TRNG H CNG NGHIP TP H CH MINH

VIN CNG NGH SINH HC & THC PHM

B MN:
PHN TCH THC PHM

TIU LUN

Ging vin hng dn:

Lp:

NGUYN C VNG
HTP 4 TLT

Tp. HCM, thng 11 nm 2011

VIN CNG NGH SINH HC V THC PHM

GVHD: NGUYN C VNG
B MN: PHN TCH NH LNG

TIU LUN:

DANH SCH NHM

STT
1
2
3
4
5
6
7
8
9
10
11
12
13

THNH VIN

Nguyn L Tho
Hong
Cp Th Thanh Huyn
Phm Th Lang
Mai Th Cm Nhung
Nguyn Th Hng
Nhung
Nguyn Phc Quang
inh Quang Thnh
Tn Thnh
H Hunh Phc
Thng
Trn Quc Thng
Bi Th Kim Thoa
H Thanh T
Nguyn Th Thy Vn

MSSV

NHIM V

10320561

Tm kim ni dung

10378431
10347691
10369471

Tm kim ni dung
Tm kim ni dung
Tm kim ni dung

10318501

Tm kim ni dung

10321621
10347681
10323171

Tm kim ni dung
Tng hp ni dung, chnh sa ni dung
Tm kim ni dung

10312591

Tm kim ni dung

10353351
10345141
10323591
10319101

Tm kim ni dung
Tm kim ni dung
Tm kim ni dung
Tm kim ni dung

Tp. HCM, thng 11 nm 2011

LI CM N

Qua thi gian thc hin bi tiu lun vi ch TM HIU V PHNG PHP
SC K TRAO I ION gip chng em hiu su hn v phng php Sc k trao
i ion trong Phn tch nh lng ca ngnh Ha hc cng nh trong ngnh cng ngh
thc phm, v phng php phn tch thc phm bng sc k trao i ion; ng thi gip
nng cao cc k nng cn thit khi lm bi tiu lun. c c nhng iu l nh s
gip ca mi ngi.
Chng em xin chn thnh cm n:
Trng H Cng Nghip HCM to iu kin cho chng em tt nghip c
tip tc hc lin thng ln i hc ti y.
Vin CN Sinh Hc V Thc Phm cung cp cc ti liu hc tp mn Phn tch
thc phm n chng em dng lm c s thc hin bi tiu lun ny.
Thy: Nguyn c Vng tn tnh hng dn cho c lp ni chung v nhm
chng em ni ring c th hon thnh trn vn bi tiu lun ny.
Gia nh, bn b ng vin v gip .

Tp. HCM, thng 11 nm 2011

Nhm: Sc k trao i ion

MC LC.
LI CM N...................................................................................................2
MC LC........................................................................................................3
PHN A. M U..........................................................................................6
1. T VN ....................................................................................................6
2. MC CH, YU CU.....................................................................................6
3. I TNG NGHIN CU............................................................................6
4. PHNG PHP NGHIN CU......................................................................7
5. PHM VI NGHIN CU..................................................................................7
6. KT QU NGHIN CU.................................................................................7
PHN B. NI DUNG.......................................................................................8
Chng 1. GII THIU V SC K..............................................................8
1.1. TNG QUAN V SC K............................................................................8
1.1.1. Vi nt lch s...............................................................................................8
1.1.2. Dnh ngha....................................................................................................9
1.2. PHN LOI V CC PHNG PHP TCH SC K............................9
1.2.1. Phn loi theo h pha....................................................................................9
1.2.2. phn loi theo c ch tch.............................................................................10
1.2.2.1. Sc k hp th............................................................................................10
1.2.2.2. Sc k phn b lng - lng........................................................................10
1.2.2.3. Sc k ion ( trao i ion)............................................................................10
1.2.2.4. Sc k ry phn t (sc k loi c)............................................................10
1.2.3. phn loi theo cch hnh thnh sc ...........................................................11
1.2.3.1. phn tch tin lu.......................................................................................11
1.2.3.2. phn tch th y........................................................................................11
1.2.3.3. Phn tch ra gii.......................................................................................12
1.3. CC LC LIN KT TRONG SC K.......................................................13
1.3.1. Lc lin kt ion.............................................................................................13
1.3.2. Lc phn cc................................................................................................13
1.3.3. Lc Van - de - Van (lc phn tn)................................................................14
5

1.3.4. Lc tng tc c bit..................................................................................14

1.4. S TNG TC GIA BA THNH PHN TRONG H SC K............14
1.5. MT S I LNG DNG TRONG SC K.........................................16
1.5.1. H s phn b KD v cch xc nh..............................................................16
1.5.2. S lin h gia tc di chuyn ca cht phn tch v KD ..........................17
1.5.3. Thi gian lu tR, thi gian lu hiu chnh tR ................................................17
1.5.4. Th tch lu Vm, th tch lu hiu chnh........................................................18
1.5.5. H s tch (cn gi l h s lu gi tng i).........................................18
1.5.6. Sc ...........................................................................................................18
1.5.7. a l thuyt.................................................................................................19
1.5.7.1. Khi nim a l thuyt..............................................................................19
1.5.7.2. a l thuyt c tnh thi gian khng lu gi, nef .....................................20
1.5.8. phn gii v cch lm tng phn gii..................................................20
1.5.8.1. phn gii...............................................................................................20
1.5.8.2. Cch lm tng phn gii........................................................................21
Chng 2. SC K TRAO I ION...............................................................24
2.1. KHI QUT V SC K TRAO I ION..................................................24
2.2. BN CHT CA QU TRNH SC K TRAO I ION..........................25
2.2.1. Ionit..............................................................................................................26
2.2.1.1. Nha trao i ion.......................................................................................26
2.2.1.2. Cationit......................................................................................................27
2.2.1.3. Anionit.......................................................................................................28
2.2.1.4. Ionit lng tnh..........................................................................................29
2.2.2. C ch trao i ion........................................................................................29
2.3. CC YU T NH HNG........................................................................31
2.4. THIT B NG DNG..................................................................................31
2.4.1. Mt s thit b sc k trao di ion dng trong phng th nghim..................31
2.4.2. ng dng ca sc k trao di ion trong phn tch nh lng......................33
2.5. SO SNH VI CC PHNG PHP KHC V TI U HA SC K
TRAO I ION..........................................................................................................34
2.5.1. im ging nhau...........................................................................................34
6

2.5.2. im khc nhau............................................................................................34

2.5.3. Ti u ha sc k trao i ion.......................................................................35
PHN C. TI LIU THAM KHO................................................................37

PHN A.

M U

1. T VN :
Ngy nay vi s php trin nhanh ca khoa hc cng ngh thc phm, to ra
nhiu to ra nhiu sn phm thc phm vi nhiu chng loi khc nhau p ng
nhu cu ngy cng cao ca con ngi.
C nhiu loi thc phm d b h hng hoc ko di thi gian bo qun, t
dc ngun nguyn liu hay sn phm nh mong mun cn s dng cht bo qun hay
thuc bo v thc vt, nhng c nhiu khi ngi ta s dng vt qu nng cho php
gy nh hng xu n ngi tiu dng, thit hi ln n doanh nghip, tn tht nn kinh
t Quc gia. S ra i v pht trin ca ngnh phn tch thc phm d to ra nhiu thit
b phn tich nhanh v chnh xc cung gii quyt mt phn no v cc vn ny.
V th, nhm chng em quyt nh chn mng phn tch thc phm bng phng
php sc k, kt hp vi phng php trao i ion thc hin nghin cu mt ti
hon chnh, l: Tm hiu v phng php sc k trao i ion
2. MC CH, YU CU:
Mc ch:
- tm hiu chung v phn tch thc phm bng phng php sc k.
- tm hiu v bn cht, cc yu t nh hng, thit b ng dng v so snh vi
cc phng php khc t nhm khc phc nhng nhc im nhng hn ch ca
phng php sc k trao i ion nng cao tnh kh dng ca phng php ny.
Yu cu:
- Vn dng side bi ging ca thy Nguyn c Vng, cc cun sch v cc ti
liu t nhiu ngun chuyn v phn tch thc phm bng sc k trao i ion nghin
cu v phng php ny.
3. I TNG NGHIN CU:
- Bn cht ca qu trnh sc k trao i ion
- Cc yu t nh hng
- Thit b v ng dng ca phng php ny
8

- So snh vi cc phng php phn tch thc phm khc

4. PHNG PHP NGHIN CU:
- Tm kim ni dung t nhiu ngun
- Tp hp ni dung
- Bin tp li thnh bi hon chnh
-
5. PHM VI NGHIN CU:
- Bi tiu lun c nghin cu v thc hin trong khong 2 tun, c thc hin ti
trng H Cng Nghip HCM
- Thng tin trong bi tiu lun c su tm t nhiu ngun.
6. KT QU NGHIN CU:
- Lm r c bn cht, c ch ca qu trnh
- Tm hiu su hn v sc kh trao i ion
- Tm ra c nhng yu t nh hng n qu trnh
- Nu c nhng ng dng v thit b trong chuyn ngnh phn tch thc phm.
- So snh u v nhc im vi cc phng php khc
- ra c nhng bin php cho s ti u ha ca sc k trao i ion.

