Ti liu ging mn k thut x l mu phn tch ha

X L MU TRONG PHN TCH HA THC PHM

X l mu trong phn tch thc phm l khu ht sc quan trng, mt
trong nhng yu t nh hng n chnh xc ca kt qu phn tch.
Tu tng i tng mu, tu tng ch tiu phn tch m phi c cch x l
khc nhau.

1. Yu cu chung ca cc k thut x l mu phn tch

1.1. X l mu l g
- X l mu l qu trnh ho tan (dissolution) v phn hu (digestion), ph
hu cu trc mu ban u ly t i tng cn phn tch, gii phng v
chuyn cc cht cn xc nh v mt dng ng th ph hp (v d dng
dung dch) cho mt php o chn xc nh hm lng ca cht m
chng ta mong mun.
V d ha tan mu hp kim Al trong axit HNO 3 45% c dung dch xc
nh Al v cc tp kim loi trong hp kim Al.
- X l mu c hai qu trnh xy ra ng thi l:
Ph hu cu trc ban u ca cht mu (digestion of Sample Matrix),
Ha tan gii phng cht cn xc nh v dng dung dch ng th.

1.2. Ti sao phi x l mu phn tch.

- a cc cht cn xc nh v mt trng thi thch hp cho php o, theo
phng php phn tch chn.
- Cc kt qu phn tch phi phn nh v i din ng cho i tng cn
nghin cu, theo di.
- Vi bt k mt phng php xc nh, mi cht phn tch ch c th c
xc nh chnh xc khi n tn ti mt trng thi nht nh v ng nht
ph hp vi k thut phn tch.

1/44

Ti liu ging mn k thut x l mu phn tch ha

V d: xc nh cc kim loi (v d: Fe, Cu, Mn, ..) trong mu tht, chng

ta khng th b ngay mu tht vo my quang ph hp th nguyn t o,
cn phi a cc kim loi tn ti trong mu v trng thi ion hay hp cht
tan c trong dung dch nc, sau mi xc nh c chng trong dung
dch ny.
- Mu phn tch c nhiu chng loi, a dng, c thnh phn n gin n
loi c thnh phn phc tp. Chng c th tn ti cc trng thi khc nhau
nh rn tng cc, tng mnh, hay lng, kh, v huyn ph. Khng th cho
nguyn mu nh th vo cc my o v xc nh c. phi x l a
cc cht cn phn tch (cn xc nh) v trng thi ph hp nht cho mt
phng php c chn xc nh n.
- Cc cht cn xc nh tn ti trng thi lin kt ho hc khc nhau, trong
cc hp cht v c, hu c khc nhau, c khi rt bn vng, lng cht mi
v tr trong mu cng khng ng u, nn khng th xc nh ng hm
lng ca n trong mt t hp phc tp, bn vng v b cc nguyn t, cc
cht lin kt khc cn tr, do cn phi x l mu ph v cc hp cht
m cht phn tch ang tn ti, a chng sang mt dng ph hp nh
lng tt v ng theo phng php chn.
Vy mun phn tch mt i tng no, chng ta phi ly mu, x l
ph hp c c mt trng thi hay mt dung dch mu phn tch xc
nh cc cht mong mun.
- Vic x l mu theo cch no, l tu thuc vo:
+ i tng mu, matrix ca mu.
+ Bn cht, tnh cht ca cc cht cn phn tch.
+ Trng thi tn ti, cu trc vt l ho hc ca cc cht trong mu.
+ Phng php phn tch c la chn xc nh chng.
+ Hm lng ca cht cn xc nh mc no trong mu.
2/44

Ti liu ging mn k thut x l mu phn tch ha

Trn c s cc yu t chng ta chn cch x l ph hp cho cht phn

tch.
Ngy nay cc k thut x l mu phn tch v ang c dng l:
K thut v c ho kh (x l kh),
K thut v c ho t (x l t).
K thut v c ho kh- t kt hp,
Cc k thut chit (lng-lng, chit rn-lng, chit rn-kh,..),
Cc k thut sc k, v.v.
Tuy nhin trong qu trnh ly mu mt s i tng cn phi x l s b
ngay trc khi mang mu v phng th nghim.

2. K thut v c ha t (x l t)
2.1. V c ha t bng axit mnh c nng
2.1.1. Nguyn tc v bn cht
Nguyn tc chung
Dng axit mnh c v nng (v d HCl, H2SO4), hay axit mnh, c v
nng c tnh xy ho mnh (HNO3, HClO4), hoc hn hp 2 axit ( HNO3 +
H2SO4), hay 3 axit (HNO3 + H2SO4 + HClO4), hoc l 1 axit c v mt cht
xy ho mnh (H2SO4 + KMnO4), v.v. phn hu mu trong iu kin un
nng trong bnh Kendan, trong ng nghim, trong cc hay trong l vi sng.
Lng axit cn dng phn hu mu thng gp 10 - 15 ln lng mu,
tu thuc mi loi mu v cu trc vt l ho hc ca n.
Thi gian phn hu mu (x l) trong cc h h, bnh Kendan, ng
nghim, cc, .. thng t vi gi n hng chc gi, cng tu loi mu, bn
cht ca cc cht. Cn nu trong l vi sng h kn th ch cn 50 - 90 pht.
Cc dung dch axit dng ho tan v x l mu

