.
Phng php sc k kh cng c dng xc nh thnh phn du
m v cc sn phm ca chng. Ngoi ra cng c dng phn tch lng
thc, thc phm, cc loi dc phm.v.v...
1.2.1.3. Sc k lng hiu nng cao (HPLC)
Phng php ny dng cc cht nhi ct nh mn, ct cng c kch c
nh nn thc hin qu trnh tch, phi dng p xut cao y cht lng
qua ct. Chnh nhng iu kin lm cho phng php ny c nhiu u
im hn so vi sc k lng c in l tc nhanh, tch tt, nhy
cao (v d dng detector UV - VIS th nhy t 10
-9
g, dng detector hunh
quang, in ho t 10
-12
g) ct tch dng c nhiu ln, mu thu li d v
khng b ph hu [12], [15].
HPLC c s dng rt rng ri phn tch nhiu i tng khc
nhau. HPLC c kh nng tch c c cc hp cht.
+ Cc hp cht cao phn t, ion thuc cc i tng sinh hc, y hc
+ Cc hp cht khng bn
+ Cc hp cht d n, km bn nhit, v.v

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14
Phng php HPLC l mt trong nhng phng php tch, xc nh iot
v cc nguyn t halogen tt nht trong cc phng php phn tch hin i,
t nhy, chnh xc cao, c th xc nh nhiu cht trong cng mt mu.
1.2.2. Phng php chit
Hm lng iot trong t, nc, lng thc, thc phm ni chung rt
thp c ppb - ppm, v vy ngi ta thng dng phng php chit lm
giu, tng nhy, chn lc v chnh xc ca php xc nh.
Nguyn tc ca phng php chit da trn s tch cht bng cc dung
mi hu c, do tan ca cht trong cc dung mi khc nhau. Nu ho tan
cht A vo 2 dung mi khng trn ln (thng l nc - nc v dung mi hu
c - hc), khi cn bng nng cht A trong 2 dung mi s tun theo nh lut
phn b Nerst: mt p xut v nhit nht nh, nu cht tan A khng
phn li hoc lin hp trong 2 dung mi th t s nng cht tan trong 2 dung
mi l mt hng s (gi l hng s phn b D
0
).
| |
| |
hc
o
nc
A
D
A
=
Trong [A]
nc
, [A]
hc
l nng cn bng ca cht A trong pha nc
v pha hu c. D
0
cng ln th cht chuyn vo pha hu c cng nhiu. Mt
cch chnh xc.
nc
hc
A
A
o
a
a
D =

a
Ahc
, a
Anc
l hot ca cht A trong tng hu c v tng nc.
Ngoi hng s phn b D
0
, ngi ta cn dng khi nim chit R.
chit R c xc nh bng t s gia khi lng G ca cht chit
A so vi khi lng ban u G ca n.

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15
'
o
o
G D
%R 100% 100%
G D r
= =
+

Trong :
nc
hc
V
r
V
= ; V
nc
v V
hc
l th tch pha nc v pha hu c (ml)
Ngi ta chia cht chit A ra lm cc loi sau:
* Cht chit A khng in ly, khi s phn b A vo 2 tng:
A
nc
A
hc

trng thi cn bng, hng s phn b v chit c tnh theo cc
cng thc n gin trn.
* Cht chit A l cht in li
Khi cht chit A l cht in ly v d A l mt axit yu, qu trnh phn
b tr nn phc tp v phng trnh cn bng gia 2 pha:
HA
nc
HA
hc
H
+
+ A
-

| |
+
( (

=
nc
H A
Ka
HA
(hng s phn ly ca axit)
| |
| |
0
=
hc
nc
HA
D
HA
;
+
0
100
1
r
[H ]
D
=
+
a
R
K

H s phn b trong trng hp ny l t s nng tt c cc dng
trong pha hu c v tt c cc dng trong pha nc.
hc 0
nc
+
[HA]
[HA] [A]
1
[H ]
= =
+
+
a
D
D
K

Nu [H+ ] >> ka th Ka/[H+] = 0 khi D = D
0
Tng t nh vy khi A l mt baz yu ta cng tnh c D v R ca
dung dch kim.

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16
* Chit cht lng tnh
Hng s phn b v chit ca cht in ly lng tnh ph thuc
vo pH kh phc tp v cht in li lng tnh s tn ti nhiu dng trong
c 2 pha.
Khi trng thi cn bng, khi lng G ca cht in ly lng tnh A l:
G = E [A
y
x
]
hc
. V
hc
+ E [A
y
x
]
nc
. V
nc

y
x hc hc
(A ) .V
R
G
=


Hng s phn b D s c tnh theo phn li v tn ti c th tng
cht gia 2 pha.
* Chit tp hp lin hp ion
Vic chit lin hp ion ch xy ra pH xc nh v tp hp ion ch c
kh nng thc hin pH m ti cc thnh phn (tc axit hay baz) ng
thi tn ti.
m bo chit tt, cht b chit phi b solvat ho yu bi cc phn
t H
2
O

v tan tt trong dung mi chit.
Cht b chit l lin hp ion th n b chit cng tt nu nhng cation v
anion trong thnh phn cng k nc.
Nhng lin hp ion to bi mt cation v mt anion v c bit l ion
mt in tch lun b chit tt hn nhng lin hp ion c thnh phn khc.
Bng tnh ton ngi ta thy c th chit cc ion v c mt cch thun
li bng cch cho n lin kt vi cc phi t hu c to thnh nhng tp
hp ion m trn mi n v in tch c khong 10-15 nguyn t cabon.
Ngi ta chia chit lin hp ion thnh my loi sau:

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17






























































(
(
(
(

(
N
N
Co
2
+

SCN
-

2
SbCl
6

_

(
(
(
(

(
+
N(C
2
H
5
)
2
(C
2
H
5
)
2
N
+

(
(
(
(

(
Nguyn
t
c mu
Phi
t
Anion
v c
khng
mu
(1)
Nguyn t
khng mu
Phi
t
Anion
hu c
c mu
(2)
Nguyn
t

Thuc th
hu c
c
gc SO
3
-

Cation
hu c

(3)
Anion phc
ca
Kim loi

Cation
hu c

(4)
Co
2
SO
3
O
O=N
SO
3
_
_
+
N








(
(
(
(

(

(
(
(
(

(
_
N
O
I
I
Er
4
+







(
(
(
(

(
COOC
2
H
5
HN NH
O

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18
Phn ng to lin hp ion l c s ca cc phng php trc quang,
chit trc quang, hunh quang xc nh nhiu kim loi. Ni chung cc lin
hp ion thng c h s hp th mol tng i ln nn rt nhy v vy cho
php xc nh lng rt nh cc cht.
1.3. MT S PHNG PHP NH LNG IOT
1.3.1. Phng php chun [16]
Nguyn tc chung ca phng php ny l chuyn tt c cc dng ca
iot c trong mu phn tch v dng I
-
, sau dng iodat IO
-
3
oxi ho I
-
v
dng I
2
, chun lng I
2
gii phng bng dung dch chun Na
2
S
2
O
3
vi ch
th h tinh bt.
5KI + KIO
3
+ 3H
2
SO
4
= 3I
2
+ 3K
2
SO
4
+ 3H
2
O
I
2
+ 2Na
2
S
2
O
3
= 2NaI + Na
2
S
4
O
6

Phng php ny c nhy thp, ch dng phn tch iot vi hm
lng ln 5 - 50mg.
u im ca phng php ny l d thao tc, khng cn my mc t
tin, nhanh. Zhao Guiging v cng s [17] lp h thng chun t ng;
ghp ni vi my tnh, tm cch chun Cl
-
, Br
-
,

I
-
trong nc t nhy
v lp li cao.
1.3.2. Phng php o ph hp th phn t (Phng php UV-VIS)
Nguyn tc ca phng php ny l chuyn cc dng iot c trong mu
phn tch v dng I
-
, sau dng NaNO
2
oxi ho I
-
thnh I
2
, chit I
2
sinh ra
bng CCl
4
, toluen, sau o hp th quang ca dung dch
max
=
657nm. Bng phng php chit ny lm tng nhy ln n 10
-6
mol/l.
[18] Bulinski R v cng s [19] dng N- N di (|- Hidroxipropyl) - o -
phenylene diamin xc nh iot trong sa v trong kh, phng php ny c
nhy c ppm v hng chc ppb. Salinao F v cng s [20] dng 2-

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19
oximiodimedone v dithiosemicacbazon lm thuc th xc nh IO
-
3
v
BrO
3
-
; o bc sng 400nm, phng php xc nh c 0,24 - 5g IO
3
-
/ml
v 0,16 - 3,6g BrO
-
3
/ml.
Cc bo v mi trng v hip hi bo v sc kho Hoa K xc
nh I
-
bng cch dng KHSO
5
oxi ho chn lc thnh I
2
, I
2
sinh ra cho phn
ng vi 4, 4,4 - metyliclynetris (N-N-dimetylanilin) (thng gi l thuc
th Leueo Crystal Violet- khng mu) to thnh hp cht mu tm m.
Phng php ny c dng lm phng php tiu chun xc nh iot.
Phc hp th cc i = 592nm v khong tun theo nh lut Lambert-
beer l 50 - 600 g/l
xc nh vi lng iot ngi ta thng dng phng php trc quang
ng hc xc tc da trn phn ng oxi ho kh gia Ce (IV) v As (III)
trong mi trng axit. [21]
Ce (IV) + As (III)
2 4
I
H SO
Ce (III) + As (V)
(mu da cam) (khng mu) (khng mu) (khng mu)
Hm lng iot trong mu c xc nh bng s gim hp th quang.
( = 370nm) AA ca dung dch trc v sau phn ng vi thi gian c
nh, khi c mt cht xc tc l iot, AA t l vi nng ca iot trong dung dch.
Ngi ta cng da vo phn ng gia clopromazin vi H
2
O
2
[22]. Khi
c mt iot to ra sn phm trung gian c mu , bn trong mi trng axit v
hp th cc i ti = 525nm. Tc phn ng t l vi nng I
-
trong
dung dch.Phng php ny c u im l xc nh c ring r cc dng
I
-,
IO
-
3
v c s dng rng ri phn tch iot trong mu nc.
Phng php ny t c s dng phn tch iot trong cc i tng lng
thc v thc phm bi v trong cc i tng ny rt phc tp, lm gim hiu
ng xc tc ca iot.