PHN B.

NI DUNG.

Chng 1. GII THIU V SC K.

1.1. TNG QUAN V SC K.
1.1.1. Vi nt lch s.
Phng php sc k c pht trin vo nm 1903 do nh thc vt hoc ngi Nga
Michael C.Txvet.ng thc s l ngi u tin c cng tm ra phng php, gii quyt
vn tch cc cht c tnh cht ging nhau theo mt c ch c o, hon ton khc vi
phng php tch tng c trc y, tuy nhin pht hin ny b lng qun nhiu
nm.
Nm 1941, Martin v Synge pht trin sc k phn b trn giy v a ra l
thuyt a gii thch cc qu trnh sc k, cc tc gi ng dng tch cc ancaloit
t cc cy thuc phc v cho ch to dc phm. Do c cng trong vic pht trin l
thuyt ca phng php
cho nn nm 1952 hai
ng c nhn gii
thng Nobel v ho
hc.
Cng t nm 1952
nhng my sc k mi
ra i t ra c u th do
c hiu qu tch rt
cao. Ct mao qun v
cc detect sau ny
c ci tin tng
phn gii v nhy
ca phng php ngi
ta c th phn tch c cc cht c hm lng nh c ppm v ppb. T y phng php
c pht trin nhanh, ng dng c nhiu trong thc t.
10

V sc k lng mt k thut mi c pht hin t nm 1970 lm tng hiu qu tch

l sc k lng hiu nng cao (high performance lipuid chromatography- HPLC): Cht
nhi ct c ci tin, my tnh v thit b vo b tr c a vo, tng cng kh
nng ca phng php.
Ngy nay k thut ghp ni gia sc k v cc phng php khc c p dng.
l k thut ghp ni gia sc k v khi ph ( GC-MS, GC-MS) sc k v cng hng
ht nhn, sc k a chiu, sc k in mao qun (CEC)... Phng php c chnh xc
v nhy rt cao, phn tch c nhiu i tng phc tp hn.
1.1.2. Dnh ngha.
Sc k l qu trnh tch da trn s phn b lin tc cc cu t cht phn tch trn
hai pha: mt pha thng ng yn c kh nng hp th cht phn tch gi l pha tnh, mt
pha di chuyn qua pha tnh gi l pha ng; do cc cu t cht phn tch c i lc khc
nhau vi pha tnh, chng di chuyn vi tc khc nhau v tch ra khi nhau.
1.2. PHN LOI V CC PHNG PHP TCH SC K.
1.2.1. Phn loi theo h pha.
Phng php u tin c nhiu ngi quan tm, y l phng php phn loi
n gin theo h pha tc l cht phn tch phn b gia hai pha l g?
S phn loi cc phng php sc k:

h
pha

C ch
11

1.2.2. phn loi theo c ch tch.

1.2.2.1. Sc k hp th.
sc kh hp th l phng php da trn c s phn b cht phn tch gia pha tnh
v pha ng nh tng tc phn t thng qua cc trung tm hp th. Pha tnh l cc cht
rn hoc lng c din tch b mt ln, bn vng v mt ho hc. Chng hp th cht phn
tch trn b mt ca chng cc mc khc nhau khi cho pha ng cha cht phn tch
tip xa vi chng. Tu thuc lc lin kt gia pha tnh v tng cu t cht phn tch c
trong pha ng, khi cho pha ng i qua pha tnh chng s di chuyn vi tc khc
nhau.
1.2.2.2. Sc k phn b lng - lng.
s phn bit gia sc k phn b lng-lng v s phn b thng thng l ch sc
k phn b lng - lng cn c gi l sc k chit, pha tnh l cht lng pha ng cng
l cht lng, s phn b cht phn tch gia hai pha lng ging nh qu trnh chit, cn
s phn b ni chung l s phn chia cht phn tch vo hai pha khng cn xt ti lng
hay rn.
im khc nhau c bn gia sc k phn b lng - lng v sc k hp ph l ch:
sc k phn b lng- lng c ng ng nhit tuyn tnh khong nhit ln, phng
php c nhy cao nhng c nhc im l pha tnh khng c bn vng, hin tng
tri mt pha tnh lm cho lp li b gim.
1.2.2.3. Sc k ion ( trao i ion).
pha tnh thng l pha rn c kh nng trao i ion ca n vi cc cht phn tch
trong pha ng.Cht c kh nng trao i cation gi l cationit, cn cht c kh nng trao
i anion gi l anionit. Lc lin kt ch yu gia cht phn tch v pha tnh ch yu l
lin kt tnh in , ph thuc nhiu vo in tch ca ion cht phn tch, pH ca dung dch
v bn knh hidrat ho ca cc ion cht phn tch. V d: phn ng trao i ion gia
cationit acid mnh v Ca2+ c th vit nh sau:
2R-SO3H + Ca2+ = (R-SO3)Ca + 2H+
Phn ng ca anionit baz mnh vi Cl- :
R-N(CH3)3OH + Cl- = R-N(CH3)3Cl

+ OH-

1.2.2.4. Sc k ry phn t (sc k loi c).

12

Pha tnh l cc cht rn c din tch b mt ln, xp, c nhng ng i trong lng
cht rn, cn gi l mao qun c kch thc c phn t. Cc phn t cht phn tch c
th thm vo cht mc khc nhau tu theo kch thc ca chng. Cc cht phn
tch c kch thc ln khng th i vo su vo pha tnh c, s b ra gii nhanh cn
cc phn t cht phn tch c kch thc nh phn b su vo pha tnh s b ra gii
chm. Th t ra gii l cc cht c kich thc nh i ra sau v ngc li. Thi gian lu
ca cc cht t l nghch vi kch thc phn t ca chng. Tuy nhin cht phn tch c
th c tng tc khc vi pha tnh. Nh vy mt php sc k c th tch theo mt hay
nhiu c ch khc nhau m chng ta khng xt y.
1.2.3. phn loi theo cch hnh thnh sc .
1.2.3.1. phn tch tin lu.
cc cu t A, B, C c i lc vi pha tnh l A < B< C. Cho hn hp cht phn tch
lin tc i qua ct, cht phn tch c i lc vi pha tnh thp nht i trc, tip theo l
cht c i lc yu hn. Tuy nhin do chng ta cho lin tc cht phn tch vo nn i sau
A l A + B v A+B+C. ch c mt phn cht tinh khit A i trc
nng

A A

C
B
A

t. V

Sc phn tch tin lu

1.2.3.2. phn tch th y.
trong sc k ny, chng ta cng np lng nh hn hp cht phn tch A, B, C vo
ct sau cho cht D l cht y lin tc i qua ct. i lc hp th l A<B<C<D. Do D
y C, C li y B,B li y A nn sc c dng nh sau:

13

nng

t,V

Sc phn tch th y
1.2.3.3. Phn tch ra gii.
a mt lng nh mu bao gm cc cht A, B, C vo ct sau dng cht E c i
lc hp th vi pha tnh yu nht ra gii lin tc. C A, B, C, E u tan tt trong pha
ng . Th t i lc hp th l E<A<B<C. Mt cu hi t ra lm sao E c i lc hp th
yu nht vi pha tnh li c th ra gii A, B, C ? tr li cu hi ny chng ta hnh
dung l s tranh chp nhng trung tm hot ng pha tnh khng phi ch c mt cu t
cht phn tch tng tc vi cu t cht ra gii m y c th c nhiu cu t ra gii
tham gia (cu t c th l ion hoc phn t).
Gi s c cht tan C(phn t hoc ion) hp th vo pha tnh, phn b C tr li
pha ng phi cn ti nhiu cu t ra gii E. Quy lut u th s ng xem ra c tc
dng. V vy khi ra gii ngi ta thng cht ra gii c nng ln hn cht phn tch
rt nhiu.
chiu cao(h)
din tch(S)
thi gian(t)
Sc phn tch ra gii
Tm li mt php sc k nhn theo cch phn loi no cng c th lin quan n
mt hay nhiu cch phn loi khc, th d sc k lng- rn ch n gin l pha tnh l
cht rn, pha ng l cht lng theo cch phn loi theo lin kt pha nhng theo cch
phn loi theo c ch th lng rn y c th l hp ph,trao i ion. Tu theo pha tnh
14

s dng, sc k lp mng c th l sc k trao i ion, hp ph, phn b, ry phn t.

Ngc li sc k hp ph xt v mt tng tc pha c th thuc loi sc k - rn hay
lng - rn.
Sc k ra gii c ng dng nhiu trong lnh vc phn tch do hiu qu tch cao.
1.3. CC LC LIN KT TRONG SC K.
Trong h sc k c ba thnh phn ch yu tc quyt nh s tn ti ca h, cht phn
tch, pha tnh, pha ng to nn s phn b cn thit, gip cho s di chuyn cc cht phn
tch dc theo chiu di ct vi tc khc nhau. Chng ta thng ni cht phn tch phn
b gia hai pha, tuy nhin y la cn bng ng cht phn tch lun thay i pha lin kt
(tr mt s trng hp c bit n ch mt pha trong sut qu trnh phn tch) vn l
ti sao cht phn tch c gi trong pha tnh? Hn na ba thnh phn ny tng tc nh
th no vi nhau, bng cc lc lin kt no m kt qu cc cht phn tch li phn b vo
pha tnh mc khc nhau? Cu tr l do bn cht cc ca cc thnh phn trong h sc
k. Cht phn tch c th l ion, phn t trung ho hay cht phn cc, i tng lin kt
ca n cng c th l ion, phn t, cht phn cc. Nh vy tuy thuc vo ln ca in
tch kich thc phn t, phn cc m chng tng tc vi nhau theo cc lc lin kt
khc nhau. Ngi ta chia cc lc lin kt thnh bn loi:
1.3.1. Lc lin kt ion.
trn b mt pha tnh c cc trung tm hot ng l ion. l cc phn t c kh
nng phn ly to thnh cc ion, to nn trung tm hot ng ion chung tham gia lin kt
vi cc ion cht phn tch trong dung dch theo lc tng tc tnh in gi l lin kt ion.
gi cc anion cht phn tch trong dung dch pha tnh cn c cc trung tm cation trn
b mt, v ngc li gi cc cation cht phn tch trong dung dch pha tnh cn c cc
ctrung tm anion cng tng t, pha ng cng c cc trung tm hot ng l cc ion,
chng tham gia tng tc vi cht phn tch v pha tnh. Chng c kh nng phn li trong
dung dch to thnh cc cation v anion. Th d khi ra gii cc ion kim loi trn ct
cationit, ta c th dng pha ng l dung dch HCl long. Cc phng php sc k
thng gp c s tham gia ca cc lin kt ion gi l sc k ion, sc k cp ion.
1.3.2. Lc phn cc .
Trong phn t cht phn tch, cht ra gii trong pha ng cng nh cc phn t
trn b mt pha tnh c cc trung tm phn cc, chng c th l cc lng cc in c
15

nh, cng c th l cc lng cc in do cm ng. Cc trung tm phn cc ca cht ny

lin kt vi trung tm phn cc ca cht khc bng lc lin kt phn cc. S phn cc
trong cc phn t i khi rt nh v s chnh lch v phn cc cng rt nh. Tuy
nhin, s chnh lch ny l yu t quan trng c bn lin kt khc nhau, l iu
cn thit phn chia chng trong cc php tch sc k.
Th d: cc Cresol (o-, m-,p- cresol) ch khc nhau v v tr nhm CH 3- trong phn
t. Chnh s khc nhau v v tr ny lm cho mt electron trong phn t cresol khc
nhau to nn mt s khc bit nh v phn cc, t lc lin kt vi pha tnh khc
nhau. L nguyn nhn chnh lch thi gian lu trong qu trnh sc k.
1.3.3. Lc Van - de - Van (lc phn tn).
Lc ny c bn cht in, tuy nhin khng h c cc in trong mng li phn t,
cng khng lin quan ti phn t lng cc hay c nh. Tng tc phn tn in hnh l
mch hidrocacbon n l tng tc phn t .
Th d n-heptan l cht lng ch khng phi l cht kh s tng tc gia cc phn
t n-heptan l lc phn tn ln gi cht ny trng thi lng. tch cc
hidrocacbon ngi ta dng hidrocacbon khc lm pha tnh.
1.3.4. Lc tng tc c bit.
Lc tng tc c bit l lc tng tc to thnh do cc lin kt hydro, lin kt cho
nhn m c.S hnh thnh lin kt gi nguyn t hidro v cc nguyn t c m in
cao nh O, N, F... gi l lin kt hidro. Khi tham gia lin kt, cc electron cn gi l m
my electron chuyn dch sang nguyn t c m in ln hn. Nh vy cc nguyn t
c m in cao hn, lin kt hidro cng bn cht.
1.4. S TNG TC GIA BA THNH PHN TRONG H SC K.
Khi np cht phn tch vo h sc k, n c phn b gia hai pha, pha tnh v pha
ng, tu theo lc lin kt gi tng pha vi cht phn tch m chng c thi gian pha
no nhiu hn. Nh vy thc cht l ba thnh phn trong h sc k tng tc vi nhau,
pha tnh, pha ng, v cht phn tch. Ta xt tng thnh phn v quan h ca chng.
Pha tnh phi lu gi c cht phn tch, tuy nhin tch c cc cht, n khng
c gi qu cht cht phn tch c iu kin phn b vo pha ng v sau , mt
thi im khc, n li b hp th vo pha tnh. Cc cht phn tch c tnh cht cng ging
nhau s phn b cng phi lp i lp li nhiu ln, y ta mun ni n s ln phn b
16

t cn bng hay s a l thuyt phi ln tch c hiu qu, do cc vn vt

liu lm pha tnh, chiu di ct tch v cch np ct cng cn c quan tm. Ngy nay
ta c th s dng nhng ct c sn trn th trng nhng i khi, cng mt loi pha tnh,
cc hng khc nhau c th to c cc sn phm vi tnh cht khc nhau.
Vn tip theo l pha ng v cch vn hnh tc l tc pha ng, nhit ,
lng mu a vo ct, ti sinh ct...Pha ng phi ho tan dc cht phn tch, tuy
nhin thnh phn pha ng phi ph hp sao cho cht phn tch khng b gi qu lu
pha ng n c th lin kt tr li vi pha tnh.
S tng tc gia pha ng v pha tnh cng l vn cn bn. Pha ng khng
c lm nh hng ti pha tnh, khng lm thay i tnh cht ho l ca pha tnh. Pha
ng khng c lin kt vi pha tnh mt cch qu bn vng to iu kin cho cc
cht phn tch c th phn b vo pha tnh c. Ngoi ra tc pha ng, nhit h
trong c nhit ca tng b phn ring, c bit l trong sc k kh phi c quan
tm khng ch mt cch cht ch.
lm sng t vn trn ta ly mt v d tch cc ion kim loi M+ bng phng
php sc k trao i ion. Pha tnh l cationit axit mnh, nhm trao i l R-SO 3H: Pha
ng l dung dch m c cht ra gii l H+. S tng tc ca ba i lng trn c
miu t bng hnh sau:
cht phn
tch M+