3/44

Ti liu ging mn k thut x l mu phn tch ha

Trong cch x l t ngi ta thng dng cc loi dung dch axit c v c

tnh oxy ho mnh, song tt nhin chn loi axit no l tu thuc vo bn
cht ca cht nn (matrix) ca mu v cht phn tch tn ti trong mu ,
v d:
+ Dng 1 axit c: HCl, HF, H3PO4, H2SO4,
+ Dng 1 axit c tnh oxy ho: HNO3, H2SO4, HClO4,
+ Hn hp 2 axit: Cng thu, (HCl+HNO3),(HNO3+H2SO4),(HF+H2SO4),
+ Hn hp 3 axit: (HCl + HNO3 + H2SO4), ( HNO3 + H2SO4 + HClO4),
+ Hn hp 1 axit v cht xy ho: (H2SO4+ KMnO4), (HNO3+H2O2),
+ Hn hp 2 axit v 1 cht oxy ho mnh (HNO3+ H2SO4+ KMnO4),
+ Dung dch mui c pH nht nh (KCl 1M, pH=5, NH4Ac 1M pH-6,.. ).
Nhit dung dch phn hu mu
Nhit si ca hn hp mu khi x l mu l ph thuc vo nhit si
ca dung dch axit dng phn hu mu. Khi cn nhit si cao th phi
dng axit c nhit si cao (bng 2.1). Trong cc h kn p sut cao s to
ra nhit si cao, tu thuc vo loi axit dng phn hu mu.
Bng 2.1. Nhit si ca cc dung dch axit c
Vi axit n:
Axit

HCl

HNO3

Ng (%)
36
65
o
T(si) C
110
121
Vi hn hp axit:
Loi hn hp ca
Cng thu (HCl/HNO3):
(HNO3+ H2SO4):
(HNO3+ H2SO4 ):
(HNO3+ H2SO4 + HclO4 ):
(HF+ H2SO4 ):
(HNO3+ H2SO4 + HF )

H2SO4

H3PO4

HClO4 HF

98
280

78
213

72
203

Thnh phn (V/V)

3/1
4/1
3/2
4/2/2
2/1
2/1/1

4/44

40
120

Nhit si oC
116-118
130-135
150-155
137-140
130-150
120-130

Ti liu ging mn k thut x l mu phn tch ha

Tt nhin khi dng hn hp, th nhit si ca dung dch axit hn hp l

tu thuc vo thnh phn ca 2 hay 3 axit ta dng trn vo nhau v nhit
si ca dung dch phn hu s nm gia nhit ca hai axit c trn vi
nhau. V th vi cc cht mu kh phn hu (kh x l) chng ta phi dng
cc axit v hn hp axit c nhit si cao v tnh oxy ho mnh.
2.1.2. Cc kiu v c ha t
Vic x l mu theo phng php t, c th c thc hin trong cc trang
b v dng c khc nhau, tu thuc phng th nghim c loi no, v d:
Trong iu kin thng:
+ X l trong cc thu tinh, khi un nng trn bp in hay ni cch thu.
+ X l trong bnh Kendan thng khi un nng
+ X l trong bnh Kendan c ng sinh hn hi lu dung mi, v.v.
Trong hp kn. Mu trong hp kn, thm dung dch axit phn
hu mu, y kn, sau thc hin phn hu bng cch:
+ Sy trong t sy, trn bp ct, hoc trong l nung nhit thch hp.
+ Ngm hay luc hp mu trong ni nc si, hay trong du si, v.v.
X l mu trong l vi sng (trong h kn v h), nh:
a/ Trong cc h l vi sng n gin v iu khin bng tay:
+ H bnh mu h,
+ H bnh mu ng kn (c p sut cao),
b/ Trong cc h nhiu bnh v hot ng theo chng trnh:
+ H bnh mu h c khng ch nhit .
+ H bnh mu ng kn (p sut cao), c khng ch nhit , p sut, v.v.
Trong cc kiu x l t ny, hin nay k thut x l t vi axit c c tnh
oxy ho mnh trong bnh kendan v trong l vi sng h kn ang c dng

5/44

Ti liu ging mn k thut x l mu phn tch ha

nhiu nht. Vi cc nc pht trin, ph bin hin nay l cch x l trong l

vi sng, v n trit , nhanh v li khng lo ngi mt cht phn tch.
2.1.3. C ch v cc tc nhn phn hu mu
2.1.3.1. C ch ca s phn hu mu
Trong iu kin thng ca h h, th tc nhn phn hu mu l:
+ Tc dng ph hu v ho tan cc ht (phn t) mu ca axit,
+ Tc nhn nng lng nhit, lm tan r cc ht mu cng vi axit,
+ S khuych tn i lu, chuyn ng nhit v va chm ca cc ht mu
vi nhau lm chng b bo mn dn.
Cc tc nhn ny tn cng v bo mn dn cc ht mu t ngoi vo, lm
cho cc ht mu b mn dn dn, b dn ri tan mt ht, khi chng ta un
mu trong bnh Kendan hay trong cc trong mt thi gian nht nh.
Trong l vi sng:
Ngoi cc tc nhn phn hu nh trn, trong l vi sng cn c s ph v t
trong lng ht mu ra ngoi, do cc phn t nc hp th (>90%) nng
lng vi sng v n c ng nng rt ln, nn chng c chuyn ng nhit
rt mnh, lm cng v x cc ht mu t trong ra. Thm vo li l h kn,
nn c p sut cao v s lm nhit si li cao hn v y l tc nhn phn
hu mnh nht, do thc y qu trnh phn hu mu rt nhanh t trong ra
v t ngoi vo. V th nn vic x l mu trong l vi sng ch cn thi gian
ngn (30-70 pht) m li trit .
2.1.3.2. Cc qu trnh xy ra khi phn hu mu: Di tc dng ca axit
c v nng lng nhit (nhit ), c nng lng vi sng, cc qu trnh vt
l v ho hc sau y s xy ra:
S ph v mng li cu trc ca ht cht mu, gii phng cc cht phn
tch, a chng vo dung dch di dng cc mui tan.