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20
1.3.3. Phng php quang ph pht x nguyn t plasma (ICP - AES) v
ph khi plasma (ICP - MS)
Vi phng php ICP - AES, mu sau khi chuyn thnh dung dch,
c bm trc tip vo ngun kch thch plasma (ICP) c nhit khong
6000
0
C, nhit mu b nguyn t ho hon ton v b kch thch ri
pht ra bc x c bc sng xc nh. o cng bc x (I
px
) ti bc sng
c trng cho nguyn t cn xc nh (l iot), t suy ra hm lng ca iot
c trong mu.
Vi phng php ICP - MS, mu cng c bm trc tip vo ngun
plasma ICP, nguyn t b ion ho, cc dng ion c a vo h phn
tch khi lng tch cc ion da vo t s
m
Z
(m, z l khi lng v in
tch ion). Dng ion sau khi tch c a vo detector chuyn thnh tn
hiu nh lng.
Tc gi [23] dng phng php ICP - MS nh lng iot trong
nc tiu vi khong tuyn tnh 0,1 - 10g I
-
/dl. Phng php ICP - MS cng
nh phng php kch hot ntron (NAA) c xem l phng php chun
vng nh lng vt v siu vt iot
1.3.4. Phng php in ho
1.3.4.1. Phng php in cc chn lc ion [24]
in cc chn lc ion dng trong phng php o th nh lng iot
l in cc mng rn, c ch to t AgI/Ag
2
S, c cu trc nh sau: Ag /
AgCl/KI 0,1M/ mng rn AgI + Ag
2
S / dung dch phn tch / KCl/AgCl/Ag.
Th o c ph thuc vo lg [I
-
]. Phng php ny b Cl
-
v SO
3
2-
cn
tr v vy phi tch cc ion ny khi dung dch trc khi o. Trong qu trnh
o iot, in cc thng b mt mng bao ph nn phi lm sch mng ph
trn in cc.

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21
Phng php ny c dng xc nh iot trong H
2
O. C mt s tc
gi dng xc nh iot trong nc tiu, sa nhng kt qu km chnh xc.
1.3.4.2. Phng php cc ph dng mt chiu (DC)
Trong phng php ny, ngi ta chuyn iot trong mu thnh IO
-
3
sau
ghi cc ph DC ca ion IO
3
-
trong nn NaCl hay KCl. IO
3
-
b kh trn cc
git thu ngn theo phn ng.
IO
3
-
+ 6H
+
+ 6e = I
-
+ 3H
2
O
Qu trnh phn ng in ho c s tham gia ca 6e nn phng php
ny c chnh xc kh cao. Phng php ny cho php xc nh nhng
nng iot c 10
-6
M.
1.3.4.3. Phng php cc ph dng xoay chiu (AC)
Phng php ny da vo tnh thun nghch ca qu trnh oxi ho I
-

thnh I
2.

2I
-
+ 2e I
2

Chiu cao pic t l vi nng I
-
. Dng phng php ng chun v
phng php thm nh lng I
-
.
1.3.4.4. Phng php Von - ampe ho tan [25]
Trong phng php ny, I
-
c tch lu trn b mt in cc git thu
ngn tnh dng Hg
2
I
2
bng mt th in phn trong mt thi gian nht nh.
Sau Hg
2
I
2
tch lu c ho tan bng qut th catot. Qu trnh ho tan in
ho s to pic th - 0,33v (vi in cc so snh l in cc calomen). Chiu
cao ca dng pic ho tan Hg
2
I
2
t l vi nng I
-
trong dung dch. Phng
php ny xc nh c I
-
trong khong 0,13 - 10,2g I
-
/l.
Anion S
2-
cn tr php xc nh, loi tr S
2-
bng cch axit dung dch
S
2-
to thnh H
2
S, ri sc khng kh ui ht H
2
S, sau chnh pH dung
dch v 8 ri mi tin hnh phn tch.

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Phng php Von -ampe ho tan c th xc nh lng nh iot, cho
kt qu nhanh, chnh xc, lp li cao. Song phng php ny khng c
dng phn tch cc mu lng thc v thc phm v nh hng ca nn
qu ln, kt qu phn tch khng chnh xc. Ch yu l dng phn tch I
-

trong nc.
1.3.5. Phng php kch hot ntron (NAA) [26]
Trong phng php ny, ngi ta thng dng ng v phng x ca
iot
128
I c thi gian bn hu ngn (25 pht) phn tch iot.
Nguyn tc ca phng php ny l dng mt chm ntron kch hot
vo mu phn tch v o bc x gama c gii phng bi
128
I. Gii hn pht
hin ca phng php ny khong 91 ppb. Mc d phng php kch hot
ntron c nhy cao, nhng nh hng ca cc nguyn t i km l rt ln
nh
56
Mn,
27
Mg,
24
Na,
28
Al v
43
K.
Cc nguyn t phng x ny cng pht ra mc nng lng nh
128
I.
loi tr nh hng ca cc nguyn t phng x trn, ngi ta thng nghin
cu s dng cc ngun kch hot v thi gian kch hot khc nhau.
1.4. MT S K THUT V C HO MU XC NH IOT
1.4.1. K thut v c ho t
Nguyn tc chung ca k thut ny l dng cc axit mnh, cc axit c
tnh oxi ho mnh, hn hp cc axit hoc hn hp axit c v mt cht oxi
ho phn hu mu.
xc nh iot trong thc phm, tc gi Takashi [27] s dng hn
hp HNO
3
13M + HClO
4
9M + H
2
SO
4
18M un nhit 230
0
C v c
ho mu. Sau iot c xc nh da trn hiu ng xc tc ca phn ng
gia Clopromazin vi H
2
O
2
trong mi trng H
2
SO
4


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23
Phng php v c ho t khng ph hp cho phn tch hng lot
mu v thi gian x l ko di, phi s dng mt lng ln axit nn c nguy
c b nhim bn.
1.4.2. K thut v c ho bng l vi sng [28]
C ch ca s phn hu mu bng l vi sng l s dng nng lng vi
sng un nng dung mi v mu c ng trong bnh kn.
Phn hu mu bng l vi sng, lng axit dng t hn, thi gian phn
hu ngn hn, m bo cht phn tch khng b mt v khng b nhim bn
do mi trng bn ngoi.
1.4.3. K thut v c ho kh [28]
K thut v c ho kh l k thut nung mu trong l nung nhit 450
0
-
750
0
(tu thuc vo bn cht v lin kt tng loi mu m chn nhit thch
hp). Khi nung cc cht hu c c trong mu s b t chy thnh CO
2
v hi
H
2
O. Sau khi nung, cn ho tan cn li c x l tip bng dung dch axit
hay mui ph hp chuyn ht cht phn tch trong cn ho tan vo dung
dch, sau xc nh cht phn tch theo phng php chn.
- K thut v c ho kh gm 2 loi:
* V c ho kh khng dng tc nhn v c ho mu
L qu trnh x l s b mu bng cch nung mu mt nhit thch
hp trong mt thi gian nht nh ph v cu trc dng ban u ca mu
phn tch, t chy cc cht hu c chuyn n sang mt hp cht khc n
gin, d tan bng cc dung mi thch hp (dung dch axit, kim) a hon
ton cht cn phn tch vo dung dch, sau xc nh cht phn tch theo
phng php chn.
Phng php ny khng dng c i vi nhng cht d bay hi khi
nung, lm mt mt lng cht phn tch, kt qu s sai.

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24
* V c ho kh c dng tc nhn v c ho mu
l qu trnh x l mu nh tc dng ca nhit (500 - 700
0
C) v c
thm cc tc nhn v c gim nhit nung, hn ch s mt mt ca mt
s nguyn t.
xc nh iot trong cc mu sinh hc, ngi ta thng dng phng
php v c ho kh bng cch nung mu nhit ~ 600
0
C vi cc tc nhn
v c ho nh: KOH, K
2
CO
3
, Na
2
CO
3
+ ZnO
4
, Na
2
CO
3
+ KNO
3
, KClO
3
+
Glycin + Na
2
CO
3

Sau khi nung, ho tan mu bng dung dch axit, lc ly dung dch
nh lng iot. Ch khi lc dung dch khng dng giy lc Whatman v
giy lc ny c th hp ph iot.
1.5. KT LUN PHN TNG QUAN
Iot l mt nguyn t vi lng quan trng trong dinh dng ngi v
ng vt ni chung. Trong c th ngi iot c phn b nhiu t chc
khc nhau nh mu, sa, nc bt, nc tiu, tc
Thiu iot s gy ri lon c th, biu hin qua mt s chng bnh nh
bu c, n n, thn kinh
Mi ngy mi ngi cn 200g iot
Ngun cung cp iot cho ngi l nc sinh hot, lng thc, thc phm.
nh gi vi lng iot trong nc, t, lng thc thc phm. Cn
phi phn tch thng xuyn. Phng php phn tch khng nhng c
chnh xc, nhy cao m cn phi ph hp vi c s vt cht hin c trong
nhiu phng th nghim.
Vi l do trn chng ti chn phng php to phc mu ca iot vi
thuc th Fucsin baz ri o bng cc my o mu thng thng m hu ht
cc phng th nghim c s u c. Theo chng ti ngh hng gii quyt
ny c thc t hn mc d nhy ca phng php ny c km hn so vi
cc phng php phn tch hin i nh AAS, AES, in ho, kch hot
ntron, ng hc xc tc..

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25
Chng 2
THC NGHIM

nh gi mc thiu ht iot i vi con ngi, cn phn tch
nh gi hm lng iot c trong t, nc v trong lng thc, thc phm.
Vi mc ch , ng thi xy dng c phng php phn tch c
th s dng rng ri, trong lun vn ny chng ti t ra nhim v sau:
1- Nghin cu phng php o quang phn tch hm lng iot bng
phn ng n gin d thc hin.
2- Nghin cu xy dng quy trnh phn tch iot trong mt s i tng
mi trng: t, nc, thc phm.
3- Dng phng php thm v phng php thng k xc sut nh
gi cc kt qu phn tch thu c.
2.1. DNG C V THIT B
- Phu chit dung tch 125ml
- Cc loi bnh ng mc 25ml, 1000ml.
- Pipet cc loi
- Cc dng c thu tinh khc.
- Cn phn tch chnh xc n 0,02mg
- My o pH
- My o hp th quang JASCO V - 530 UV - VIS
Spectrophotometer ca Nht. My thit k o c gii ph hp th t
200 -1100nm. Ngun n deterium khi o ph t ngoi (200 - 400nm), nu o
vng ph kh kin (400 - 1100nm) th dng n halogen.
nh sng ca ngun c hi t v i vo b phn to n sc bi cch
t v hi t khe ra. Ngun sng ny c chia thnh hai tia, mt tia i qua
dung dch phn tch, mt tia i qua dung dch so snh.