Pha tnh
R-SO3-

Pha ng
H+

S tng tc ca 3 i lng ch yu trong h sc k

Pha tnh (RSO3) c kh nng hp th cht phn tch theo phn ng sau:
R-SO-3 +M+

R-SO3M *

Mt khc cht ra gii trong pha ng cng tng tc vi pha tnh theo phn ng
R-SO3- + H+

R-SO3H **

Ion kim loi M+ cn lin kt vi pha tnh mt mc khng qu bn vng, phn

ng hp th y l phn ng thun nghch. Cn bng phn b l cn bng ng v hp
17

cht R-SO3M c lin kt bn vng sao cho M+ d dng i vo pha ng. n lt H+,
khng c lin kt bn vng vi R-SO3-, ni mt cch khc l nng H+ khng qu
cao sao cho phn ng ** xy ra thun nghch. Mt khc tng tc gia M + v H+ l tng
tc ph nh nhau, cnh ranh nhau. Chnh H + l yu t cnh tranh cho phn ng ** xy
ra. Nh vy vai tr ca nng cht ra gii,(H+) y rt quan trng n c gi tr ph
hp sao cho hiu qu tch tt nht. Phng php a thm cht to phc vo pha ng
cng thng c p dng trong sc k trao i ion.
1.5. MT S I LNG DNG TRONG SC K.
1.5.1. H s phn b KD v cch xc nh.
Cu t A phn b gia pha ng v tnh khi cn bng c thit lp
As

Am

(1)

H s phn b c nh ngha l t s ca nng cht phn tch gia hai pha

DK =

[ A] m
[ A] s

(2)

Trong : [Am ] l nng cht phn tch trong pha ng

[As ] l nng cht phn tch trong pha tnh
Cn bng phn b trong pha kh gi l cn bng ng l cn bng gia lng lng, kh-lng, rn-lng. Gi s cht phn tch c phn b phn no ca ct, a
th n. Nhng do pha ng di chuyn, cht phn tch li i xung a th (n+1) v y
li thit lp cn bng mi ca c a th n v n+1.
cn bng thit lp nhanh mt yu cu rt cn thit l lp pha tnh phi mng, h
s khuch tn ca cht phn tch trong pha tnh ln hn h s khuch tn trong pha ng.
H s phn b KD c th c xc nh theo phng php tnh bng cch o nng cht
phn tch trong pha ng v nng cht phn tch trong pha tnh sau khi t cn
bng. Mt cch gn ng KD c xc nh theo cng thc sau:

KD =

( M M1 ) .
M 1. m

V
(3)

Trong : M l lng cht ban u tnh bng mg

M1 l lng cht phn tch cn li sau khi tip xc mg
V l th tch pha ng ml
18

M l lng cht hp th, gam

1.5.2. S lin h gia tc di chuyn ca cht phn tch v KD .
Cht phn tch A mun di chuyn c phi pha ng. Gi f A l phn thi gian A
fA =

pha ng:

[ A] m .Vm
[ A] m .Vm + [ A] s .[ V ] s

(4)
fA =

chia c t v mu cho [A]m . Vm ta c:

fA =

1
1+ KD

VS
Vm

(5)

1
1+ f A

Hay

(6)

Trong kA l h s dung tch.Tc tuyn tnh ca cu t A trong pha ng l:

uA = u.fA = u / (1+fA)

(7)

U l tc tuyn tnh ca pha ng (cm/s). T biu thc (6) v (7) ta c nhn xt:
Khi DK hoc fA cng ln ; thi gian cht phn tch trong pha ng cng t, ni cch khc
l cht phn tch di chuyn cng chm, ngc li khi fA cng nh, cht phn tch di
chuyn cng nhanh.
1.5.3. Thi gian lu tR, thi gian lu hiu chnh tR .
Thi gian lu tR l thi gian lc bt u bm mu vo u ct ti khi pic t gi tr
cc i.
(8)

tR =

L
L(1 + k A )
=
uA
u

L/u l thi gian m cu t khng lu gi trn ct cn gi l thi gian cht

(9)

Vs
t R A = tm
1 + K D . V
m

= tm (1 + k A )

thi gian lu hiu chnh tR l thi gian lu khng tnh thi gian cht
19

(10)

tR A

"
R

'
R

t
V
=t R A tm =tm k => k =
=
1.5.4. Th tch lu V , th tch lu hiu chnh.
t mu vo ctVm
Th tch lu V l th tch ca dung dch ra gii t khi bt u bm m
'

'

cho n khi pic t cc i. Gi F l tc chy ca pha ng ml/pht,th tch lu V R

c tnh theo cng thc:VRA = tRAF; Vm = tmF
VRA = Vm(1 + k)

(11)

Th tch lu hiu chnh VR l th tch lu loi i th tch trng ca ct

VR = VR Vm = VmkA = KDAVS
Th tch lu ring Vg l th tch ring cho cu t, l th tch dung dch ra gii
ra cht phn tch trong mt n v trng lng hay th tch ca pha tnh
VRA
= K DA = Vg
VS

(12)

1.5.5. H s tch (cn gi l h s lu gi tng i)

H s tch l i lng nh gi kh nng tch hai cht bng phng php sc k.
N ph thuc vo h s phn b ca chng v t s ca h s phn b ca hai cht: mt
cht phn tch A v mt cht khc B hoc mt cht chun.
iu kin hai cht tch khi nhau l 1
=

k
K DA
= A' 1
K DB k B

(13)

Ni mt cch khc h s phn b ca hai cht A v B gia pha tnh v pha ng

phi khc nhau. Mt khc t s th tch lu ca hai cht, tRA/ tRB cng chnh l t s ca
h s phn b.
Vy c th tm tt l:

'
k
K DA
t'
VRA
= A' = RA
=
'
'
K DB
k B t RB
VRB

(14)

1.5.6. Sc .
Sc l s biu din s ph thuc din tch (S) hoc chiu cao (h) tn hiu o c
c th l hp th quang,cng c th l dn in hoc l tn s xung in ...lin
quan cht ch ti nng cht phn tch c trong mu v thi gian. Cc tn hiu ny
c gi l pic sc k. tnh ton hm lng cht phn tch, tnh din tch pic sc k
20

l chnh xc nht.Ngy nay hu ht cc my hin i u c trang b cc thit b tnh

din tch ca pic sc k mt cch t ng.
t RB .VRB

S, h

'
'
t RB
,VRB

t RA ,VRA
'
t ' RA , VRA

tm

t, V
t0
WB

WA

Sc hai cu t A&B
1.5.7. a l thuyt
1.5.7.1. Khi nim a l thuyt:
a l thuyt l phn no ca ct m cn bng c thit lp. Theo quan
nim ca Martin v Synge, cn bng c thit lp nhanh chng, tc thi. Tuy nhin
iu ny gp kh khn khi gii thch hin tng gin rng vng mu, hin tng pic sc
k khng cn i. Amundson v Lapidus v sau l Van Deemter cho rng a c
cn bng khi t cn bng chuyn khi lng cht tan t pha ng vo pha tnh v ngc
li v tc gi a ra thuyt
tc .

Xc nh s a l thuyt thc nghim

21

Nh vy c th ni rng phn nh ca ct gi l a l thuyt khi t c cn bng

phn b cht phn tch.
Gi n l s a l thuyt, l lch chun; ~

. i vi ct sc k n cng

ln pic cng hp, thi gian lu t l vi s a l thuyt n, tR ~ n, nn ta c th vt:

2
tR
n
tR
=
hay n =

mt khc w = 4 hay =

W
4

s a l thuyt c th vit li l:

(14)
1.5.7.2. a l thuyt c tnh thi gian khng lu gi, nef .
nef

( t t )
=16 R m=
w

16
t= (
W2

'
R

t R2
k2
k2
nef = 16 2
= 2n .
w (1+ k )
1
+( k

) Wt16k
2

2 '
m

(15)

V t (8) ta c tm= tR/(1+k). Chiu cao a l thuyt hiu lc c tnh:

Hf =

t (15) v (16) ta c:
H ef

L
nf

L
=
16

(16)

w 2
= H
tm
( tR

(1 +k )
'

k'

(17)

1.5.8. phn gii v cch lm tng phn gii.