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Ti liu ging mn k thut x l mu phn tch ha

Qu trnh xy ho kh lm thay i ho tr, chuyn i dng, lm tan v

cc ht vt cht mu, gii phng cht phn tch v dng mui tan.
Nu x l mu hu c phn tch kim loi, th c s t chy, ph hu cc
hp cht hu c v mn to ra kh CO 2 v nc, gii phng cc kim loi
trong cht mu hu c v dng mui v c tan trong dung dch.
To ra hp cht d bay hi, lm mt i cc anion trong phn t cht mu,
lm mu b phn hu to ra cc hp cht tan trong dung dch.
S to thnh cc hp cht hay mui phc tan trong dung dch.
C th tch cht phn tch ra khi mu ban u dng kt ta khng tan v
nh ngi ta tch c cc cht phn tch v lm giu chng.
Nh vy trong trong qu trnh x l mu y cng c th c cc phn ng
ho hc xy ra, nh phn ng oxy ho kh, phn ng thu phn, phn ng
to phc, phn ng ho tan, phn ng kt ta, v.v. ca cc phn t cht mu
vi cc axit dng phn hu mu v cc cht c trong mu vi nhau.
Trong qu trnh no l chnh hay ph l c quyt nh bi thnh phn,
cht nn, bn cht ca cht mu v cc loi axit dng phn hu v ho tan
mu.
2.1.4. V d theo cch x l t
V d 1: X l mu rau qu bng hn hp 2 axit (HNO 3 + H2O2), trong
bnh Kendan, xc nh cc kim loi nng (Cd, Cu, Fe, Mn, Ni, Pb, Zn).
Ly 5,00 g. mu nghin mn v trn u vo bnh Kendan, thm 60 mL
HNO3 65%, 5 mL H2O2 30%, cm phu nh vo bnh kendan, lc u v un
si nh cho mu phn hu, n khi c dung dch trong khng mu (6-8
gi tu loi mu). Chuyn mu sang cc 250 mL, lm bay hi ht axit bng
n IR n cn mui m, ngui, nh mc bng dung dch HCl 2% thnh
25 mL. Trong qu trnh x l ny cc nguyn t kim loi dng cc hp
cht c kim ca mu rau qu, s b axit c oxy ho cc cht hu c, a cc
7/44

Ti liu ging mn k thut x l mu phn tch ha

kim loi v cc mui v c tan trong dung dch nc. Qu trnh ho hc

chnh:
(Mu) +HNO3 + H2O2 Men(NO3)m + H2O + CO2+ NO2
(mui tan ca kim loi )
Tt c cc v d t 1 n 3 c th x l trong l vi sng h kn, v lng axit
s bt i n 1/3. Thi gian x l ch trong 40 - 50 pht. Cn x l nh trn
trong h h bnh thng, th phi mt t 4-8 gi, m li khng trit bng
x l trong l vi sng.
2.1.5. Cc u nhc im v ng dng
Cc u v nhc im chnh ca k thut ny l:
+ Hu nh khng b mt cc cht phn tch, nht l trong l vi sng,
+ Nhng thi gian phn hu mu rt di, trong iu kin thng,
+ Tn nhiu axit c tinh khit cao, nht l trong cc h h,
+ D b nhim bn khi x l trong h h, do mi trng hay axit dng,
+ Phi ui axit d lu, nn d b nhim bn, bi vo mu, v.v.
ng dng ch yu ca k thut x l t ny l x l mu:
Xc nh cc kim loi v mt s phi kim, hay anion v c, nh Cl -. Br-, I-,
AsO43-, SO42-, PO43-, SiO32, .. trong cc mu sinh hc, mu hu c, mu v
c, mu mi trng, mu t, mu nc, mu bi khng kh, mu kim loi,
hp kim, rau qu v thc phm, v.v.
2.2. X l t bng dung dch kim mnh c nng
2.2.1. Nguyn tc chung
Trong phng php ny ngi ta thng dng cc dung dch kim mnh c
nng (NaOH, KOH 15-20%), hay hn hp ca kim mnh v mui kim loi
kim (NaOH +NaHCO3), hay mt kim mnh v peroxit (KOH + Na 2O2),
nng ln (10 -20%), phn hu mu phn tch trong iu kin un nng
trong bnh Kendan hay trong hp kn, hoc trong l vi sng.
8/44

Ti liu ging mn k thut x l mu phn tch ha

Lng dung dch phn hu: cn lng ln t 8-15 ln lng mu.

Thi gian phn hu: t 4 - 10 gi trong h h. Cn trong h l vi sng kn
ch cn thi gian 1-2 gi.
Nhit d phn hu: L nhit si ca dung dch kim. N thng trong
vng 150 -200 oC.
Cc qu trnh xy ra khi phn hu mu
Di tc dng ca kim v nhit , c nng lng vi sng, c th xy ra cc
qu trnh sau:
+ Ph v cu trc ca cht mu, chuyn cc cht ca mu vo dung dch,
+ Cc cht ca mu tng tc vi kim to ra cc sn phm tan c,
+ C th sinh ra cc kh bay ra, gip s tan ca mu tt hn,
+ C th to ra cc hp cht bn t phn li v tan trong dung dch,
+ To ra cc sn phm kt ta mi khc ca cht phn tch tch n ra khi
mu ban u.
2.2.2. Cc cch ho tan v dung dch ho tan
Cht phn hu: Theo k thut x l t ny chng ta c th dng cc dung
dch ca cc cht sau y x l mu:
Dung dch kim c (20-25 % NaOH, hay KOH),
Dung dch kim c nng c cht xy ho mnh (NaOH + Na2O2),
Hn hp kim c nng c cht kh (KOH+NaHSO3),
Hn hp kim mnh v mt mui (NaOH + NaHCO3), (KOH+Na2CO3),
Hn hp kim, mt mui v peroxit (KOH+ NaHCO3+ H2O2),
Hn hp kim, mt mui v peroxit kim (KOH+ NaHCO3+ Na2O2), v.v.
Qu trnh phn hu
Qu trnh phn hu c thc hin khi un si dung dch mu, trong mt
thi gian nht nh trong bnh Kendan hay trong ng nghim, thng l t 6