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26
nh sng i ti detetor chuyn tn hiu thnh tn hiu in, sau khi
c chnh ng b, chuyn thnh tn hiu s i vo b vi x l. Tn hiu sau
khi c x l bng b vi x l v hin th d kin di dng s hng ph.
2.2. CC VN NGHIN CU
- Bn cht ca phng php m chng ti nghin cu l
Iot trong mi trng phn ln nm dng I
-
, dng NaNO
2
oxi ho
chuyn v dng I
2
. Di tc dng ca cc baz hu c c mu nh mtyl tm,
malachit xanh, brilliant xanh, Fucsin baz phn t iot b phn cc, s lin
kt tnh in vi phn t Fucsin baz to thnh lin hp ion, mu ca lin hp
ion ny ging vi mu ca thuc th Fucsin baz nhng Fucsin baz l hp
cht phn cc, cn lin hp ion l hp cht khng phn cc.
Vy ta c th dng phng php chit tch lin hp ion ra v o
mu, t tnh c hm lng iot c trong mu phn tch.
Trn c s lp lun , qu trnh nghin cu ca chng ti c thc
hin theo cc bc sau:
- Kho st nh hng pH ca mi trng n qu trnh chit thuc th
v cc dung mi hu c.
- S dng phng php c nh mt thnh phn [29] kho st nh
hng pH ca mi trng nc n s to thnh hp cht lin hp ion v
kho st lng thuc th ti u.
- Kho st ph hp th ca hp cht lin hp ion
- Kho st kh nng chit hp cht lin hp ion
- Kho st cc yu t nh hng n s to thnh hp cht lin hp ion.
- Kho st khong tuyn tnh ca hp th quang A v nng iot.
- S dng phng php thm v phng php thng k xc sut
kim tra ng v chnh xc, xc nh LOD, LOQ.
- Xy dng quy trnh phn tch.
- Xc nh hm lng iot trong mu gi v mt s mu t, nc, thc phm

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27
2.3. QU TRNH THC NGHIM C TIN HNH NH SAU
2.3.1. Gii thiu v Fucsin baz
2.3.1.1. Tnh cht
Fucsin baz l nhng tinh th xanh l cy sm, sng nh
ho tan trong 100g dung mi: nc 0,26g (26
0
C), ru 5,9g (25
0
C).
Tan tt hn trong nc nng cho dung dch mu hng, dung dch ny c
hp th quang cc i = 487,1nm v 543,9nm. Kt tinh t dung dch nc
c ngm 4 H
2
O.
2.3.1.2. ng dng
Dung dch sunfua Fucsin (thuc th anhit) dng xc nh brm v
cc cht oxi ho bng phng php o quang.
Ngi ta nghin cu phn ng mu ca fucsin baz vi SO
2
[30].
S dng Fucsin baz xc nh AuCl
-
4
, TaF
5
-
[31] bng phng
php chit trc quang.
2.3.2. C ch tng tc gia I
2
vi cc cht mu baz hu c
Tng tc gia iot v cc cht mu baz hu c nh tm tinh th,
malachit xanh, brilliant lc, rodanin, fucsin bazkhng phi l phn ng
trao i, axit baz hay oxi ho kh v.v m l phn ng to lin hp ion.
Cc cht mu baz hu c l cc cht phn cc mnh [32], khi chng tng
tc vi I
2
, lm cho phn t I
2
phn cc I
+o
- I
-o
do s chuyn di ca cc in
t trong phn t. Hai phn t cht mu baz hu c v iot u phn cc, cc
cc tri du s ht nhau do lc ht tnh in to thnh hp cht lin hp. Cc
dng ca phn t iot phn cc tng tc vi cc m ca phn t cht mu
baz hu c v cc m ca phn t iot ny s tc dng vi cc dng kia ca
phn t thuc th, bi v khong cch gia hai u cc ca phn t iot ngn
hn gia hai u cc ca phn t thuc th. Phn t iot nm gn trong l
hng ca cc phn t thuc th gn nh theo c ch hp ph ca lc ht tnh

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28
in to thnh t hp cht mu baz - iot. T hp lin hp mu ny d dng
b chit bi cc dung mi nh benzen, toluen, diclometan, dicloetan,
tetracloruacacbon Trong khi cc phn t thuc th li phn cc nn
chng khng b chit bi cc dung mi ny. Li dng tnh cht ny ta c th
dng cc dung mi khng phn cc chit tch hp cht lin hp ion gia
iot vi cht mu baz hu c khi thuc th d. Chnh v vy phn ng ny
c chn lc tt.
2.3.3. Cc thc nghim kho st
2.3.3.1. nh hng ca pH n s chit ca Fucsin baz bng cc dung mi
hu c
Ly 3ml dung dch fucsin baz vo dy phu chit, sau thm vo
mi phu 5ml dung dch m c pH = 1, 2, 3, 4, 5, 6. Thm nc ct n th
tch 25ml. Thm cn thn 5ml dung mi hu c, y phu chit bng nt
nhm, lc k trong mt pht.
yn tch pha. Tch pha hu c vo bnh nh mc 25ml. Tin
hnh chit li 2 ln na, mi ln bng 5ml dung mi hu c. Thm dung mi
hu c ti vch, lc v trn u. o hp th quang (A) ca dch chit
Fucsin baz ti bc sng hp th cc i ca hp cht fucsin baz - iot. Ghi
cc kt qu thu c v bin lun trong mc bn lun kt qu thc nghim.
2.3.3.2. nh hng pH ca mi trng n s hnh thnh hp cht lin
hp ion gia fucsin baz v iot
Chun b mt dy dung dch c pH thay i, cn tt c cc cu t khc
u nh nhau. Ly 5ml dung dch KI 1mg/l, 1ml dung dch NaNO
2
0,1M. 1ml
dung dch HCl 2M v 3ml dung dch Fucsin baz. Thm tip 1ml NaOH 2M
trung ho vi 5ml dung dch m c pH = 1, 2, 3, 4, 5, 6 vo phu chit
c nh s t 1, 2, 3, 4, 5, 6. Thm nc ct ti th tch 25ml v lc trn.
Tin hnh chit hp cht lin hp fucsin baz - iot 3 ln, mi ln bng 5ml

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29
dung mi hu c. Dch chit c thu vo bnh nh mc 25ml. nh mc
dch chit bng dung mi hu c, lc trn u. o hp th quang (A) ca
dung dch thu c ti bc sng hp th cc i ca hp cht lin hp fucsin
baz v iot.
2.3.3.3. Kho st ph hp th ca hp cht fucsin baz - iot
Chun b mt dy dung dch chun bng cch ly vo dy phu chit
nhng lng dung dch nh sau:
S dung dch 1 2 3 4 5 6
Th tch dung dch KI 1mg/l 0 1 2 3 4 5
Thm vo mi phu chit 1ml dung dch NaNO
2
0,1M, 1ml dung dch
HCl 2M lc trn, thm tip 3ml fucsin baz, thm tip 1ml dung dch NaOH
2M trung ho, 5ml dung dch m pH = 4, pha long bng nc ct n th
tch 25ml.
Tin hnh chit hp cht lin hp fucsin- baz- iot 3 ln, mi ln bng
5ml dung mi hu c. Dch chit c gom vo bnh nh mc 25ml. nh
mc ti vch bng dung mi hu c, lc trn u. o hp th quang (A)
ca tng dung dch trong khong bc sng t 450 - 600nm. Biu din s ph
thuc (A) = f () ta c ph hp th ca dch chit. T xc nh c

max
ca hp cht lin hp fucsin -baz - iot.
2.3.3.4. Kho st s ph thuc hp th quang A vo lng dung dch
HCl 2M
Chun b mt dy phu chit, ly vo lng HCl 2M t 0; 0,5; 0,8; 1;
1,5; 2ml, thm vo mi phu 5ml dung dch KI 1mg/l, 1ml dung dch
NaNO
2
0,1M lc u, thm tip vo mi phu 3ml dung dch fucsin baz,
dng dung dch NaOH 2M va trung ho lng axit d ri thm vo
mi phu 5ml dung dch m c pH = 4, pha long bng nc ct n th

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30
tch 25ml. Tin hnh chit 3 ln, mi ln bng 5ml 1,2 - icloetan. Dch
chit c thu vo bnh nh mc 25ml. nh mc bng dung mi hu c
ri o A ca dy dung dch bc sng
max
va tm c trn. Kt qu
thu c s cho thy lng axit ti u cn dng.
2.3.3.5. Kho st s ph thuc lng dung dch NaNO
2
0,1M
NaNO
2
dng oxi ho I
-
thnh I
2
vy lng NaNO
2
dng bao nhiu l
v khi th c nh hng g khng. Chng ti thit lp th nghim sau:
Ly 5ml dung dch KI 1mg/l cho vo 6 phu chit sch c nh s th
t. Thm lng NaNO
2
0,1M ln lt vo cc phu chit nhng lng nh
sau: 0; 0,2; 0,4; 0,8; 1,2; 1,6 ml. Thm vo mi phu 1ml dung dch HCl 2M
lc u, thm vo mi phu 3ml dung dch fucsin baz, 1ml dung dch
NaOH 2M trung ha, 5ml dung dch m c pH=4. Thm nc ti 25ml.
Tin hnh chit hp cht mu 3 ln, mi ln bng 5ml dung mi hu c.
Dch chit c 3 ln c gom vo bnh nh mc 25 ml. nh mc ti vch
bng dung mi, lc trn, em o A ca dy dung dch
max
va tm c
th nghim trn.
2.3.3.6. nh hng ca lng thuc th fucsin baz.
I
2
to hp cht lin hp ion hon ton cn dng d thuc th fucsin
baz. Lng fucsin baz d khng b chit (th nghim 3.1).
Tuy nhin kho st lng thuc th bao nhiu th va, chng ti tin
hnh th nghim sau:
Ly 5ml dung dch KI 1mg/l, 1ml dung dch NaNO
2
0,1M v 1ml dung
dch HCl 2M cho vo 6 phu chit sch c nh s th t thm vo cc phu
theo th t lng dung dch fucsin baz nhng lng khc nhau: 0,5; 1; 1,5;
2; 2,5; 3ml, trung ho dung dch bng dung dch NaOH 2M, thm 5ml dung
dch m c pH = 4. Tin hnh chit hp cht mu 3 ln, mi ln bng 5ml
dung mi hu c. Gp dch chit c li vo bnh nh mc 25ml, ri nh mc
bng dung mi. Tin hnh o A ca dy dung dch.