1.5.8.1. phn gii.
phn gii ni ln mc tch cu t khi nhau trong mt php tch sc k. Hai
cu t A v B c tch khi nhau cng trit , phn gii cng cao. phn gii
c nh gi qua cc i lng c trng l: thi gian lu, tRA, tRB v rng peak WA, WB.
phn gii R c tnh theo cng thc:
22

R=

2( t RB t RA )
WA + WB

(18)
Trong : tRB tRA= tR l s chnh lch thi gian lu(cng c th dng th tch lu
VRA- VRB)ca hai cu t A v B. i lng ny c so snh vi tng bn chiu rng pic,
o bng giy hoc mililt, ni ln kh nng tch ca ct.
Khi tng chiu di ct, s a l thuyt tng: tR ~ n, chiu rng pic t l vi
vy

R~

n
n

hay

R~

1.5.8.2. Cch lm tng phn gii

Cch th nht: Da trn s thay i cu trc ct. Trong phng php ny c cc
bin php: Tng chiu di ct, s dng cht nhi c kch thc ht nh hn, ng u
hn, thay i pha tnh v cui cng l gim ng kinh ct
Cch th hai: Da trn cch vn hnh ct: l ti u ho tc pha ng, gim
lng mu, gim nhit ct (GC) v cui cng l thay i thnh phn pha ng (LC)
Thuyt tc , phng trnh Van Deemter:
thuyt c cc tc gi Lapidus v Amundsion a ra nm 1952, sau ny c Van
Deemter pht trin.
Theo thuyt ny cc yu t: ng knh ht nhi, k thut np ct v cc yu t tc
ca pha ng, h s khuch tn ca cht phn tch trong pha ng v pha tnh nh
hng rt nhiu ti s gin rng vng cht phn tch hay rng ca pic trong sc .
i lng c trng cho gin rng ca vng cht phn tch l chiu cao a l thuyt
H, c hnh thnh do ba thnh phn H1,H2, H3.
H = H1+H2+H3 (19)
H1 l i lng khuch tn xoy, c trng cho s ng u ca ct nhi, ng
knh ca ht nhi, kh nng np ct.
H1 = 2dp

(20)

Trong l h s np ct, nu np ct tt th = 1,5; dp l knh ht nhi.

23

H2 l i lng khuch tn theo chiu dc. N c hnh thnh do s khuch tn ca

cht phn tch v hai u ca ct, ph thuc vo tc ca pha ng, h s khuch tn
ca cht pht phn tch trong pha ng, ng i ca cht phn tch, c biu din bng
phng trnh:
H2 = B/u trong B= 2Dm
L i lng c trng cho h s khuch tn ca cht phn tch trong pha ng v
h s ng i ca n. Trong iu kin np ct tt, ng i ca cht phn tch khng
qu khc khuu, = 1; Dm l h s khuch tn ca cht phn tch trong pha ng, nh
vy H2 c th vit li l:
H2 = 2Dm/u

(21)

H3 l i lng c trng cho qu trnh chuyn khi lng l yu t ph thuc vo

tc hp th v gii hp. Qu trnh ny ph thuc vo c pha ng v pha tnh, v vy
H3 c th vit: H3= (CS - Cm)u (22)
Trong Cs l h s dc trng cho qu trnh chuyn khi lng ca cht phn tch
trong pha tnh, ph thuc vo pha tnh, n c gi tr nh khi tc dng F1ml/pht, C s
0

Cs= K.df2/Ds

(23)

Trong : K- h s
Ds- h s khuch tn cht phn tch trong pha tnh
df2- chiu dy pha tnh

H
Cu
H min

B
u

A
utu

u , cm / s

ng cong Van Deemter

24

Cm l hng s chuyn khi ca cht phn tch trong pha ng, ph thuc vo pha
ng, c xc nh theo biu thc:
Cm = dp2/Dm

(24)

l h s thc nghim c gi tr t 0,5- 1

Dm l h s khuch tn ca cht phn tch trong pha ng.
Tng hp li H c biu thc tng qut l:
H = 2dp + 2Dm/u + (Kdf2/Ds + df2/Dm)/u

(25)

Phng trnh trn c vit tt l:

H = A+B/u +Cu

(26)

Trong thc t c th tnh gn ng H= 3-4dp

xt cc tiu chiu cao ca a l thuyt ly o hm ca phng trnh Van
Deemter ta c: H= -B/u2 +C, ti cc tiu H=0 => ut =

25

B
C

Chng 2. SC K TRAO I ION

2.1. KHI QUT V SC K TRAO I ION.
Sc k trao i ion (IC) l mt phn ca sc k lng (LC). Theo Lin minh Quc t
ca C bn v ng dng Ha hc (IUPAC) sc k trao i ion c nh ngha nh sau:
"Sc k trao i ion da trn s khc bit ca cc phn t gn nhau tao i ion vi nhau
trong cht phn tch. Nu cc ion v c c tch ra v c th c pht hin bi cc
my o dn hoc bng cc tia UV pht hin gin tip sau cng gi l sc k ion".
V mt vi l do m nh ngha ny khng c s dng. K thut pht hin cn c
xem xt ring bit t c ch phn tch hin c. Ngoi ra, mt hn ch ca sc k ion cc
ion v c l kh hiu trong thc t khi s dng trong h thng cho c hu c v cc
ion v c c th c tch ra v xc nh cng mt lc.
Mt nh ngha tng qut hn v ph hp hn xc nh ion sc k: Ion sc k
bao gm tt c cc phn tch sc k lng nhanh chng ca cc ion trong cc ct cng
trc tuyn vi pht hin v nh lng trong dng chy thng qua mt my d. nh
ngha ny c trng cho sc k ion khng phn bit ca c ch tch v pht hin phng
php trong khi ti cng mt thi gian nht nh. Sau y nguyn tc ca s phn tch p
dng trong sc k trao i ion:
trao i ion
hnh thnh cp ion
ion loi tr
Phng php sc k c xc nh bi c ch tch tnh hoc tch ng c s
dng. Ngy nay sc k
trao i ion ch n
gin l c gi l sc
k ion (IC), trong khi
cp sc k ion (IPC) v
sc k ion loi tr
(IEC) c coi nh l
cc ng dng chuyn
su hn.
26

Sc k trao i Ion (IC) l mt qu trnh cho php phn tch cc ion hay cc phn t
phn cc da trn tnh cht ca chng. Hin nay, ti Vit Nam c kh nhiu h thng sc
k ion ca nhiu hng ni ting khc nhau. i vi h Metrohm, min Bc c rt nhiu
Vin nghin cu, Trung Tm,...s dng cc my nh 881, 882, 861,...cn Thnh ph H
Ch Minh, c Trung Tm Dch V Phn Tch Th Nghim ang s dng l 850 IC
professional. y l h thng phn tch Ion c nhiu u im v tin li cho phn tch
vin: - Phn tch cc Cation - Phn tch cc Anion - Phn tch hp cht: polyphosphate,
tripolyphosphate, choline,... Kh nng phn tch ppb - ppm - % chnh xc cao. i km
vi phn mm MagicNet d dng s dng.
Sc k trao i ion da trn hin tng trao i thun nghch gia cc ion linh ng
ca pha tnh rn vi cc ion trong DD phn tch, khi cho DD ny i qua ct c np y
pha tnh. Cc pha tnh trong trng hp ny c gi l cht trao i ion
2.2. BN CHT CA QU TRNH SC K TRAO I ION.
Sc k trao ion da trn hin tng trao i thun nghch gia cc ion linh ng
ca phn t tnh rn vi cc ion trong dung dch phn tch, khi cho dung dch ny i qua
ct c np y pha tnh. Cc pha tnh trong trng hp ny c gi l cht trao i
ion, bn cht ca cc qu trnh phn tch l do i lc khc nhau ca cc ion trong dung
dch i vi cc trung tm trao i ion ( nhm cha ion) ca ionit.
Sc k trao i ion (IC) c da trn mt phn ng ha hc stoichiometric gia
cc ion trong mt mng li v mt cht rn thng thng mang theo cc nhm chc
nng m c th sa cha cc ion nh l mt kt qu ca in cc. Trong trng hp n
gin trong sc k cation y l nhng nhm axit sulfonic, anion sc k l amoni nhm
bc bn. Trong cc ion l thuyt vi cng bn cht c th c trao i hon ton thun
nghch gia hai giai on. Qu trnh trao i ion dn n mt iu kin ca cn bng.
Trao i Ion thng thng bao gm cc giai on vng chc trn b mt c cc
nhm ion c c nh. Bi v cc iu kin ca electroneutrality lun lun c mt in
tch tri du khi nhn ion trong vng ln cn ca cc nhm chc nng. Ion nhn thng
bt ngun t giai on di ng v do cn c gi l eluent ion. Nu mu c b
sung, trong c hai ion cht phn tch A- v B- sau mt thi gian ngn thay eluent
ion E- v c gi li c nh trc khi chng ln lt trao i ion eluent. i vi anion
sc k kt qu ny trong cn bng th hi phc sau y:
27