9/44

Ti liu ging mn k thut x l mu phn tch ha

-10 gi trong bnh kenan h, trong l vi sng h kn (c p sut cao) th ch

mt khong 40 - 70 pht, tu loi mu.
C ch ph v (phn hu) mu theo cch ny cng tng t nh trong
trng hp dng cc axit trn, trong h h hay h kn, nhng y tc
nhn phn hu l dung dch kim mnh nng.
Nhit phn hu: Nhit si ca cc dung dch kim l tu thuc vo
thnh phn v nng ca dung dch kim ta s dng x l mu. Ni
chung trong vng t 115 230 oC, tu thuc nng ca kim v mui c
trong dung dch phn hu mu v y l mt yu t thc y s phn hu
xy ra nhanh hn. Ngha l tc nhn phn hu mu y l kim v nhit
(nng lng nhi ) v nng lng vi sng, nu dng l vi sng.
2.2.3. V d ng dng k thut ny
V d 1: Ho tan oxit nhm bng dung dch NaOH 10% nng. Ly
0,5g. mu dng bt vo bnh kendan, tm t bng vi git nc ct, thm
10 mL NaOH 10%, un si ho tan mu. C ch y l: Chuyn trng
thi tinh th rn xit sang ion tan trong dung dch l mui NaAlO 2 v kh
hydro theo phn ng:
Al2O3 + NaOH H2 + NaAlO2 + H2O
2.2.4. Cc u nhc im v phm vi ng dng
K thut x l t trong dung dch kim c nng cng c u im l hu
nh khng lm mt cc cht phn tch, nht l cc nguyn t c hp cht d
bay hi v cc nguyn t v cc matrix ca mu d tan trong kim.
Nhng cch ny c mt nhc im lon l tn rt nhiu kim tinh khit cao,
thng phi dng gp t 10 15 lng mu, kh nng gy nhim bn d xy
ra. Lng kim d nhiu, sau khi x l xong thng phi loi ht, nhng rt
kh, ch bng cch trung ho bng axit, song li lm long mu v d dng
nhim bn, mt thi gian c c mu. y l mt cng vic rt kh khn v
10/44

Ti liu ging mn k thut x l mu phn tch ha

mt nhiu th gi v cng li hay lm nhim bn mu. y chnh l mt

nhc im ln ca k thut ny.
V th cch ny ch c dng cho mt s trng hp, m cch x l axit
cho kt qu khng tt. V d phn hu mu xc nh mt s anion v c, phi
kim hay kim, nh cc cht: Cl 1-, Br1-, NO31-, SO42-, PO43-,v.v. trong cc i
tng mu sinh hc v mt s mu thc phm khng x l c bng
phng php axit.
Cch ny thch hp cho:
+ Cc hp cht hay cc mu tan tt trong kim.
+ Phn hu cc cht hu c ly cc phi kim.
Cc v d khc c th xem thm chng 3 v 4 phn II.

3. K v c ha kh
3.1. Nguyn tc v cc qu trnh xy ra khi v c ha mu
3.1.1. Nguyn tc: K thut x l kh (v c ha kh) l k thut nung
x l mu trong l nung mt nhit thch hp (450-750 oC), song thc
cht y ch l bc u tin ca qu trnh x l mu. V sau khi nung, mu
b cn li phi c ho tan (x l tip) bng dung dch mui hay dung dch
axit ph hp, th mi chuyn c cc cht cn phn tch trong tro mu vo
dng dung dch, sau xc nh n theo mt phng php chn. Khi
nung cc cht hu c ca mu s b t chy thnh CO2 v nc.
3.1.2. Nhit nung: Nhit nung x l mu thng trong vng 450 -750
o

C, tu thuc vo mi loi mu (cht nn v cu trc ca n) v cc cht cn

phn tch v l yu t quyt nh. Nhng phi m bo t chy c ht

cc cht hu c v khng lm mt cht phn tch. V d khi nung x l cc
mu rau qu v thc phm nhit t 500 550oC, xc nh cc kim
loi nng, cc kim loi kim v kim th. Song nu khng c cht ph gia

