TT LUYN THI & BI DNG KIN THC NGY MI 18A/88 INH VN T - TP.

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GII THIU V PHNG PHP SC K
TS. Vi Anh Tun
Trng THPT Chuyn KHTN- HKHTN HQG H NI

Sc k l qu trnh tch da trn s phn b lin tc cc cu t cht phn tch ln hai pha. Mt pha
ng yn, c kh nng hp thu cht phn tch c 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 nn chng di chuyn vi tc khc
nhau v tch ra khi nhau.
V d th nghim ca Txvet c tin hnh nh sau: Ho tan cc sc t thc vt trong ete du ha, sau
np mt lng nh vo ct nhi bt CaCO
3
. Tip theo, cho lin tc ete du ha tinh khit i qua ct, sau mt
thi gian nht nh sc t thc vt tch thnh cc gii ring bit. Sau ny, ngi ta bit c l cc o-
Clorophyl, |-Clorophyl, o-Xantophyl, |- Xantophyl ..., chng l cc cht mu nn khi tch chng to thnh cc
gii mu khc nhau, v vy, Txvet gi n l "Chromatography". Theo ting Hy Lp, "Chroma" c ngha l mu,
cn "Graphy" l c ngha l ghi, danh t c s dng cho ti ngy nay ch phng php sc k.
1 Phn loi cc phng php sc k
C nhiu tiu ch phn loi cc phng php sc k, trong tiu ch c s dng nhiu nht l
phn loi theo h pha, tc l cht phn tch phn b gia hai pha g?
PHNG PHP SC K
Sc k kh
Sc k lng
SK kh- rn
SK kh-lng
HPLC
SK phng
SK in di mao qun
SK phn b lng- lng
SK lp mng
SK giy
SK rn- lng

Hnh 1 Phn loi cc phng php sc k
2 Cc lc lin kt trong h sc k
Trong h sc k c 3 thnh phn ch yu quyt nh s tn ti ca h: cht phn tch, pha tnh v pha
ng. Chng tng tc vi nhau, 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. Vn c t ra l ba thnh phn ny tng tc nh th no,
bng cc lc lin kt no, m kt qu l cc cht phn tch phn b vo pha tnh mc khc nhau? Cu
tr li l do bn cht ca cc thnh phn trong h sc k ni trn. Cht phn tch c th l cc ion, phn t
trung ho hay cc cht phn cc; i tng tc ng ca n cng c th l ion, phn t trung ho hay cht
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phn cc. T chng tng tc vi nhau theo cc lc lin kt khc nhau. Ngi ta chia cc lc lin kt
thnh 4 loi:
a) 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 cc trung tm hot ng ion. Chng 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 trung 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.
b) 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 nh, cng c th l nhng lng cc
in do cm ng. Chng tham gia lin kt vi cc phn t phn cc 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 rt quan trng bn lin kt khc nhau, l iu cn thit phn chia chng
trong cc php tch sc k.
Th d: cc cht ng phn o-, m- v p-cresol ch khc nhau v v tr ca nhm CH
3
- trong phn t.
Chnh nh s khc nhau v v tr ny lm cho mt electron trong phn t ca cc cresol khc nhau to
nn mt s khc bit nh v phn cc, t lc lin kt phn cc vi pha tnh khc nhau, l nguyn nhn
chnh lch v thi gian lu trong qu trnh sc k.
c) Lc phn tn (lc Van-de-van)
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 cm ng hay c nh. Tng tc phn tn in hnh l gia cc mch hyr
cacbon, n l tng tc phn t.
Th d: n-heptan l cht lng ch khng phi kh v s tng tc gia cc phn t n-heptan l lc
phn tn ln gi cht ny trng thi lng. tch cc hyr cac bon ngi ta c th dng hyr
cacbon khc lm pha tnh.
d) Lc tng tc c bit
Lc tng tc c bit l lc to thnh do cc lin kt hydro, lin kt cho nhn m c.
S hnh thnh lin kt gia cc nguyn t hydro v cc nguyn t c m in cao nh O, N,
F...to thnh lin kt hidro. Khi tham gia lin kt, cc electron cn gi l "m my electron" chuyn dch
sang nguyn t c m in cao. Nh vy cc nguyn t ca nguyn t c m in cng cao, lin kt
hydro cng bn cht. Ngi ta nhn thy nng lng lin kt gim theo dy sau y:
FH
...
F > OH
...
O > NH
...
N > CH
...
C
TT LUYN THI & BI DNG KIN THC NGY MI 18A/88 INH VN T - TP. HI DNG
HOAHOC.ORG NG XUN QUNH
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Nh vy lc tng tc ca cc phn t trong h sc k gm: lc ion, lc phn cc, lc phn tn v
lc tng tc c bit. Cc lc ny i vi cc cht khc nhau c gi tr khc nhau v quyt nh i vi qu
trnh tch sc k.
3 Mt s i lng dng trong sc k
3.1 H s phn b K
D