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31
2.3.3.7. Kho st s ph thuc hp th quang ca hp cht mu theo
thi gian
Ly 5ml dung dch KI 1mg/l, 1ml dung dch NaNO
2
0,1M, 1ml dung
dch HCl 2M, 3ml dung dch fucsin baz, lc u dung dch, ho dung dch
thu c bng dung dch NaOH 2M. Thm 5ml dung dch m c pH = 4.
Tin hnh chit hp cht mu 3 ln, mi ln bng 5ml dung mi hu c. Dch
chit thu c nh mc thnh 25ml ri o A ca dung dch theo thi gian
(tnh t sau khi chit xong): 5, 6, 7, 8, 9, 10, 15, 20, 30, 40 pht.
2.3.3.8. Lp ng chun
Tng hp tt c cc iu kin ti u m chng ti kho st c, chng
ti tin hnh xy dng ng chun biu din s ph thuc A vo lng iot.
2.3.3.9. Kho st nh hng ca mt s cation v anion n phn ng
S dng cc kt qu kho st c trong cc th nghim trn, chng
ti tin hnh kho st nh hng ca mt s cation v anion n phn ng.
Phng php nghin cu ca chng ti da vo nguyn tc c nh cc
iu kin ti u ca phn ng, thm dn cc yu t gy nh hng vo ri tm
s ph thuc hp th quang ca dung dch theo hm lng yu t gy nh
hng thm vo A = f (yu t nh hng).
T bin lun tm c t l no th yu t l gy nh hng cho
phn ng v tm bin php loi tr.


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32
Chng 3
KT QU TH NGHIM V BN LUN

Cc kt qu ghi trong cc bng l kt qu trung bnh ca 3 ln o
3.1. KHO ST NH HNG CA pH N S CHIT THUC TH FUCSIN
BAZ BNG CC DUNG MI
Fucsin baz l phn t phn cc nn n khng b chit bi cc dung
mi hu c khng phn cc nh Benzen, Tetracloruacacbon khi chit
Fucsin baz bng tetracloruacacbon (CCl
4
), pha hu c hon ton khng c
mu tt c cc gi tr pH kho st, chng t Fucsin baz khng b chit bi
CCl
4
. Khi dung mi hu c l Clorofom (CHCl
3
), pha hu c chit c
khng c mu cc pH tr gi tr pH = 2, dch chit c mu hng nht. i
vi dung mi chit l diclometan v 1,2 - icloetan, dch chit c mu hng
m pH s 2, cc pH kho st cn li, dch chit c mu hng rt nht. Khi
chit bng hn hp dung mi diclometan: clorofom vi cc t l theo th tch
l 1:4; 1:3; 1:2; 1:1; 2:1; 3:1; 4:1 th cng ch pH = 2 lp chit mi c mu
hng cn trong mi trng pH t 3 n 6 lp chit hu nh khng c mu. S
chit fucsin baz bng cc dung mi hu c phn cc ph thuc vo pH dung
dch nc c ghi trn cc bng t 3.1 n3.3.
Bng 3.1: Gi tr A ca dch chit Fucsin Baz bng CHCl
3

cc pH khc nhau ca dung dch nc
pH 1 2 3 4 5 6
A
551nm
0,019 0,040 0,018 0,016 0,018 0,020

Cc s liu ghi trong bng 3.1 cho thy, trong khong pH kho st (t 1
n 6) thuc th fucsin baz hu nh khng b chit bi CHCl
3
v cc gi tr
hp th quang A u nh (tr pH = 2 dung dch c mu hi hng nht).
Vi kt qu ny cho thy nu chit bng CHCl
3
th thuc th fucsin baz d
khng b chit, nh vy thuc th d khng nh hng n qu trnh phn
tch khi chit hp cht mu.

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33
Bng 3.2: Gi tr A ca dch chit fucsin baz bng CH
2
Cl
2

cc pH khc nhau ca dung dch nc
pH 1 2 3 4 5 6
A
537nm
0,102 0,196 0,022 0,039 0,045 0,036

Cc s liu ghi trong bng 3.2 cho thy, trong khong pH t 3 n 6
thuc th hu nh khng b chit nn nu tin hnh th nghim trong khong
pH ny, thuc th d khng gy nh hng, cn pH t 1 n 2 th fucsin
baz c b chit v vy khng nn tin hnh th nghim cc gi tr pH ny.
Bng 3.3: Gi tr A ca dch chit fucsin baz bng 1,2 - dicloetan
(C
2
H
4
Cl
2
) cc gi tr pH khc nhau ca dung dch nc
pH 1 2 3 4 5 6
A
539nm
0,056 0,159 0,044 0,047 0,048 0,046

Cc s liu ghi trong bng 3.3. cho thy fucsin baz b chit bi dung
mi 1,2- dicloetan pH = 2 v khong pH 3-6 thuc th gn nh khng b
chit. Ta ch nn thc hin cc th nghim trong khong pH 3 - 6 th lng
thuc th d khng gy nh hng cho qu trnh phn tch.
Chng ti dng dung mi chit l hn hp CH
2
Cl
2
: CHCl
3
theo cc t
l v th tch l 1: 4; 1: 3; 1: 2; 1:1; 2:1; 3: 1 v 4: 1. Kt qu cng cho thy
ch pH = 2 lp chit mi c mu hi hng, cn cc gi tr pH khc lp
chit hu nh khng mu.
Vi kt qu th nghim trn khi chit hp cht lin hp Fucsin- baz -
iot c th dng cc dung mi trn nhng tin hnh pH trong khong 3 - 6 th
lng thuc th d khng gy nh hng g cho qu trnh phn tch.
Chng ti chn pH th nghim bng 4; dng dung dch m.

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3.2. KHO ST NH HNG pH CA MI TRNG NC N S HNH
THNH HP CHT MU LIN HP GIA FUCSIN BAZ VI IOT
Th nghim c tin hnh nh trnh by mc 3.2 chng 2 v thu
c cc kt qu nh sau:
* Dng dung mi chit l Clorofom, hp th quang ca dung dch
chit c o bc sng 551nm, kt qu o c ghi trong bng 3.4.
Bng 3.4: Gi tr A ca dch chit hp cht mu Fucsin baz - Iot
trong Clorofom cc pH khc nhau trong mi trng nc
pH 1 2 3 4 5 6
A
551nm
0,159 0,218 0,246 0,246 0,246 0,246

Cc s liu ghi trong bng 3.4 cho thy, gi tr pH 1 - 2 hp th
quang ca dch chit nh, iu ny c th gii thch nh sau: trong khong
pH ny dung dch c axit cao nn thuc th Fucsin baz dng cation
cn t, tc ng phn cc ca n i vi phn t iot t nn hp cht mu lin
hp to thnh cn t. pH 3 - 6 gi tr hp th quang A o c gn
bng nhau, chng t cc gi tr pH ny Fucsin baz nm dng cation ht,
chng phn cc ton b cc phn t iot to thnh hp cht mu lin hp
Fucsin baz -iot.
Kt hp vi kt qu khi kho st nh hng ca pH n s chit ca
thuc th trn, chng ti thy pH t 3 - 6 iot to hp cht mu lin hp
ht vi Fucsin baz, hp cht ny b chit bi CHCl
3
, nhng thuc th d
khng b chit. iu ny rt thun li cho qu trnh phn tch, chng ti chn
pH = 4 kho st cc yu t tip theo. bo m gi tr pH ny trong cc
th nghim chng ti dng dung dch m.
* Nu chit bng dung mi diclometan, hp th quang ca dch chit
o ti bc sng cc i 537nm, cn nu dng dung mi l 1,2 -dicloetan th
o ti 539nm. Kt qu c ghi trong bng 3.5 v 3.6.

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Bng 3.5: Gi tr A ca dch chit hp cht mu lin hp Fucsin baz -
Iot trong diclometan t mi trng nc cc gi tr pH khc nhau
pH 1 2 3 4 5 6
A
537nm
0,174 0,238 0,271 0,271 0,269 0,270

Bng 3.6: Gi tr A ca dch chit hp cht mu lin hp Fucsin baz -
iot trong 1, 2 - dicloetan cc pH khc nhau ca mi trng nc
pH 1 2 3 4 5 6
A
539nm
0,150 0,205 0,234 0,235 0,234 0,235

Cc gi tr ghi trong bng 3.5 v 3.6 cho thy dng dung mi chit l
diclometan v 1 - 2 dicloetan trong mi trng c pH 3 - 6 iot cng to hp
cht mu lin hp ht vi Fucsin baz. Ta c th dng cc dung mi ny
chit tch hp cht mu ra khi dung dch v loi tr cc nh hng khc.
3.3. PH HP TH CA HP CHT MU FUCSIN BAZ - IOT
Cc th nghim c chun b nh trong mc 3.3 ca chng 2
Chng ti tin hnh ghi ph hp th ca hp cht mu lin hp
Fucsin baz - iot trong dch chit bng cc dung mi nh Clofom, diclometan,
1 - 2 dicloetan.
Cc ng biu din ph hp th ca hp cht mu lin hp Fucsin
baz - iot chit trong cc dung mi th c cc i hp th khc nhau (chit
bng CHCl
3
th
max
= 551nm, chit bng CH
2
Cl
2
th
max
= 537nm, cn
bng C
2
H
4
Cl
2
th
max
= 539nm) nhng tng loi dung mi vi cc nng
iot khc nhau u c cng mt cc i hp th. iu chng t hp cht
mu c thnh phn khng i v c bn mu tt, iu ny rt c li cho
php phn tch.