(1)
(2)
2.2.1. Ionit.
Ionit l hp cht polymer v c v hu c khng tan c cha nhm hot ng, bao
gm ionit v c t nhin (nhm zeolite, nhm t st, nhm glauconit,) ionit v c
tng hp (cc xenlulose nh permunit, zeolite) v cc hu c t nhin v cc ionit hu
c tng hp, c gi l nha trao i ion.
Cc ionit v c v hu c t nhin t c s dung trong thc t v c bn c v
bn ha v kh nng trao i ion thp. c s dng nhiu nht l cc ionit hu c
tng hp chc nha trao i ion.
2.2.1.1. Nha trao i ion.
Nha trao i ion c cu to hp cht polymer hu c gm cc
sn hydrocarbon c mang cc nhm cht hot ng. cc nhm chc ny
ni vi cc ion linh ng bng lc ht tnh in. C hai loi na chnh:
cation (nha trao i cation), anion (nha trao i anion). Ngoi ra cn c
cc loi ionit c bit nh ionit lng tnh (trao i c anion v cation) ionit c cha
nhm to phc: Ionit cha nhm oxy ha kh: ionit lng v c mng trao i ion.
+ Tnh cht vt l ca nha.
Mu sc: vng, nu, en, thm. Trong qu trnh s dng nha, mu sc ca nha
mt hiu lc thng thm hn mt cht.
Hnh thi: nha trao i ion thng dng trn.
n: khi em nha dng keo ngm vo trong nc, th tch ca n bin i ln.
m: l % khi lng nc trn khi lng nha dng kh ( m kh), hoc
dng t ( m t).
Tnh chu nhit: cc loi nha b nh hng bi nhit u c gii hn nht nh ,
vt qu gii hn ny nha b nhit phn gii khng s dng c. Nhit hot ng
tt t 20-50o C.
Tnh dn in: cht trao i ion m dn in tt, tnh dn in ca n ph thuc vo
dng ion.
Kch thc ht: Resin c dng hnh cu d = 0,04 - 1,00 mm.
28

Tnh chu mi mn: trong vn hnh cc cht trao i ion c st ln nhau v n ngt,
c kh nng d v vn. y l mt ch tiu nh hng n tnh nng thc dng ca n.
Tnh chu oxy ho: cht oxy ho mnh c th lm cho nha b lo ho (tr)
+ Tnh nng thun nghch ca phn ng trao i ion.
Phn ng trao i ion l phn ng thun nghch. Da trn tnh cht ny ngi ta
dng dung dch cht hon nguyn, thng qua cht trao i ion mt hiu lc khi
phc li nng lc trao i ca n. CaR2 + 2H +( nhaTh d: 2HR + Ca

2+

trao i)

2HR + Ca 2+(hon nguyn)CaR 2 + 2H+. Tnh acid, kim: tnh nng ca cht Cationit RH
v cht Anionit ROH, ging cht in gii acid, kim.
Tnh trung ho v thu phn: tnh nng trung ho v thu phn ca cht trao i ion
ging cht in gii thng thng. Tnh chn la ca cht trao i ion.
hm lng ion thp trong dung dch, nhit bnh thng, kh nng trao i tng
khi ho tr ca ion trao i tng.
+ Th t u tin khi trao i.
i vi nha Cationit acid mnh (SAC),
Fe 3+ > Al 3+ > Ca 2+ > Mg 2+ > K+ > H+ > Li+.
i vi nha Cationit acid yu (WAC)
H+ > Fe3+ > Al 3+ > Ca2+ > Mg 2+ > K+ > Na+ > Li+
i vi nha Anionit kim mnh (SBA), i vi nha anionit kim yu (WBA)
hm lng ion thp nhit bnh thng v nhng ion cng ho tr, kh nng
trao i tng khi s in t ca ion trao i ln (bn knh hydrat ho ln)
hm lng ion cao, kh nng trao i ca cc ion khng khc nhau nhiu lm.
Hin nay, cc loi nha trao i ion c sn xut ch yu bng phng php
ngng t hp trng hp
monomer.
2.2.1.2. Cationit.
Cationit

cha

nhm

hot ng l cc anion R-,

ion linh ng l M+ anion Rc th l nhm sulphonate, nhm phosphoate, carboxylate hoc amino diacetate.
29

Nha trao i cation c trao tng hp bng phng php ngng t u l sn

phm phn ng ngng t ca phenol hoc dn xut phenol vi fomalin. Do phenol cha
OH- nn sn phm thu c c tnh acid rt yu v ch thch hp lm vic trong mi
trng kim. khc phc nhc im ny, ngi ta a vo mng li khng gian ca
cation cc nhm chc khc nhau thu c cation acid mnh hn. Cc nhm chc
c th l nhm sulphonate, nhm photphate, nhm carboxylate hoc nhm amino
diacetate nh ni trn. Cationit cha nhm chc ni vi nhn benzene c tnh acid
mnh hn so vi cationit c nhm chc mch nhnh. Cationit c tng hp bng
phng php ngng t bn i vi cc tia nhng khng bn trong mi trng c cht oxy
ha. Sn phm thu c dng khi to, a chc, kh iu chnh mc lin kt ngang.
Cc cationit tng hp bng phng php trng hp monome c a chung hn
cc cationit ngng t v c bn ha hc, c hc v bn nhit cao, li ch cha mt loi
nhm chc nn rt d iu chnh mc lin kt ngang. Sn phm thu c l cc ht trn
nh nn rt thun tin khi s dng. Phn ng trng hp ph bin nht l trng hp
styrene vi divinylbenzene (DVB). Ngoi styrene, cn c th trng hp acid metacrylic
hay acid acrylic vi duvinylbenzene sn xut cc cationit acid yu. Mun thu c cc
sn phm cationit acid mnh hn, tip tc sulpho ha (hoc photphate ha...) cc sn
phm cationit acid yu ni trn.
2.2.1.3. Anionit.
Anionit
dng R+X-

c
vi

nhm hot ng
R+ thng l nhm
amin. Do c nhm
amin gn trn mng li cao phn t nn anionit mang tnh baz. baz ph thuc vo
baz ca nhm amin (amin thng > ammoniac > amin thm;amin bc 4> amin bc 3 >
amin bc 2 > amin bc 1). Anionit ph bin thng cha amin bc 4.
Anionit c th c tng hp bng phng php ngng t hoc phng php trng
hp. tng hp anionit bng phng php th nht, ngi ta ngng t amin mch
thng hoc amin thm vi formalin hoc vi halogenepoxy. Anionit ngng t c tnh baz
yu, bn ha hc km, khng bn trong mi trng cha cc cht oxy ha.
30