Cu t A phn b gia pha tnh v pha ng theo mt cn bng:
A

A
t

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

t
D
A
A
K
] [
] [
=
(1)
3.2 S lin h gia tc di chuyn ca cht phn tch v K
D
Cht phn tch A mun di chuyn c n phi pha ng. Gi f
A
l phn mol cht A pha ng:
f
A
=
s mmol cht A trong pha ng
s mmol cht A trong ton ct
t t

V A V A
V A
] [ ] [
] [
+
=
Chia c t s v mu s cho [A]

ta c:

'
1
1
1
1
A

t
D
A
k
V
V
K
f
+
=
+
=
(2)

t
D A
V
V
K k =
'
c gi h s dung tch. Tc tuyn tnh ca cu t A trong pha ng l:
'
1
1
.
A
A A
k
u f u u
+
= =
(3)
trong u l tc tuyn tnh ca pha ng (cm/s). T biu thc (3) ta thy khi K
D
hoc k
A
cng ln, thi
gian cht phn tch trong pha ng cng t, ni mt cch khc l cht phn tch di chuyn cng chm,
ngc li khi k' cng nh, cht phn tch di chuyn cng nhanh.
3.3 Thi gian lu t
R
, thi gian lu hiu chnh t'
R


Thi gian lu t
R
l thi gian tnh t lc bt u bm mu vo u ct ti khi pic t gi tr cc i.

u
k L
u
L
t
A
A
RA
) 1 (
'
+
= = (4)
t
m
= L/u l thi gian cu t khng lu gi trn ct, hay cn gi l thi gian cht.
(4) =>
) 1 (
'
A m RA
k t t + =
(5)
3.4 Th tch lu V
R

Th tch lu V
R
l th tch ca dung dch ra gii tnh t khi bt u bm mu vo ct ti khi pic t
gi tr cc i. Gi F l tc chy ca pha ng (ml/ pht). Khi th tch lu V
R
c tnh theo cng
thc:
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F t V
RA RA
= (6)
3.5 H s tch
H s tch o l i lng nh gi kh nng tch 2 cht bng phng php sc k. N ph thuc vo
h s phn b ca 2 cht v vy l t s ca h s phn b ca 2 cht. Mt cht phn tch A v mt cht
khc B hoc mt cht chun.
iu kin cn thit hai cht A v B tch khi nhau l o = 1

'
'
B
A
DB
DA
k
k
K
K
= =
(7)
3.6 Sc
Sc l ng 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 tn s xung in lin quan cht ch ti nng cht phn
tch c trong mu vo thi gian. Cc tn hiu ny c gi l "pic"sc k. tnh ton hm lng cht phn
tch, tnh din tch pc sc k l chnh xc nht. Ngy nay, hu ht cc my hin i u c trang b cc
thit b tnh din tch ca pc sc k mt cch t ng.
3.7 a l thuyt v xc nh s a l thuyt bng thc nghim
a l thuyt l phn no ca ct m cn bng c thit lp.
Gi n l s a l thuyt, o l lch chun; o ~ n . i vi ct sc k th n cng ln th pic
cng hp. Thi gian lu t l vi n : t
R
~ n, nn ta c th vit:
n
n t
R
=
o
hay n = (t
R
/ o)
2

Mt khc w = 4o hay o = w / 4

Hnh 2: Cc i lng xc nh s a l thuyt ca cu t A
S a l thuyt n c th vit li l:

2
2 / 1
R
2
R
w
t
54 , 5
w
t
16 n
|
|
.
|

\
|
= |
.
|

\
|
= (8)
3.8 phn gii, cch lm tng phn gii
phn gii (R) ni ln mc tch cc 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 ring l: thi gian lu, t
RA
, t
RB
, rng pic W
A
,W
B
.
TT LUYN THI & BI DNG KIN THC NGY MI 18A/88 INH VN T - TP. HI DNG
HOAHOC.ORG NG XUN QUNH
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B A
RA RB
W W
) t 2(t
R
+