11/44

Ti liu ging mn k thut x l mu phn tch ha

bo v th thng cc nguyn t Cd, Pb, Zn,.. c th b mt t 10 - 15%, m

chng ta khng khng ch c. Nhit nung thng ph thuc vo:
+ Bn cht ca cht mu v cht phn tch,
+ Cu trc, dng lin kt, loi hp ca cc cht trong mu,
3.1.3. Thi gian nung: C th t 5 12 gi, hoacj tu thuc vo:
+ M loi cht mu,
+ Mi cht phn tch,
+ Cu trc, dng lin kt, loi hp ca cc cht trong mu,
3.1.4. Cc loi cht ph tr (ph gia)
+ K thut tro ho kh thng c dng cho cc mu hu c, x l xc
nh cc kim loi, v cc mu qung v c c cu trc bn vng rt kh tan
trong cc axit mnh. Vic tro ho cng c th c thc hin khi c thm
cht ph gia, cht bo v hay cht chy. Cc cht bo v v cht chy thng
hay c dng l:
+ Cc axit: HNO3, H2SO4, H3PO4, vi nng ph hp,
+ Mt s mui: KNO3, Ca(NO3)2, Mg(NO3)2, LiBO2, Na2B4O7,
+ Hn hp axit v mui: (Mg(NO3)2+ HNO3), (HNO3 + H2SO4),
+ Hn hp kim v mui: (KOH + NaHCO3), (KOH+ Na2SO4),
+ Hn hp mui v peroxit: (KHCO3 + Na2O2), (NaHCO3 + Na2O2),
+ Hn hp kim mnh v peroxit: (NaOH + Na2O2), (KOH + Na2O2).
+ Hn hp kim, mui v cht oxyha (KOH+NaHCO3+Na2O2).
+ Hn hp kim v mui pyrosnphat (KOH + Na2S4O7), v.v.
Cc cht ph gia ny c hai tc dng:
+ Bo v cc cht phn tch khng b mt,
+ Gp phn lm cho mu c phn hu nhanh v trit hn,

12/44

Ti liu ging mn k thut x l mu phn tch ha

3.1.5. Cc qu trnh xy ra: Trong qu trnh nung x l mu c th c

nhiu qu trnh vt l v ho hc xy ra, tu theo bn cht, thnh phn ca
mi loi mu v cht ph gia c thm vo, l cc qu trnh:
+ Trc tin lm bay hi mt nc hp th v nc kt tnh trong cht mu,
+ S tro ho, t chy cc cht mn v cc cht hu c ca mu,
+ Ph v cu trc ban u ca cht mu,
+ Chuyn dng cc hp cht phc tp ca cht mu v dng n gin hn,
+ Qu trnh oxy ho kh thay i ho tr ca nguyn t trong cc cht mu,
+ Gii phng ra mt s kh, nh CO, CO2, SO2,..
+ C mt s tng tc ho hc ca cc cht vi nhau, tng tc vi cht ph
gia thm vo,.. to ra cc cht lc u khng c.
Tt c cc qu trnh u gp phn lm tan v cu trc ban u ca cc ht
mu to ra tro b mu, sau ho tan cht phn tch vo dung dch axit.
Bng 2.2 sau y l vi v d v s nung mt s mu phn tch trong iu
kin c ph gia v khng c ph gia.
l nhng qu trnh c th xy ra, tt nhin l a dng v phc tp, n xy
ra nh th no l tu thuc vo cc yu t sau y:
Thnh phn, cht nn v trng thi lin kt ca cht mu v cht phn tch,
Cc cht ph gia, cht chy v cht bo v thm vo mu,
Cc iu kin nung, trong nhit l yu t chnh, sau l mi trng
nung l khng kh, hay trong kh tr (Ar, N2, He,..).
Kt qu ca s nung c th xy ra cc qu trnh to ra cc sn phm c thnh
phn n gin hn, v d trong bng 2.2, nn chng d ho tan c trong
axit hay kim long.
3.2. Cc loi trang b v dng c x l kh
Cc trang b x l mu theo phng php kh thng khng c nhiu.

13/44

Ti liu ging mn k thut x l mu phn tch ha

Thng thng mu c cho vo chn hay bt nung (thch anh, s, Ni, Fe,
hay Pt, hoc Au, hay W,..) c dung tch khc nhau (t 30 - 200 mL). Sau
c nung ti nhit ph hp trong l nung.
Dng c cha ng mu nung:
+ Cc loi chn nung thch anh, s, graphit, platin, vng, zirconi, v.v.
+ Cc loi bt nung thch anh, s, kim loi (platin, vng, zirconi), v.v.
+ Cc loi chn v bt Teflon chu nhit.
Thit b nung mu c hai loi chnh:
1. Trang b thng thng: T sy v l nung cc loi.
2. Trang b hin i: Cc loi l vi sng v l cao tn, v.v.
Bng 2.2. V d v cc qu trnh trong x l kh trong l nung
Loi mu
t st
Qung Silicat
Qung Ferrit
Qung CuS
Dolomit
LnCO3FxH2O
Nha ng
Thc phm
Rau qu
Rau qu
Cht hu c

Ph gia
Nhit Sn phm sau khi nung
KOH+Na2O2 550-650 Na2SiO3+K2SiO3+H2O
KOH+Na2O2 500-600 Na2SiO3+K2SiO3+H2O+MeX
550-600
FeO+Fe2O3+SO2+H2O
550-600
CuO+SO2+H2O + MenXm
550-650
CaO+MgO+H2O+CO2+ MenXm
550-650
Ln2O3+CO2+HF+H2O +MenXm
550-650
MexOy+CO2+SO2+H2O+MenXm
KNO3+HNO3 500-550 MexOy+CO2+H2O+ KxXy+NO
KNO3+HNO3 500-550 MexOy+CO2+H2O+ KxXy+NO
500-550
MexOy+CO2+H2O+MenXm
500-600
MexOy + CO2 + H2O + (NOx)

3.3. Tro ho kh khng c ph gia v cht bo v

Nung x l mu khng c ph gia v cht bo v l qu trnh x l
mu s b nh tc dng ch ca nng lng nhit (nhit ) thch hp trong
mt thi gian nht nh, ph v cu trc tinh th dng ban u ca mu
phn tch, t chy cht hu c, chuyn n sang mt dng cc hp cht
khc n gin, d ho tan tip bng dung dch axit hay bng dung dch kim,