Anionit c tng hp bng phng php trng hp c tnh baz mnh, bn ha v

bn nhit tt li n chc nn c s dng rng ri hn anionit ngng t. Qa trnh sn
xut anionit bng phng php trng hp c tin hnh bng cch trng hp styrene
hoc dn xut cu styrene vi divinylbenzene DVB ( c clometyl ha) v tip tc
amin ha vi trimetylamin hoc dimetyletanolamin thu c anionit baz mnh.
2.2.1.4. Ionit lng tnh.
Trn mng li khng gian ca ionit lng tnh va cha nhm chc acid va cha
nhm chc baz nn c kh nng trao i c cation ln anion. Ionit lng tnh cng c
tng hp bng hai phng php trng hp v ngng t. V d tng hp ionit lng
tnh bng phng php trng hp, u tin trng hp styren hoc clorua vinyl vi DVB
ri sau tip tc amin ha v sulpho ha sn phm thu c.
Trong cc loi ionit, cationit sulphonate (- SO3H) l cationit acid mnh, anionit amin
t l anionit kim mnh (hot ng tt trong mi mi trng acid, baz, trung
tnh);cationit carboxylate (- COOH) l cationit acid yu (hot ng tt trong mi trng
kim); anionit amin tam, nhi, nht l cc anionit kim yu (hot ng tt trong mi
trng acid).
2.2.2. C ch trao i ion.
Mng li ca ionit l mng khng gian cao phn t khng ng u ca cc mch
lin kt hydrocacbon. Kh nng trao i ion ca ionit ph thuc rt ln vo mng li
cu trc ca ionit, c th l cc mc lin kt ngang,s lng v bn cht cac nhm chc.
ni kh nng trao i ion ca ionit ph thuc vo cu trc bi v tnh a nc ca ionit
c quyt nh bi cu trc, m chnh tnh a nc ny lm cho ionit c kh nng
trng trong nc, ch php cc ion t dung dch khuyt tn nhiu hay t bn trong mng
li.
Khi ngm nha vo nc, nha truong n, cc nhm cha ion tr nn linh ng hn
v c th b phn li mt phn. cc phn ng trao i xy ra gia cc ion pha tnh v cc
ion trong dung dch rt tng ng cc phn ng trao i gia cc cu t tip sc vi
nhau trc tip trong dung dch theo phn ng ho hc thng thng. tuy nhin, khi dung
dch cha nhiu ion cng c kh nng trao i ion vi nha th s c s cnh tranh gia
cc ion trong dung dch v qua trnh tr nn phc tp.
31

Ion trong lp in tch kp theo mc hot ng ln nh c th phn ra: lp hp

ph v lp khuch tn. Lp ion c tnh hot ng tng i km b hp ph bm cht vo
b mt cao phn t gi l lp hp ph hay lp c nh, n bao gm lp ion bn trong v
mt b phn ion ngc du. Cnh ngoi lp hp ph, cc ion c tnh hot ng tng i
ln, c kh nng khuch tn vo trong dung dch nn gi l lp khuch tn.
Khi nha trao i ion gp dung dch nc c cht in gii, cc tc dng sau y s
din ra:
+ Tc dng trao i.
Cc ion ngc du trong lp khuch tn v ion ngc du khc trong dung dch trao
i v tr ln nhau. Nhng do qu trnh trao i ion khng gii hn lp khuch tn, do
quan h cn bng ng, trong dung dch cng c mt s ion ngc du trc tin trao i
n lp khuch tn, sau s trao i vi cc ion ngc du trong lp hp ph.
+ Tc dng nn p.
Khi nng mui trong cc dung dch tng ln, c th lm cho lp khuch tn b
nn p li. T , mt s ion ngc du trong lp khuch tn bin thnh ion ngc du
trong lp khuch tn bin thnh ion ngc du trong lp hp ph , Phm vi hot ng
ca lp khuch tn nh li lm bt li cho qu trnh trao i ion. Do cn ch nu
nng dung dch hon nguyn qu ln, khng nhng khng th nng cao m cn gim
thp hiu qu hon nguyn.
+ Tc qu trnh trao i ion.
Nh trong qu trnh hp ph, tc trao i ion tu thuc trn tc ca cc qu
trnh thnh phn sau:
- Khuch tn ca cc ion t trong pha lng n b mt ca ht rn.
- Khuch tn ca cc ion qua cht rn n b mt trao i.
- Trao i cc ion (tc phn ng)
- Khuch tn ca ion thay th ra ngoi b mt ht rn
- Khuch tn ca cc ion c thay th t b mt ht rn vo trong dung dch.
+ iu kin s dng ca nha trao i ion
- Nha ch s dng trao i ion ch khng dng lc huyn ph, cht keo v
nh mu. S c mt cc cht ny c th rt ngn tui th ca nha.
- Loi b cc cht hu c bng nha rt phc tp, cn c nghin cu c bit
32

- S c mt ca kh ho tan trong nc vi lng ln c th gy nhiu lon hot

ng ca nha.
- Cc cht oxy ho mnh Cl2, O3,.c th tc dng xu ln nha.
V mt nh lng, kh nng trao i ionit l trao i theo dng lng cc cht.
2.3. CC YU T NH HNG.
Cc yu t c th nh hng n kh nng p dng v hiu qu ca qu trnh ny
bao gm:
* Du v m trong nc ngm c th lm tc nghn cc nha trao i. Cht rn l
lng ln hn 10 ppm c th gy ra nha lm m.
* PH ca nc chay n c th nh hng n vic la chn nha trao i ion.
* Oxy ha trong nc ngm c th lm hng nha trao i ion. X l nc thi
c to ra trong cc bc ti to v s cn iu tr b sung v x l.
i vi sc k trao i ion cationit acid mnh, khi cc cation c bn knh cng nh
th kh nng hidrat ha trong dd nc cng ln. Do nhng ion c bn knh cng nh
th bn knh hidrat ha cng ln, do i lc tng tc vi pha tnh cng yu nn t b gi
li. Cn i vi ct cationit acid yu th kh nng lu gi ch yu trn tng tc ca pha
tnh vi H c tnh acid ca cc phn t nc b hidrat ha nn th t ngc li (nh
chnh vi ln trc l tong tc gia pha tnh vi cht tan cha khng phi dung mi ra
gii vi cht tan) Cn i vi ct anionit bazo th th t ra gii ph thuc vo kh nng
tng tc ca pha tnh vi cht tan.
2.4. THIT B NG DNG
2.4.1. Mt s thit b sc k trao di ion dng trong phng th nghim.
+ My sc k ion (MetroHM ngun gc Thy S)
HNG CUNG CP: METROHM THU S
MODEL: 883 COMPACT IC PLUS
L h thng phn tch sc k thng minh, vi chnh xc cao,
n v o ppm, ppb, %
Gii hn pht hin: < 1ppb
Thit k gn nh, hiu sut lm vic cao

33

p ng tt c cc yu cu GLP v FDA
H thng thng minh vi cc
thnh

phn:

iPump,

iDetector,

iColumn ng dng anion chun : F,

Cl, Br, NO2, NO 3, SO4, PO 4,..
ClO2, ClO 3, ClO 4, BrO4, BrO3
Phn tch cc cation chun : Li,
Na, K, Mg ,Ca , NH4 , Cs, Sr, Ba,
Rb,
+ My phn tch sc k ion
Phn tch cc loi mu v mi
trng vi cc anion & cation hm
lng vt nh NH4+; Cr6+ ; Cr3+ ;
Fe2+ ; Fe3+ PO43- ; NO2- ; NO3- ; SO42-; Cl- Phn tch hm lng Phosphate:
monophosphate, pyrophosphate, metaphosphate, trypolyphosphate & polyphosphate
trong mu thc phm, thy hi sn, cht ph gia
My sc l t ng.
Automated Ion Chromatography System
Model: ICS 900. Hng
sn xut: Dionex - M Xut x:
M. Tiu chun p ng: ISO
9001, CE Thit b c thit k
t ng hon ton, chuyn dng
cho mc ch phn tch cc ion trong mu ho hc, mi trng, thc phn,... vi thao tc
s dng n gin, tin dng v t kt qu nhanh,
chnh xc. iu khin qua phn mm my tnh C th
Kt ni c vi b a mu t ng AS-DV hay AS
Dionex.
+ My sc l ion.
Model: Water 1525 Binary HPLC Pump
Hng sn xut: Waters-M
34