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Di y chng ti trnh by 1 ph hp th ca hp cht mu lin hp
gia Fucsin baz vi iot khi chit bng diclometan. Khi dng cc dung dch
iot c nng khc nhau. Mc d nng iot bng bao nhiu cc ph hp th
u c 1 dng v c cc i hp th
max
= 537nm.










Hnh 3.1: Ph hp th ca hp cht mu Fucsin baz - iot cc nng
iot khc nhau c chit bng diclometan.
3.4. KHO ST NH HNG CA LNG AXIT HCl LN PHN NG
Phn ng oxi ho I
-
thnh I
2
bng NO
2
-
thc hin trong mi trng axit.
NO
2
-
+ 2H
+
+ 2I
-


NO + H
2
O + I
2

V vy cn kho st tm lng axt ti u cn cho s oxi ho.
Qu trnh th nghim c trnh by trong mc 3.4 chng 2.
Di y chng ti ch trnh by kt qu th nghim thu c v
bin lun.
Kt qu kho st s ph thuc hp th quang A vo nng axit
HCl trong dung dch c trnh by bng 3.7 (chit bng dung mi 1,2 -
dicloetan).


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37
Bng 3.7: S ph thuc hp th quang (A) vo nng HCl
V
HCl 2M
(ml) 0 0,5 0,8 1,0 1,5 2,0
A
539nm
0,020 0,130 0,210 0,215 0,210 0,205

Cc gi tr ghi trong bng 3.7 cho thy hp th quang ca dung
dch tng. khi tng lng HCl 2M t 0 n 0,8 (ml). T gi tr 0,8 - 2,0ml
th hp th quang ca dung dch hu nh khng i. iu c th
gii thch nh sau, nng axt thp cha thc hin phn ng oxi
ho ht iodua thnh I
2
t do. Khi tng lng axt ln 0,8ml HCl 2M lc
ny lng axit oxi ho ton b iodua thnh I
2
nn lng hp cht
mu trong dung dch n nh. Chng ti chn lng axt cn dng l 1ml
HCl 2M.
Sau khi thc hin phn ng xong, phi to pH ca dung dch nc ti
u (pH = 4) thc hin phn ng to hp cht mu lin hp. Mun vy
phi trung ho lng axt d bng dung dch NaOH 2M sau mi dng
dung dch m pH = 4 gi gi tr pH ca dung dch.
3.5. KHO ST S PH THUC CA LNG CHT OXI HO NaNO
2
0,1M
Qu trnh th nghim c tin hnh nh trnh by trong mc 3.5
chng 2.
Kt qu kho st trnh by trong bng 3.8.
Bng 3.8: Gi tr A ca dch chit hp cht mu Fucsin baz - iot
bng 1,2 - dicloetan ph thuc vo lng cht oxi ho NaNO
2

V
NaNO2 0,1M
(ml) 0 0,2 0,4 0,8 1,2 1,6
A
539nm
0,025 0,06 0,11 0,190 0,190 0,20


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38
Cc kt qu ghi trong bng 3.8 chng t trong iu kin th nghim
(5ml dung dch KI 1mg/l) th cn dng lng cht oxi ho NaNO
2
0,1M l
0,8ml l oxi ho ht I
-
thnh I
2
, lng d NaNO
2
khng nh hng
n qu trnh phn tch. Chng ti dng 1ml dung dch NaNO
2
cho cc th
nghim kho st.
3.6. NH HNG CA LNG THUC TH
Th nghim c pha ch nh trong mc 3.6 chng 2.
Kt qu th nghim khi chit hp cht mu bng dung mi 1,2 -
dicloetan c ghi trong bng 3.9.
Bng 3.9: Kt qu kho st nh hng ca lng thuc th Fucsin baz
V
thuc th
(ml) 0,5 1 1,5 2 2,5 3
A
359nm
0,102 0,115 0,213 0,215 0,214 0,215

T cc kt qu bng 3.9 cho thy trong iu kin th nghim (5ml
dung dch KI 1mg/l) ti u th khi lng Fucsin baz 1,5ml dung dch c
hp th quang ln nht v khng i. iu ny rt hp l bi v iot to hp
cht mu hon ton vi thuc th cn phi dng d thuc th, mt khc lng
thuc th d li khng b chit cng vi hp cht mu. m bo lng
thuc th dng d nhng khng cn d qu nhiu, s tn km, trong iu kin
th nghim chng ti dng 3ml dung dch Fucsin baz. Tt nhin tu thuc
vo hm lng I
-
c trong dung dch m ta dng lng thuc th thch hp
nhng phi m bo d nhiu so vi lng iot.
3.7. KHO ST S PH THUC HP TH QUANG CA HP CHT MU
THEO THI GIAN
Cch pha ch dung dch v quy trnh th nghim c thc hin nh
trong mc 3.7 chng 2.

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39
Cc kt qu th nghim c trnh by trn hnh 3.2.








Hnh 3.2: nh hng ca thi gian n bn mu ca hp cht mu
lin hp Fucsin -baz -iot (dung mi chit l CHCl
3
)
Kt qu kho st cho thy kh nng hp th ca hp cht mu lin hp
to bi Fucsin baz v iot gn nh khng i trong khong 30 pht sau khi
chit, sau A gim dn. V vy phi tin hnh o trong vng 30 pht sau
khi chit hp cht mu. Kho st khi chit bng dung mi khc nh
diclometan, 1, 2 - dicloetan cng cho kt qu tng t.
3.8. NH HNG CA NHIT
Nh trn trnh by, phn ng gia Fucsin baz vi iot l phn ng
hp ph tng t nh phn ng gia h tinh bt vi iot. V vy nhit c
nh hng ln ti phn ng. Nhit thp th phn ng xy ra chm, nhng
nhit cao th hp cht mu b phn hu. m bo cho phn ng xy
ra tt v ph hp vi iu kin phng th nghim, chng ti tin hnh th
nghim trong phng iu ho nhit c nhit khong ~ 20
0
C.
3.9. LP NG CHUN
Sau khi kho st tt c cc yu t nh hng n phn ng, chng ti
rt ra cc iu kin ti u khi thc hin phn ng. Da vo cc iu kin
ti u , chng ti tin hnh lp ng chun. kim tra ng ca

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40
ng chun, chng ti xy dng ng chun theo phng php thm tin
hnh song song vi th nghim xy dng ng chun.
Chng ti xy dng ng chun vi tng loi dung mi chit. xy
dng ng chun, chng ti lp th nghim iu kin ti u, nhng lng dung
dch iot chun tng dn. Sau khi chit hp cht mu, tin hnh o hp th
quang ca dy dung dch bc sng
max
i vi tng loi dung mi, dung dch
so snh l dung dch khng c iot. ng chun l ng biu din A = f (C
I
-
).
lp ng chun, chng ti tin hnh nh sau:
Dng dung mi chit l Clorofom. Chng ti xy dng ng chun
hai khong nng I
-:
0,001 - 0,1 mg/l v t 1 n 9mg/l.
* ng chun 1: Dng dung dch KI 1mg/l.
Bng 3.10: S ph thuc gi tr A vo nng iot
C
I
-
(mg/l)
0 0,04 0,08 0,12 0,16 0,2 0,24 0,28 0,32 0,36
A
551nm
DD so snh 0,04 0,081 0,13 0,17 0,21 0,25 0,29 0,34 0,38

0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40
0.00
0.05
0.10
0.15
0.20
0.25
0.30
0.35
0.40
Y = A + B * X
Parameter Value Error
------------------------------------------------------------
A -0.00131 0.00227
B 1.05708 0.01006
------------------------------------------------------------
R SD N P
------------------------------------------------------------
0.99968 0.00312 9 <0.0001
------------------------------------------------------------
A
b
s
nong do iot (mg/lit)

Hnh 3.3: ng chun xc nh iot bng thuc th fucsin baz

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41
* ng chun 2: Dng dung dch KI 0,1mg/l.
Bng 3.11: S ph thuc gi tr A vo nng iot

C
I
-
(mg/l)

0 0,002 0,0038 0,008 0,012 0,016 0,02 0,024 0,028 0,036
A
551nm
dd so snh 0,002 0,005 0,01 0,015 0,021 0,026 0,031 0,036 0,045
0.00 0.01 0.02 0.03 0.04
0.00
0.01
0.02
0.03
0.04
0.05
Y = A + B * X
Parameter Value Error
------------------------------------------------------------
A 1.00192E-5 3.38031E-4
B 1.27443 0.01705
------------------------------------------------------------
R SD N P
------------------------------------------------------------
0.99937 5.51127E-4 9 <0.0001
------------------------------------------------------------
A
b
s
nong do iot (mg/lit)

Hnh 3.4: ng chun xc nh iot bng thuc th fucsin baz
Kt qu thu c sau khi x l thng k theo phng php bnh
phng ti thiu ta c
Phng trnh hi quy: A A = (1,274 0,017)
I
C

+ (0.00001 0,00034)
H s tng quan: R
2
= 0,999
V kt qu thc nghim biu din trn hnh v kt qu x l thng k
cho thy hp th quang ca hp cht lin hp ion gia iot v fucsin baz
trong clorofom tun theo nh lut Lambert-Beer trong khong nng ca
iot t 0,002 n 0,036M (0,6 8,2 g/ml).

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42
xc nh gii hn pht hin LOD v gii hn nh lng LOQ ca
phng php, ta chun b mu trng ging nh mu chun ch khc l khng
c mt iot. Th nghim c tin hnh 6 ln, kt qu c x l theo phng
php thng k vi.
Th nghim trng: 0,016; 0,015; 0,014; 0,015; 0,014; 0,014
lch chun S = 8,165x10
-4
Gii hn pht hin LOD =
b
S 3
=
274 , 1
10 165 , 8 3
4
x x
= 0,0019 mg/l
V b l h s gc ca ng chun.
Gii hn nh lng LOQ =
b
S 10
=
274 , 1
10 165 , 8 10
4
x x
= 0,0064 mg/l
T cc kt qu trn cho thy c th dng thuc th fucsin baz xc
nh vi lng iot bng phng php chit - trc quang.
* Chng ti tin hnh lp ng chun bng phng php thm (thm
vo mi dung dch chun 0,2 mg/l KI = C
x
ri cng tin hnh th nghim nh
xy dng ng chun. Sau v ng A = f (C
I
+ C
x
).
Nu ng chun lp c l chnh xc th 2 ng chun bng
phng php thm v khng thm s song song vi nhau v dng phng
php ni suy ta s tnh c C
x
ng bng lng C
x
thm vo.
Kt qu th nghim cho thy 2 ng chun A = f (C
I
-
) v A = f (C
I
+ C
x
)
l 2 ng thng song song nhau.
Dng phng php ngoi suy ko di ng chun (A = f (C
I
+ C
x
) th
n ct trc tung im c honh tnh t 0 ng bng C
x
= 0,2 mg/l. Vy
ng chun xy dng c l ng v chnh xc.
Xy dng ng chun bng cch dng dung mi chit l diclometan
v 1,2 - dicloetan cng cc dng tng t v chnh xc.