= (9)
Trong : t
RB
- t
RA
= At
R
l s chnh lch thi gian lu (cng c th dng th tch lu V
RA
- V
RB
) ca
2 cu t A v B. i lng ny c so snh vi tng bn chiu rng pc, o bng giy hoc ml ni ln kh
nng tch ca ct.
Khi R=1, hai cu t A v B mi tch khi nhau t 95% ngha l cn 2,5% ca A cn trong B ,
2,5% B trong A.
Khi R= 1,5 th hai cu t A v B tch khi nhau t 99,8 % c ngha l cn 0,1% A trong B v
ngc li.
Khi tng chiu di ct, s a l thuyt tng:
t
R
~ n, chiu rng pic t l vi n
R ~
n
n
hay R ~ L
Th d khi tng gp i chiu di ct, phn gii mi R' s l: R' = 2 R
4 Mt s phng php sc k c in
4.1 Sc k giy
Phng php s dng vt liu cht mang l giy cn pha tnh l cht lng trn b mt giy.

Hnh 3: Sc k giy
Giy l mt vt liu c bit bao gm nhng si xenluloz trn c nhng nhm -OH phn cc
cho nn n l vt liu a nc. Khi tm bng nc, trn b mt giy c mt lp nc mng, phn cc lm
pha tnh cn pha ng l dung mi khng phn cc. y l loi sc k phn b L-L. Theo quan nim thng
thng pha tnh phn cc cn pha ng khng phn cc l sc k pha thng
Nu tm t giy bng dung mi hu c t phn cc cn pha ng l dung mi phn cc Th d H
2
O
th trong trng hp ny l sc k pha ngc.
4.2 Sc k lp mng
Sc k lp mng l khi nim a ra phng php s dng lp mng pha tnh ph trn mt bn
mng bng thu tinh hay plastic. Pha ng l cc dung mi khc nhau c th l phn cc hoc khng phn
cc hoc dung dch m.
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Trong sc k lp mng pha tnh rt a dng: cht hp ph, trao i ion, cht ry phn t v ngoi ra
ngi ta cn tm cc dung mi khc nhau trn cht mang rn. Do c ch tch cng c th l hp ph,
trao i ion, ry phn t hoc phn b. Ni cch khc, sc k lp mng c y 4 c ch tch tu thuc
vo pha tnh s dng.
Sau khi ph lp pha tnh ln bn mng, np cht phn tch vo mt pha ca bn mng sau cho
bn mng tip xc vi pha ng pha gn mu nht, tt nht l thc hin trong h kn, khng kh bo ho
pha ng. Sau mt thi gian nht nh, ly bn mng ra cho hin cht phn tch. Tin hnh nh tnh v nh
lng cht phn tch. i lng nh gi s di chuyn ca cht tan trong sc k lp mng cng tng t nh
trong sc k giy.
4.3 Pht hin cc cht phn tch trn bn mng v giy
Cc cht phn tch i khi khng c mu, v nu c mu thng rt nht v khng r. th hin
c mu trn giy hoc bn mng, ta p dng mt vi nguyn tc sau:
- Tn dng tnh cht ca cc cht c kh nng pht hunh quang, xc nh trc tip cht sau khi dng nh
sng kch thch.
- a thm cc cht ch th hunh quang v dng nh sng t ngoi (UV) chiu vo ghi nhn mu
(thng s c mu xanh). l cc dn xut ca piren, fluorexein, morin hay rodamin B. i vi sc k bn
mng c th p dng cch:
- Phun cc cht oxi ho mnh nh HNO
3
, KMnO
4
hay H
2
SO
4
c vo oxi ho cc cht hu c, s c cc
im b oxiho v chuyn sang mu m l cht phn tch.
- a cc thuc th c bit vo nh ninhydrin hin -NH
2
. S dng cc cht to phc mu lm cho kim
loi c th nhn thy.
3.4 ng dng ca sc k lp mng
Sc k lp mng c th p dng trong cng nghip, sinh hc, lm sng hay phn tch cc dc phm.
a) Phn tch cc cation kim loi: Ni
2+
, Co
2+
, Cu
2+
, Fe
3+
, Hg
2+
, Cd
2+

-Pha ng: axeton 5%, HCl 8% trong nc; thuc hin: 8-oxiquynolin.
-Phn tnh: Glucoz.
b) Tch cc amin
-Pha ng: Butanol: CH
3
COOH : H
2
O = 4:1:5; Thuc hin: Ninhydrin 0,2% trong axeton khan.


TI LIU THAM KHO
1. Douglas A. Skoog, F.James Holler, Stanley R. Crouch, Principles of Instrumental Analysis, six
edition, Canada, 2007.