Bao gm:Bm dung mi a knh gradient, Bm gradient: 2 dng dung mi (thit

k kiu bnh rng cam 40 mL/bc rng, piston kp, ton b c ngm trong du, bo
m bm chy n nh, sai s nh, bn, khng gy n, khc vi cc hng khc s dng
curoa ko bnh cam t ( n ln, chnh xc dng RSD ln, nh pic khng n
nh..).
( Thit k c quyn ca hng to chun xc ca lu lng dng t (0,075% ti
0,1% RSD : Flow precision of < 0,075 RSD or better) , v mc phn gii 0,001 ml/pht).
S ng dung mi: 02 dng
Tc dng: 0.001 - 10.000 ml/min,
Mc phn gii: 0, 001 ml/ph.
chnh xc ca lu lng dng: < 0.1 % RSD (0,075% ti 0,1% RSD : Flow
precision of < 0,075 RSD or better)
n nh p sut: 1% cho ton b thang cho mt chu trnh bm 1 ml/ph
n di mc tiu chun cho php ti v tr thao tc < 70 dB(A), p sut bm : 0
- 6000 psi,
chnh xc dng :

1.0%

T ng b chnh p sut
Kh kh dung mi cho h thng
C h thng kim tra s r r
Chng trnh gii hn p sut trn, gii hn p sut di chn la psi, kPa, bar.
Khi lng: 32 kg
in p: t 88 V - 264 V AC
Tn s: 47 - 63 Hz
Nhit thao tc trong khong: 40C - 400C
m thao tc trong khong: 20 - 80%
Cu to bung o: loi 5 in cc (Duy nht trn Th gii)
Gii o dn : 0 ~ 10 000 mS/cm
c ng dng phn tch cc cation v anion : Na+ ; K+ ; Mg 2+ ; Ca 2+ ; NH4 + ; Cl
-

; F - ; NO2- ; NO3- ; CN - ; SO42- ; HCO3- ; Br - ; acide hu c bc I ...

2.4.2. ng dng ca sc k trao di ion trong phn tch nh lng.
35

- Trao i ion chng t l mt trong nhng phng php chnh ca phn on

ca bt n nh sinh hc cht,sc k trao i ion ng mt vai tr quan trng trong
vic tch v tinh ch phn t sinh hc v ng gp ng k vo s hiu bit ca chng ta
v qu trnh sinh hc,sc k ion trao i, ph bin vi cc k thut tch khc trong khoa
hc i sng, l giai on lc duy nht trong tch hoc phn tch cc mu sinh hc phc
tp. Ion trao i thng xuyn kt hp vi cc k thut khc c phn chia theo cc
thng s khc nh kch thc (Gel lc), s nc (k nc tng tc sc k hoc sinh
hc hot ng (mi quan h sc k).
- Khng ch l s la chn ca cc k thut quan trng. Th t m chng c lm
vic cng s ng mt vai tr quan trng trong vic xc nh tc , tin li v nng sut
tng th cho thch hp.
- Phng php sc k trao i ion c s dng rt hiu qu trong vic tch v phn
tch cc cht phc tp dng kh hoc lng, thm ch c cht rn.. phng php trao
i ion thng c d dng d kh cng ca nc do cc mui ha tan di dng
ion ca Ca2+, Mg2+; kh khong ca nc loi hon ton cc cation anion c trong
nc; tinh ch cc cht th ha hc nh tinh ch HCl k thut, tinh ch cht khng in
ly ra khi hp cht in ly; tch chit protein; iu ch hp cht ha hc nh iu ch
phn bn ha hc dng lng t nc thi; tch lng nh ca mt s nguyn t
2.5. SO SNH VI CC PHNG PHP KHC V TI U HA SC K
TRAO I ION.
2.5.1. im ging nhau.
- S dung nh tnh v nh lng mt hn hp nhiu cu t.
- Thit b sc k thng bao gm cc b phn chnh nh: b phn np mu, ct sc
k v u d.
- Gm hai qu trnh l qu trnh tnh v qu trnh ng.
2.5.2. im khc nhau.
Sc k hp ph
lng
+ L qu trnh

Sc k trao i ion

Sc k giy

+ Da trn hin

+ Sc k giy

Sc k kh
+ Sc k kh l

khc nhau ca cu tng trao i thun thuc dng sc k sc kh m pha dng

36

t lng v cht hp nghch gia cc ion phn b lng, m l dng kh hoc

ph rn.

linh ng ca pha cht mang pha lng dng hi.

+ Lc hp ph tnh rn vi cc ion l giy sc k.

bao gm lc Vander trong

dung

dch

Waats l lc tng phn tch.

tc gia cc phn t:

+ Khi pha tnh l

+ Nh c cu to cht hp ph rn th
c bit giy sc k ta c sc k kh hp

+ Bn cht ca c kh nng gi ph. Khi pha tnh l

Lc cm ng: qu trnh tch l do trong l xp mt mng

mng

cht

hnh thnh khi trong i lc khc nhau ca lng cht lng nht lng trn b mt
phn t c sn in cc ion trong dung nh.
trng.

Trong

qu cht hp ph rn ta

dch vi cc trung trnh sc k cc cu c sc phn b hay

Lc lin kt ha tm trao i ion t c tch dc cn gi l sc k kh

hc: gia cht hp (nhm cha ion) ca theo lp mng ca lng.
ph v cht b hp ionit

l giy.

ph
2.5.3. Ti u ha sc k trao i ion.
t c hiu sut cao v gim chi ph iu ch cc k thut v quy trnh sc k
cn c ti u ha. Qu trnh ti u ha quy trnh lun l mt vn phc tp, i hi
mt thi gian th nghim lu di v c phng php ph hp.
Trong thc t ti u ho c ngha l dung ha cc yu t sao cho t dc phn
gii cao nht c th trong thi gian cht nhn c hoc t dc trong thi gian ngn
nht ng vi phn gii t yu cu (cc peak tch hon ton ra khi nhau).
Khi nh gi kh nng tch cc cu t ra khi nhau, s khng y nu cho rng
kh nng ny ph thuc hon ton vo hiu nghim ca ct. Thc ra chiu cao a l
thuyt ch th hin tt rng ca peak sc k, cn mun nh gi kh nng tch ca ct
(hay lp mng) mt cch hon thin phi xem xt ng thi hiu nng ca ct, chn
lc, tch v dung lng ct thng qua chiu cao a l thuyt H, h thng chn lc ,
phn gii Rs v h s cha K.
Ni mt cch c th hn thc hin ti u ha ngi ta thay i cc iu khin th
nghim nhm mc ch lm gim s dn rng ca peak v lm bin di vn tc di chuyn
tng i ca cc cu t. Nh chng ta bit, s dn rng vng cht sc k tng ln l
37

do cc bin i ng hc lm tng chiu cao a l thuyt ca ct, cn tc di chuyn

ca cc cu t cn ph thuc rt nhiu vo cc yu t gy nh hng n h s cha v
h s chn lc.

38

PHN C.

TI LIU THAM KHO

1. Phn tch nh lng Nh xut bn i hc Quc gia tp. H Ch Minh.

2. Slide bi ging Thy Nguyn c Vng.
3. Phn tch ha hc nh lng NXB Khoa hc K thut H Ni, 1995.
4. Cc phng php Sc k NXB Khoa hc k thut H Ni.
5. http://baigiang.violet.vn/present
6. http://tailieu.vn/tag/tai-lieu
7. http://www.hcmbiotech.com.vn
8. http://www.dlu.edu.vn
9. http://traitimnamdinh.net
10. http://www.cyberchemvn.com
11. http://www.taybacuniversity.edu.vn
12.http://www.scribd.com/doc/45986487/Ph%C6%B0%C6%A1ng-phap
%E1%BA%AFc-ki-trao-%C4%91%E1%BB%95i-ion

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