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43
0.00 0.01 0.02 0.03 0.04
0.00
0.01
0.02
0.03
0.04
0.05
0.06
A
b
s
nong do iot (mg/l)

Hnh 3.5: ng chun xc nh iot bng phng php thm
3.10. KHO ST NH HNG CA MT S NGUYN T
Sau khi tm c cc iu kin ti u cho phn ng xc nh iot
bng fucsin baz. Chng ti mun s dng phn ng ny xc nh iot c
trong mt s mu thc t mi trng (t, nc, thc phm). V vy, cn xt
nh hng ca mt s nguyn t.
kho st cc nguyn t nh hng n phn ng gia iot vi Fucsin
baz, chng ti kho st da vo nhng cht c kh nng gy nh hng
n phn ng nghin cu, c th l nhng cht.
- C kh nng phn ng vi Fucsin baz (tc l c phn ng cnh tranh
vi iot nh clo, Brom).
- C kh nng phn ng vi iot lm cn tr phn ng nh lng ca
iot vi thuc th.
C
x


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44
C th chng ti s xt nh hng ca cc anion nh Cl
-
, Br
-
ClO
-
3
,
CN
-
, S
2 -
v cation Fe
3+
.
Iot va th hin tnh oxi ho khi n tc dng vi cc cht kh mnh.
(SO
3
2-
, S
2
O
3
2-
, S
2-
, CN
-
, HCHO, SCN
-
, AsO
3
2-
...) va th hin tnh kh
khi n tc dng vi cc cht oxi ho mnh hn [33]
Tuy nhin trong mi trng kim yu I
2
mi oxi ho c CN
-
, S
2-
,
2
s 3
A O


2
CN I ICN I

+ = +
2 2
2 4 2
S 4I 8OH SO 8I 4H O

+ + = + +
Phn ng gia Fucsin baz v iot c tin hnh trong mi trng axit
yu (pH = 4) nn nh hng ny b hn ch nhiu. i vi Cl
-
,

Br , ClO
3
th

2
NO trong mi trng axit khng oxi ho c chng thnh Cl
2
v Br
2
nn
nh hng khng th xy ra.
Mc d vy chng ti vn tin hnh mt s th nghim kim tra lp
lun trn. Th nghim c tin hnh nh trnh by mc 3.9 chng 2.
Bng 3.12: Kt qu kho st nh hng ca Br
-

V
Br
-
1mg/l
(ml) 0 3 5 7 10
A 0,220 0,215 0,210 0,225 0,182

Kt qu cho thy ch khi lng Br
-
gp 2 ln I
-
th mi gy nh hng.
Bi v khi Br
-
ln n cng b

2
NO oxi ho 1 phn thnh Br
2
v Br
2
c phn
ng cnh tranh vi Iot.
Bng 3.13: Kt qu kho st nh hng ca

3
ClO
3
ClO 1mg / l
V

(ml)
0 3 5 7 10
A 0,215 0,205 0,210 0,216 0,215

Kt qu cho thy

3
ClO khng h gy nh hng g.

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45
Bng 3.14: Kt qu kho st nh hng ca Cl
-
Cl 1mg / l
V

(ml)
0 3 5 7 10
A 0,220 0,215 0,210 0,225 0,223

Kt qu cho thy Cl
-
khng gy nh hng g cho php phn tch iot
Bng 3.15: Kt qu kho st nh hng ca CN
-

CN 1mg / l
V

(ml)
0 3 5 7 10
A 0,210 0,215 0,22 0,210 0,205

Kt qu cho thy CN
-
cng khng gy nh hng g n phn ng phn
tch iot bng Fucsin baz.
Bng 3.16: Kt qu kho st nh hng ca S
2-

2
S 1mg / l
V


(ml)
0 3 5 7 10
A 0,215 0,210 0,205 0,210 0,215

Kt qu cho thy S
2-
ln hn I
-
2 ln khng gy nh hng ti php
phn tch.
Bng 3.17: Kt qu kho st nh hng ca Fe
3+
3
Fe 1mg / l
V
+

(ml)
0 3 5 7 10 15
A 0,210 0,215 0,214 0,210 0,220 0,130
Kt qu cho thy khi Fe
3+
ln gp 2 ln nng I
-
th khng gy nh
hng, khi nng Fe
3+
ln th phi tch hoc kh n v Fe
2+
.
3.11. p dng nhng kt qu nghin cu c phn tch mt s mu
mi trng: t, nc, trng
3.11.1. Phn tch iot trong t
It tn ti trong t thng dng mui iodua ca cc loi mui bc,
mui ng (AgI, CuI, Cu
2
I
2
v.v), cng nh Brm trong t nhin iot lun

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46
chuyn theo mt chu trnh lin tc t dng iodua (I
-
) c oxi ho thnh iot
(I
2
) nh oxi khng kh, bay hi t bin theo my gi chuyn vo t lin ri
xung theo ma. Iot trong t chim 1,8.10
-4
% (tc l gn 2 ppm). Ni c
hm lng iot thp nht ch vo khong 10
-5
- 10
-6
% (tc l 0,1 ppm 0,01
ppm) v ni c hm lng iot cao nht cng ch vo khong 7 8 ppm.
t nhng ni c dn c sinh sng chn nui, trng trt, t canh tc,
t rung, t i, trong t c chia thnh.
- t phong ho ti ch (a thnh) l loi t pht trin t nhin t
nhiu loi nham thch khc nhau, loi t ny thng c hm lng it thp.
- t hi t ph xa (bn thu thnh - thu thnh) l loi t tp trung ti
cc thung lng, sng ngi, c a hnh tng i bng phng, d khai thc
nng nghip, loi t ny gi l "t tr", c ph cao.
t phong ho ti ch c nhiu tnh cht ca khong ni, cn t hi t
ph sa l t dng cho canh tc nng nghip.
Trong vic ly mu phn tch iot nhm nh gi tc ng ca mi
trng, ngi ta ch ch trng t i, t vn, t rung l mi trng t
m con ngi sng trn . Cc loi cy trng trn nhng vng t ny c
hm lng iot cao hay thp tu thuc vo hm lng iot c trong t. Con
ngi v gia sc n cc loi cy trng trn t ny s hp th iot nhiu hay t
theo lng iot m cy trng hp th iot t t.
Iot trong t gm 2 loi: Loi d b ra tri theo nc, cn phn iot
nm su trong t khng b nc ra tri. Ngi ta chia iot trong t thnh 2
phn: iot d tiu (linh ng) v iot ton phn. Iot d tiu l phn iot d b nc
ho tan, cun theo nn d b ra tri theo nc ma, nc l ri chuyn ra
sng ra bin. Cy trng v con ngi d dng hp th loi iot ny. Iot ton
phn bao gm c iot d tiu v c phn iot lin kt nm su trong t phi
dng phng php ho hc ho tan t thnh dung dch mi tch c iot
ton phn ra khi t.

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Tch iot di ng khi t: Da theo ti liu tham kho v qua thc t
kho st chng ti rt ra c quy trnh chit tch iot di ng khi mu t
nh sau. Cn 5(g) t kh nghin mn, em ngm chit trong 50ml nc
ct trong 240 pht v c 30 pht khuy u 1 ln sau lng, lc ly nc
em phn tch. Lng iot di ng tch ra theo nc l ln nht v khng i.
phn tch iot ton phn trong t, chng ti da theo [34],[35] x l
mu t theo 2 cch:
- Nung kim chy (nung 5g t vi 5g NaOH)
- Ho tan bng dung dch HNO
3
37%
Kt qu x l cng mt mu t c thm 5ml dung dch KI 1mg/l bng
2 cch ri tin hnh o A ca tng mu c kt qu nh sau:
Bng 3.18: Kt qu xc nh iot khi x l mu bng phng php
kim chy, phng php ha tan bng Axit
S th
t mu
hp th quang A ca dung dch sau khi ch ho o c
Phng php nung chy kim
Phng php ho tan
bng HNO
3
37%
1 0,215 0,206
2 0,160 0,154
3 0,300 0,205

Kt qu phn tch cho thy nu ph mu bng dung dch HNO
3
37% th
kt qu thp hn mt cht so vi ph mu bng phng php kim chy, iu
ny cng d gii thch, khi ph mu bng HNO
3
37% th I
-
s b oxi ho mt
phn thnh I
2
v un nng s bay mt.
6KI + 8 HNO
3
= 3I
2
+ 6KNO
3
+ 4 H
2
O + 2NO
V vy khi x l mu t phn tch iot ton phn (tng s) chng ti
dng phng php kim chy.