14/44

Ti liu ging mn k thut x l mu phn tch ha

ly cc cht phn tch vo dung dch, sau c th xc nh c chng

theo mt phng php nht nh. Sau y l mt s v d.
V d 1: Tro ho kh mu rau qu xc nh cc kim loi (Na, K,
Ca, Mg, Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Zn). Cn ly 5 g. mu nghin
mn vo trong chn thch anh, em sy t t cho n khi mu kh en, ri
em nung 3 gi u nhit 450 oC, sau nng ln 550 oC, cho n khi
mu ht than en, s c tro mu trng. Sau ho tan tro thu c trong
12-15 mL dung dch HCl 18% (1/1), v c 0,5 mL HNO 3 65%, un nh cho
tan ht, ui ht axit d n cn mui m v nh mc thnh 25 mL bng
dung dch HCl 2%. Cc nguyn t Cd, Cu, Pb, Zn s b mt mt t (10 15%) khi nung. Cch ny thch hp cho xc nh cc kim loi kim, kim
th v Fe, Mn, Ni.
+ Theo cch ny, thng thng mt s nguyn t trong mu s c th b mt
khi nung, nh Cd (10-15%), Cu (7-12%), Pb (15-20%),.. V hm lng mt
b mt i ny li khng kim sot v khng khng ch c trong qu trnh
nung. S mt ny cng nhiu khi nung mu nhit cng cao, hay thi
gian nung cng lu. Nh v d 1 trn, nu nung mu nhit 550 oC, Cd,
v Pb s mt t 12-10%, khi 600 oC, th Cd v Pb s mt n 18-20%, v.v.
l vn cn phi ch .
3.4. Tro ho kh c ph gia v cht bo v
Tro ho kh c ph gia v cht bo v cng l qu trnh x l mu s
b nh tc dng ca nhit thch hp (500-600 oC ), c thm tng tc h
tr ca cht ph gia hn ch s mt mt s nguyn t nh cch nung
khng ph gia trn. Cc cht ph gia thng l cc cht chy, mui kim,
axit c ph v cu trc tinh th dng ban u ca mu phn tch,
chuyn n sang mt dng khc d ho tan tip bng axit.

15/44

Ti liu ging mn k thut x l mu phn tch ha

Khi c cht chy v cht ph gia nhit nung thng thp hn khi khng
c cht chy, thi gian ngn hn, song li trit hn, m li khng mt cht
phn tch. Nht l cc mu c cu trc bn, chu nhit, hay mu matrix hu
c, th tc dng ca cht bo v l rt quan trng. Nh hai v d trn, nhng
khi x l c cht bo v, th khng b mt mt s nguyn t phn tch
nu.
V d 2: Tro ho mu sa xc nh cc kim loi (Na, K, Ca, Mg,
Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Zn). Ly 5 gam mu vo chn thch anh,
thm cht ph gia ( 8 mL H2SO4 45% v 2g. KNO3 (hay 2 g. LiBO3 )), trn
u, sy kh cn thn cho mu kh (mu d si bt v bn, cn thn v un
nh ) v thnh than en, sau em nung 3 gi u nhit 400-450 oC,
ri sau 550 oC, n khi ht than en, c tro mu trng. Sau ho tan
tro thu c trong 15 mL dung dch HCl 18% v 1 mL HNO 3 65%, un nh
cho mu tan ht, un nh lm bay hi axit n cn mui m, nh mc thnh
25 mL bng dung dch axit HCl 2%. l dung dch xc nh cc nguyn
t kim loi ni trn.
3.5. Cc u nhc im v phm vi s dng
Cc u v nhc im chnh ca k thut x l mu ny l:
+ Thao tc v cch lm n gin,
+ Khng phi dng nhiu axit c tinh khit cao t tin,
+ X l c trit , nht l cc mu nn hu c.
+ t chy ht cc cht hu c, v th lm dung dch mu thu c sch,
+ Nhng c nhc im l c th mt mt s cht d bay hi, v d nh Cd,
Pb, Zn, Sn, Sb, v.v. nu khng c cht ph gia v cht bo v.
Bng 2.3. So snh kt qu tro ho t v kh

16/44

Ti liu ging mn k thut x l mu phn tch ha

Ng CX

Cch tro ho

Ph gia

Nh.

Bo v

Khng

450

97-100

HNO3+HClO4

H2SO4

550

93- 98

HNO3+HClO4+H2SO4

HNO3

650

90 - 94

HNO3H2SO4

Mg(NO3)2

450

97-100

Kh:

Mg(Ac)2

550

93-95

650

71-83

450

97-99

550

95-97

650

90-96

450

97-99

550

97-99

650

70-84

450

98-99

550

92-95

650

91-96

t ppm
Pb 10
t:

97-98
95-98
Hg 10

t:

Khng

HNO3+HClO4

450

92-94
78-80

550

90-94

HNO3+HClO4+H2SO4

92-94

HNO3+H2SO4+K2Cr2O7

Kh:

17/44

tm

Ti liu ging mn k thut x l mu phn tch ha

Zn 10

t:

Khng

550

97-100

HNO3+HClO4

HNO3

550

94-102

HNO3+HClO4+H2SO4

H2SO4

550

96-100

HNO3+H2SO4

Mg(NO3)2

550

87-96

Kh:

93-97
97-100

As 10

t:

Khng

550

98-99
96-98

HNO3+HClO4

HNO3

550

97-99

HNO3+HClO4+H2SO4

H2SO4

550

91-98

HNO3+H2SO4

Mg(NO3)2

550

80-88

Kh:

80-84
90-96

Cu 10

t:

Khng

550

92-99
99-100

HNO3+HClO4

HNO3

550

99-101

HNO3+HClO4+H2SO4

H2SO4

550

99-100

HNO3+H2SO4

Mg(NO3)2

550

86-92

Kh:

94-96
95-97

Cd 10

t:

Khng

550

97-99
98-100

HNO3+HClO4

HNO3

550

98-100

HNO3+HClO4+H2SO4

H2SO4

550

97-100

HNO3+H2SO4

Mg(NO3)2

550

86-94

Kh:

82-91
93-97
94-97

18/44

Ti liu ging mn k thut x l mu phn tch ha

Sb 10

t:

Khng

550

94-98

HNO3+HClO4

HNO3

550

95-98

HNO3+HClO4+H2SO4

H2SO4

550

97-99

HNO3+H2SO4

Mg(NO3)2

550

90-94

Kh:

92-96
94-98

Cr

10

t:

Khng

550

96-97
97-100

HNO3+HClO4

HNO3

550

98-100

HNO3+HClO4+H2SO4

H2SO4

550

98-100

HNO3+H2SO4

Mg(NO3)2

550

94-98

Kh

95-98
97-99

Fe

10

t:

Khng

550

95-98
96-100

HNO3+HClO4

HNO3

550

98-100

HNO3+HClO4+H2SO4

H2SO4

550

97-100

HNO3+H2SO4

Mg(NO3)2

550

94-98

Kh:

96-99
97-100

Ag 10

t:

Khng

550

98-100
95-98

HNO3+HClO4

HNO3

550

97-99

HNO3+HClO4+H2SO4

H2SO4

550

97-99

HNO3+H2SO4

Mg(NO3)2

550

93-99

Kh:

87-98
97-99
97-100

Mu th nghim bng trn: L cc loi:

19/44

Ti liu ging mn k thut x l mu phn tch ha

+ Khoai lang v khoai ty.

+ Rau mung, rau ci, bp ci v xu ho.
+ Bt go v bt ng.
+ Tht cc loi v c.

4. K thut v c ho kh-t kt hp
4.1. Nguyn tc chung
Nguyn tc ca k thut ny l mu c phn hu trong chn hay cc
nung. Trc tin ngi ta thc hin x l t s b bng mt lng nh
axit, v cht ph gia, ph v s b cu trc ban u ca cc hp cht mu
v to iu kin gi mt s nguyn t c th bay hi khi nung. Sau mi
nung nhit thch hp. V th lng axit dng x l thng ch bng
1/4 hay 1/5 lng cn dng cho x l t. Sau nung s nhanh hn v qu
trnh x l s trit hn x l t, ng thi li hn ch c s mt ca
mt s kim loi khi nung. Do tn dng c u im ca c hai k
thut x l t v x l kh, nht l gim bt c cc ho cht (axit hay
kim tinh khit cao) khi x l t, sau ho tan tro mu s thu c dung
dch mu trong, v khng cn cht hu c v sch hn tro ho t bnh
thng.
Cc qu trnh vt l v ho hc xy ra khi x l l tng t nh trong x l
t v kh nu trn, song y l s kt hp c hai k tip nhau. Trong
x l t ban u l bo v mt s nguyn t cho x l kh tip theo
khng b mt. Cch ny thch hp cho cc mu c nn (matrix) l cht hu
c, nh rau qu, thc phm,.., x l xc nh cc kim loi v mt s phi
kim. Nhng phng th nghim khng c thit b l vi sng, th y l mt
cch tt cho vic x l mu xc nh cc kim loi nng trong cc i tng
mu sinh hc, mu mi trng v qung t .
4.2. Cch thc hin v mt s v d
20/44

Ti liu ging mn k thut x l mu phn tch ha

V l x l kh t kt hp l k tip nhau, trc tin x l t s b, sau

mi nung, nn tnh cht v s din bin ca n cng tng t nh trong hai
kiu ni trn. Ch c khc l sau khi x l mu khng phi ui lng
axit d qu nhiu nh trong x l t. Sau y l vi v d.
V d 1: X l mu rau qu xc nh cc kim loi (Na, K, Ca, Cd,
Co, Cr, Cu, Fe, Mn, Ni, Pb, Zn). Ly 5,000 g. mu nghin mn vo chn
nung, thm 5 mL HNO3 45% v 5 mL Mg(NO3)2 5%, trn u, ri sy, hay
un nh trn bp in cho mu si v n khi kh thnh than en dn. Sau
em nung lc u 400-450 oC trong 3 gi, ri nng ln 550 oC, n ht
than en. Ho tan tro thu c trong 20 mL dung dch HCl 1/1 v c thm 1
mL HNO3 65%, un nng cho tan, lm bay hi ht axit d n cn mui m,
nh mc bng dung dch HCl 2% thnh 25 mL. y l dung dch xc
nh cc nguyn t ni trn (Na, K, Ca, Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb,
Zn).
V d 2: X l mu sa xc nh cc kim loi (Na, K, Ca, Mg, Cd,
Co, Cr, Cu, Fe, Mn, Ni, Pb, Zn). Ly 5,000 g mu vo chn nung, thm 5
mL HNO3 45%, 2 mL H2SO4 98% v 5 mL Mg(NO3)2 5% ( hay KNO3), trn
u, x l t s b sy mu trn bp in hay trong t sy cho n khi
kh v thnh than en dn. Sau nung 400-450 oC trong 3 gi, tip
550 oC cho mu tro ho n khi thy b khng cn en. Ho tan tro thu c
trong 18 mL HCl 1/1v c thm 1,0 mL HNO 3 65%, un nng cho mu tan
hon ton, ui ht axit d n cn mui m, v nh mc thnh 25 mL
bng axit HCl 2%. y l dung dch mu xc nh cc kim loi bng cc
phng php UV-VIS, hay AAS, hay ICP-OES, hoc ICP-MS.
V d 3: X l mu tm, cua, c,.. xc nh cc kim loi (Na, K, Ca,
Mg, Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Zn). Ly 5,00 gam mu vo chn
thch anh, thm 8 mL H2SO4 75% v 3 mL Mg(NO3)2 5% , trn u, x l
21/44