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3.11.2. Phn tch iot trong nc
Iot c nhiu trong nc bin, thnh phn ca iot trong nc bin tng
i n nh. Chu trnh lun chuyn iot t nc bin theo chu k nc bin
bc hi c ko theo iot, hi nc c gi v my chuyn i cc ni, ngng
t v khi gp lnh ri xung thnh ma mi vng trn tri t.
Iot c trong t c ho tan ri chuyn vo cc ngun nc mt, thm
vo nc ngm, chy ra sng, sui v cui cng ra bin c.
- Nc t nhin c cha nhiu tp cht dng ho tan v khng ho
tan, c thnh phn v c v hu c, c cc nguyn t a lng v vi lng.
Cc nguyn t vi lng c trong nc, c nhiu nguyn t c ngha
rt c li v cn thit i vi s sng, c bit l iot.
Iot trong nc ch dng vt cho nn phn tch trc ht phi lm
giu mu, thng l bng cch c cn mu.
Iot trong nc t tn ti di dng hp cht hu c, v vy khng cn
thit phi v c ho mu nc bng HNO
3
. Kt qu kho st cho thy khi v
c ho mu nc bng HNO
3
th hm lng iot tm c thp hn khi ch c
cn lm giu mu. L do l iodua trong mi trng HNO
3
b oxi ho thnh iot
khi c s b bay mt.
Ly 200ml nc ct, thm vo 5ml dung dch KI 1mg/l. Mt mu em
c lm giu ri phn tch, mt mu tin hnh v c ho bng HNO
3
37% ri
phn tch kt qu cho thy khi x l mu bng HNO
3
lng iot b mt kh nhiu.
Bng 3.19: Kt qu xc nh iot trong mu nc khi c cn mu
v khi x l bng HNO
3
37%
STT Mu ch c cn lm giu Mu x l bng HNO
3
37%

1 0,210 0,200
2 0,200 0,180
3 0,165 0,140

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3.11.3. Phn tch iot trong trng
Iot c a vo c th con ngi qua thc n v nc ung l chnh.
Con ngi n cc loi thc n ng vt l cc loi tht nh tru, b,
nga, d, ngan, ngng, g, vt v.v cc loi c, tm, cua, c, ch v.v Cc
loi ng vt ny cng chu tc hi ca s thiu ht iot nh con ngi, ngha
l chng cng mc cc bnh ri lon do thiu ht iot nh con ngi nht l
tc ng n kh nng sinh sn. Iot tc ng rt ln n kh nng to hocmon
sinh sn ni chung [3],[4].
S thiu ht iot con ngi v gia sc u gy hin tng sy thai,
non. Con ci sinh ra u m yu, n n, khng c kh nng khng,
c khi tr thnh d dng. Cc loi ng vt trng, nu thiu ht iot s
dn ti trng b nh, thiu ht lng , lng trng, khng u, ngt
qung. Trong lng trng trng c cht albumin l cht c kh nng hp th
iot rt tt, v vy phn tch nh gi hm lng iot trong trng ca cc loi
gia sc c th nh gi c tnh trng thiu ht iot trong vng, qua m
c k hoch b sung iot cho con ngi qua con ng n trng ca cc loi
gia cm nui c iot.
Trng g, vt, chim ct l cc loi trng m nhn dn ta thng x
dng lm thc n hng ngy. Vic phn tch hm lng ca iot trong trng
c bin php thc y sinh sn v nui dng, y mnh sn lng chn nui
trong cc h gia nh, cc hp tc x v cc tri chn nui tp trung.
X l mu trng phn tch iot.
* Phn tch iot trong lng trng v lng ring bit. Trng p v
tch 2 phn lng v lng trng ring bit. Phn hu lng v lng trng
bng dung dch NaOH 10% v bng dung dch HNO
3
1:1 cn chnh xc 1g
lng v 1g lng trng, em phn hu ring r bng dung dch HNO
3
1: 1
n tan ht lc ly dung dch c cn cn 10ml. Tin hnh phn tch iot c
trong dch chit.

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* Phn tch iot trong hn hp c lng v lng trng. Trng p v,
nh tan c lng trng ln lng thnh mt hn hp cn 1g hn hp ri phn
hu bng HNO
3
1: 1 n tan ht, lc, c cn cn 10ml. Tin hnh phn tch iot.
Kt qu kho st cho thy x l mu trng bng HNO
3
tan tt hn l phn
hy bng NaOH 10%. ho tan 1g mu trng cn khong 5ml HNO
3
1:1
T cc kt qu kho st trn, chng ti xy dng quy trnh phn tch iot
trong cc mu mi trng t, nc v trng nh sau:
3.12. Cc quy trnh phn tch iot trong cc mu mi trng t, nc, trng
3.12.1. Quy trnh phn tch iot trong mu t
* Phn tch iot di ng: Cn 5g t hong kh nhit phng
(khong 25 - 30
0
C) v nghin mn, cho vo bnh nn c 250ml c nt nhm.
Thm vo bnh 50ml nc ct, ngm mu trong 4 gi, c 30 pht li lc,
khuy trn 1 ln. Lc ly 25ml dch lc, c cn ~ 10ml, chuyn vo phu
chit, thm vo 1ml dung dch NaNO
2
0,1M, 1ml dung dch HCl 2M, 3ml
dung dch Fucsin baz 30mg/l, lc u dung dch, trung ho dung dch thu
c bng dung dch NaOH 2M (khong ~ 1ml). Thm 5ml dung dch m
c pH = 4; lc phu chit. Tin hnh chit hp cht mu 3 ln, mi ln bng
5ml dung mi hu c (CHCl
3
, CH
2
Cl
2
, trong 1,2 - icloetan).
Khi xy dng ng chun dng dung mi no th khi phn tch dng
dung mi . Dch chit gom tt c vo bnh nh mc 25ml ri nh mc ti
vch bng dung mi chit (cch tin hnh ging hon ton nh lp ng
chun). em o hp th quang ca dung dch (A) vi dung dch so snh l
dung dch trng ca dy dung dch chun, vi cuvet ng l cuvet dng o
A dy dung dch chun bc sng
max
ti u (tu tng loi dung mi).
o gi tr A t nht 3 ln ri ly gi tr trung bnh. Cn c vo gi tr A
o c, da vo ng chun s tnh c gi tr iot c trong mu phn tch.

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51
* Phn tch iot ton phn
Cn 1g t hong kh v nghin mn, cho vo chn niken, cn 1g
NaOH khan, ly khong 0,9 gam trn u vi 1g mu t, cn 0,1 gam li
ph ln b mt. a chn vo l nung nhit 250 - 300
0
C. Nung mu
khong 20-25 pht. Ly mu ra ngui v ha tan mu nung bng 50ml
nc ct, lc v c n cn ~ 10ml. Sau tin hnh phn tch nh trn.
3.12.2. Quy trnh phn tch iot trong nc
Ly 100ml mu nc cn phn tch, em c cn cn khong 10ml, sau
tin hnh phn tch theo quy trnh trn v tnh ra hm lng iot c trong nc.
3.12.3. Quy trnh phn tch iot trong trng
p trng vo cc, nh u, cn 1g hn hp (c lng trng v lng )
cho vo cc 100ml, thm t t mi ln 1ml dung dch HNO
3
1: 1 n khi mu
tan ht, thm ~ 15ml nc ct, lc u, lc, ly ton b dch lc thu c cho
vo phu chit, ch ho v tin hnh chit nh quy trnh phn tch t, nc.
Dng ng chun tnh hm lng iot c trong trng.
Song song vi vic phn tch bng phng php ng chun, chng
ti cng phn tch bng phng php thm nh gi hiu xut thu hi,
cng nh chnh xc ca php xc nh.
Chng ti phn tch mt s mu t, mt s mu nc v mt s mu
trng bng c hai phng php, tnh hiu xut thu hi ca phng php xc
nh. Kt qu thu c nh sau:
Bng 3.20: Kt qu phn tch iot di ng trong mu t
STT 1 2 3 4
Lng I
-
di ng c trong t Cx Cx Cx Cx
Lng I
-
thm vo mu (ppm) 0 1 2 3
Lng I
-
xc nh c (ppm) 2,02 3,05 3,90 5,05
Hiu sut thu hi (%) 103 94 101
Sai s (%) +7 -6 +1

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52
Bng 3.21: Kt qu phn tch iot trong mu nc
STT 1 2 3 4 5 6 7 8
Lng I
-
c trong mu nc Cx Cx Cx Cx Cx Cx Cx Cx
Lng I
-
thm vo mu (ppm) 0 0,1 0,2 0,3 0,4 0,5 1,5 2,0
Lng I
-
tm thy (ppm) 0,01 0,112 0,205 0,30 0,405 0,55 1,502 2,02
Hiu sut thu hi (%) ~ 102 97,5 96,6 98,8 108 99,5 100,5
Sai s mc phi (%) - +2 -2,5 -3,4 -1,2 +8 -0,5 +0,5
Bng 3.22: Kt qu phn tch iot trong mu trng vt
STT 1 2 3 4 5 6 7 8
Lng I
-
c trong mu trng Cx Cx Cx Cx Cx Cx Cx Cx
Lng I
-
thm vo mu (ppm) 0 0,2 0,4 0,6 0,8 1,0 1,5 2
Lng I
-
tm thy (ppm) 4,85 5,08 5,21 5,48 5,70 5,80 6,40 6,70
Hiu sut thu hi (%) ~ 115 90 105 106,25 95 103,3 92,5
Sai s mc phi (%) - +15 -10 +5 +6,25 -5 +3,3 -7,5
Kt qu xc nh c cho thy, php phn tch mc sai s s 15%.
Trong phn tch lng vt sai s mc phi nh vy l chp nhn c.
Vy c th dng phng php phn tch ny xc nh iot trong i
tng mi trng.
Sau y chng ti trnh by kt qu phn tch mt s mu t, mu
nc v mu trng mt s ni.
Chng ti p dng cc quy trnh phn tch xy dng c xc nh
iot trong mu t (c iot di ng v iot tng s), mu nc (nc ging, nc
h v nc my) v mu trng (g, vt v chim ct mua ch H Ni do cc
a phng em v bn).

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53
i vi t, chng ti phn tch iot di ng v tng s trong cc loa
t: t rung, t vn, t i, trong t i chng ti ly 3 v tr ca
i l nh i, sn i v chn i. Kt qu phn tch c ghi trong
cc bng sau:
Bng 3.23: Kt qu phn tch iot trong cc mu t i Thi Nguyn
K hiu mu
Hm lng
iot di ng
(ppm)
Hm lng
iot ton
phn (ppm)
T l (%)
iot d iot tp
Gi tr trung bnh
Iot di
ng
(ppm)
Iot
ton
phn
(ppm)
T l
(%)
iot d
iot tp
t nh i


1 0,07 0,96 7,3
0,07 0,95 7,37
2 0,08 0,98 8,2
3 0,085 0,85 10
4 0,065 1,00 6,5
5 0,06 0,95 6,3
t sn i

s
1 0,08 0,98 8,16
0,08 1,01 7,92
2 0,085 1,00 8,50
3 0,075 1,05 7,14
4 0,07 1,05 6,67
5 0,09 0,99 7,09
t chn i

c
1 0,098 1,24 7,9
0,1 1,25 8,0
2 0,10 1,26 7,9
3 0,099 1,25 7,92
4 0,105 1,23 8,54
5 0,103 1,27 8,10

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54
Bng 3.24: Kt qu phn tch iot trong cc mu t vn v t rung
H Ni v Thi Nguyn
K hiu mu
Hm
lng
iot di
ng
(ppm)
Hm
lng
iot ton
phn
(ppm)
T l
(%)
iot d
iot tp
Gi tr trung bnh
Iot di
ng
(ppm)
Iot
ton
phn
(ppm)
T l
(%)
iot d
iot tp
t vn
Thi Nguyn

vTN

1 0,11 1,26 8,73
0,11 1,25 8,80
2 0,098 1,25 7,84
3 0,12 1,24 9,68
4 0,099 1,23 8,05
5 0,103 1,27 8,11
t rung
Thi Nguyn

r TN
1 0,27 2,30 11,74
0,28 2,32 12,07
2 0,28 2,32 12,07
3 0,29 2,33 12,45
4 0,26 2,29 11,35
5 0,30 2,35 12,80
t vn
H Ni
(T Lim)

vHN
1 2,02 6,51 31,03
2,06 6,52 31,6
2 2,05 6,50 31,54
3 2,10 6,52 32,21
4 2,08 6,51 31,95
5 2,06 6,505 31,67
t rung
H Ni
(T Lim)

rHN
1 2,40 6,86 35,0
2,39 6,87 34,8
2 2,39 6,88 34,74
3 2,41 6,90 34,93
4 2,38 6,85 34,74
5 2,39 6,87 34,79


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55
* Nhn xt: Qua cc kt qu phn tch, chng ti c nhn xt sau:
- t vng Thi Nguyn ngho iot hn t H Ni.
- Vng t i th t nh i ngho iot hn t sn i v
ngho hn t chn i, iu ny c th gii thch t cao cng ln,
iot cng d b ra tri.
- t vn v t rung c hm lng iot gn tng ng nhau v
u cao hn t i, cng l do ma l iot min trung du b ra tri
nhiu hn vng ng bng, t vn v t rung trong cng mt vng
thng l ni thp, iot theo dng nc ra tri tch t li .
Nhng nhn xt trn hon ton ph hp vi tng iu tra v iot v bnh
bu c nc ta ca Unicef nm 1993. (xem bn trang 8)
Bng 3.25: Kt qu phn tch iot trong mt s mu nc
khu vc Thi Nguyn v H Ni
Loi nc
Gi tr
x
i
iot
tm c
(ppm)
n
x
x
i
=
1
2

n
) x x (
S
i 2

2
s S =
Tra bng t
n
S
t
f , o
c =
c = x
Nc
sui ly
Thi
Nguyn
1 0,001
0,0014 3.10
-7
0,000548 6,813.10
-4
0,0014
6,813.10
-4
2 0,001
3 0,002
4 0,002
5 0,001
Nc
khe ly
Thi
Nguyn
1 < 0,001
Lng rt
t khng
xc nh
c
- - - -
2 -
3 < 0,001
4 -
5 -

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56
Loi nc
Gi tr
x
i
iot
tm c
(ppm)
n
x
x
i
=
1
2

n
) x x (
S
i 2

2
s S =
Tra bng t
n
S
t
f , o
c =
c = x
Nc
ging
ly
Thi
Nguyn
1 0,002
0,0023 2.10
-7
4,472.10
-4
5,560.10
-4
0,0023
5,560.10
-4
2 0,0025
3 0,003
4 0,002
5 0,002
Nc
sng ly
H
Ni
1 0,003
0,0033 2.10
-7
4,472.10
-4
5,560.10
-4
0,0033
5,560.10
-4
2 0,0035
3 0,003
4 0,004
5 0,003
Nc
my ly
H
Ni
1 0,003
0,0032 2.10
-7
4,472.10
-4
5,560.10
-4
0,0032
5,560.10
-4
2 0,004
3 0,003
4 0,003
5 0,003

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57
Nhn xt: Kt qu phn tch iot trong nc ghi trong bng 3.25 cho thy.
- Ni chung lng iot trong nc rt thp. Cc kt qu xc nh c
nm trong sai s ca php o, chnh v vy c th ni, kt qu phn tch iot
trong nc khng th c nh gi c th c.
- Hm lng iot trong nc sui v nc khe thp nht, c l v nc
sui, nc khe c ngun gc t cc vng cao, t c hm lng iot thp
nn iot trong nc rt thp.
- Hm lng iot trong nc ging, nc sng v nc my gn nh nhau.
Bng 3.26: Kt qu phn tch iot trong mt s mu trng H Ni
Loi
mu
Gi tr
x
i
iot
tm
c
(ppm)
n
x
x
i
=
1
2

n
) x x (
S
i 2

2
s S =
Tra bng t
n
S
t
f , o
c =
c = x
Trng
g
1 4,90
4,88 3,25.10
-3
0,06 0,07 4,88 0,07
2 4,80
3 4,85
4 4,90
5 4,95
Trng
vt
1 5,84
5,84 1,72.10
-3
0,04 0,05 5,84 0,05
2 5,85
3 5,90
4 5,80
5 5,80
Trng
chim
ct
1 4,54
4,54 2,2.10
-4
0,015 0,018 4,540,018
2 4,52
3 4,55
4 4,56
5 4,54

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58
- Dng phng php thng k nh gi kt qu phn tch.
1 - Tnh gi tr trung bnh ca cc kt qu tm c
5
i 1
xi
x
5
=
=


2. Tnh phng sai:
5
2
i
2
i 1
(x x)
S
n 1
=

=


3. Tnh lch chun:
2
S S =
4. Tra bng t
o,f
= t
0,95, (5-1)
= 2,78

- Tnh tin cy
,f
S
t
n
o
c =
5. Gi tr thc nm trong khong
,f
S
x t
n
o
=
* Nhn xt: Cc kt qu phn tch iot trong trng ghi trong bng 3.26
cho php nhn nh nh sau:
- Trong trng vt c hm lng iot cao hn trng g v trng chim ct
iu ny c th gii thch thc n ca vt phong ph hn thc n ca g v
chim ct. Vt n c thc vt v ng vt (tm, tp, cua, c, ch, nhi, giun)
m thc n ng vt c hm lng iot cao hn, trong khi g v chim ct
thc n ch yu l thc vt (thc, ng)
- Trong c th ca ng vt iot tp trung tuyn gip, ngoi ra iot cn
tp trung c quan sinh sn, c th vi gia cm l trng. iu ny cn nghin
cu k hn chng minh. Nu iu ny ng th c th thng qua, vic phn
tch hm lng iot trong trng nh gi s thiu ht iot trong mi trng
sng v iu ny ng th c th ly hm lng iot c trong trng lm ch th
nh gi hin tng thiu ht iot ca cng ng. i vi con ngi qua ch

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59
s iot niu nh gi c thiu ht iot trong c th, nhng i chiu vi
cc loi gia sc, gia cm th ch s iot trong trng rt thun li cho vic nh
gi iot c trong mi trng sng: t v nc. Tuy nhin, c cng nhn
ch s iot trong trng l ch th th cn cn phi nghin cu nhiu, ton din
hn v phi nghin cu nh gi nhiu vng khc nhau.
Nu iu ny ng th rt c li, ta c th tng hay b sung iot vo thc n
cho gia cm tng iot trong trng v con ngi c th n trng b sung s
thiu ht iot, chc chn cch b xung ny thun li hn l n mui iot v iot
trong trng nm trong nhng hp cht m con ngi d hp thu hn l mui iot.

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60
KT LUN

Vi ti nghin cu phng php phn tch vi lng iot trong cc i
tng mi trng. Qua thi gian nghin cu lun vn t c nhng kt
qu sau:
1. nghin cu xy dng c quy trnh phn tch vi lng iot bng
phng php trit trc quang trn c s cc phn ng n gin d thc hin
l phng php trc quang UV-VIS da trn phn ng to phc mu ca
iot vi thuc th fucsin baz, l phc mu lin hp ion.
2. tin hnh cc thc nghim kho st.
3. nghin cu c quy trnh x l mu: mu t (dng phng
php kim chy) mu nc (dng phng php c cn mu), mu trng (x
l bng dung dch HNO
3
) t xy dng c quy trnh phn tch vi lng
iot theo phng php o quang i vi mu t, mu nc, mu trng. tin
cy ca cc quy trnh ny c nh gi qua cc yu t nh thu hi v
chnh xc.
4. p dng nhng quy trnh phn tch xy dng c phn tch
hng lot mu c th nh t, mu nc (nc ging, nc h, nc my),
mu trng v qua x l thng k cc s liu thc nghim thu c a ra
nhng nhn xt v hm lng iot trong cc i tng mi trng, cng nh
xc nh c mi tng quan gia chng
* Hm lng iot trong t (t i, t vn, t rung)
+ t vng thi nguyn ngho iot hn t H ni
+ t nh i ngho iot hn t sn i v ngho hn t
chn i.
+ t vn v t rung c hm lng iot gn tng ng nhau v
u cao hn t i.

S ha bi Trung tm Hc liu i hc Thi Nguyn http://www.Lrc-tnu.edu.vn
61
* Hm lng iot trong nc
Ni chung hm lng iot trong nc rt thp, cc kt qu xc nh
c nm trong sai s ca php o, chnh v vy c th ni, kt qu phn tch
iot trong nc bng phng php ny cha c nh gi c th c.
+ Hm lng iot trong nc sui v nc khe thp nht c lin quan
n nc sui, nc khe c ngun gc t vng cao
+ Hm lng iot trong nc ging, nc sng v nc my gn nh nhau
* Hm lng iot trong trng
C lin quan cht ch n ngun thc n ca gia cm v mi trng sng.
+ Trong trng vt c hm lng iot cao hn trng g v trng chim ct
do thc n ca vt phong ph hn ca g v chim ct
5. dng phng php thm v phng php thng k xc sut
nh gi cc kt qu phn tch thu c, qua kt qu phn tch trn mu trng
cho thy phng php c thu hi v chnh xc cao.
6. Kt qu nghin cu thu c gii quyt c nhng mc tiu m
lun vn ra, quy trnh phn tch iot n gin, d thc hin, ph hp vi
nhiu phng th nghim c s c kh nng phn tch hng lot mu vi thu
hi, chnh xc cao.

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62
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