Ti liu ging mn k thut x l mu phn tch ha

t s b, ta sy hay un trn bp in cho mu si nh v un t t cho n

kh v thnh than en. Sau em nung 3 gi u 400-450 oC, v nung
tip 550 oC cho mu tro ho n c b khng cn en. Ho tan tro thu
c trong 18 mL HCl 1/1 v c thm 1,0 mL HNO 3 65%, un nng cho
mu tan ht, lm bay hi ht axit d n cn mui m, nh mc thnh 25
mL bng HCl 2%. y l dung dch mu xc nh cc kim loi ni trn
bng cc phng php ph UV-VIS, hay ph AES, AAS hoc ICP-OES.
Cc v d khc p dng phng php x l ny c th xem thm trong
chng 3 v 4 phn II.
4.3. Cc u nhc im v phm vi ng dng
Cc u v nhc im ca k thut ny l tn dng c cc u im ca
k thut x l t v c x l kh, c th l:
+ Hn ch c s mt ca mt s cht phn tch d bay hi,
+ S tro ho trit , sau khi ho tan tro cn li c dung dch mu trong,
+ Khng phi dng nhiu axit tinh khit cao tn km,
+ Thi gian x l nhanh hn tro ho t,
+ Khng phi ui axit d lu, nn hn ch c s nhim bn,
+ Ph hp cho nhiu loi mu khc nhau xc nh kim loi, v.v.
Cch ny c ng dng ch yu x l mu cho phn tch cc nguyn
t kim loi v mt s anin v c, nh Cl 1-. Br1-, SO42-, PO43-,..trong cc loi
mu sinh hc, mu mi trng, mu hu c v v c. Khng dng c cho
x l mu xc nh cc cht hu c. Trong cc phng th nghim bnh
thng, khng c trang b l vi sng, th cch x l ny vn l mt phng
php thch hp, n gin, m vn m bo c c kt qu tt.

5. Cc k thut chit trong x l mu

5.1. C s, nguyn tc v iu kin chit
5.1.1. H s phn b ca cht
22/44

Ti liu ging mn k thut x l mu phn tch ha

H s phn b ca cht tan (cht phn tch) trong 2 pha khng tan vo
nhau l mt hng s ho l (hng s nhit ng) v n c trng cho s phn
b ca mi cht. N cho ta bit s phn b ( hay s ho tan ) ca cht phn
tch vo trong hai pha (2 dung mi) khng trn ln vo nhau theo t l, hay
mc no. Nu gi tr hng s ny cng ln, th s phn b cng khc
nhau nhiu v cng thun li cho s chit tch cc cht t pha ny sang pha
kia.
V d c cht tan X c phn b vo h pha gm 2 dung mi A v B
(v d Benzen v nc) khng trn vo nhau, th h s phn b c xc
nh theo biu thc sau.
Kfb = Cx(A)/ Cx(B)
Trong :
+ Cx(A) l nng cht X trong pha A (dung mi A, pha Benzen);
+ Cn Cx(B) l nng ca cht X trong pha B (dung mi B, pha nc).
Nh vy nu nh h s phn b Kfb > 99/1, th coi nh cht X chuyn
gn ht vo pha A. l mt iu kin ca qu trnh chit ly cht phn
tch v tch chng ra khi cht nn (matrix) ca mu ban u, chuyn cht
cn phn tch vo dung mi chit. Sau xc nh chng trong dung mi
ny. Thng thng ngi ta chit cht phn tch t pha nc vo pha hu c
khng tan vo nc. Hai pha ny to thnh h chit (h pha), v d h pha:
(Benzen/ H2O), (CCl4/ H2O), (CHCl3/ H2O), (MIBK/ H2O), v.v.
5.1.2. Nguyn tc v c s ca s chit
Chit l da trn c s s phn b (hay ho tan) khc nhau ca cht phn
tch vo trong hai pha (2 dung mi) khng trn ln vo nhau. Tc l cc cht
phn tch tan tt trong dung mi ny, nhng li khng tan tt
trong dung mi kia. Ngha l s phn b ca mt cht trong hai dung mi ( 2
pha) l rt khc nhau. Nh m chng ta ly c cht cn phn tch ra
23/44

Ti liu ging mn k thut x l mu phn tch ha

khi pha mu ban u, chuyn n vo pha th 2 (dung mi) m chng ta

mong mun. Sau xc nh n trong dung mi chit. Nh th yu t quyt
nh s tch v x l mu y l h s phn b ca cht trong 2 pha ( dung
mi), v cc iu kin thc hin lc chit. Khi h s Kpb ln s c hiu sut
chit cao.
5.1.3. Cc iu kin ca s chit
c c kt qu chit tt, qu trnh chit phi c cc iu kin v
m bo c cc yu cu nht nh sau y:
Dung mi chit phi tinh khit cao, khng lm nhim bn thm cc cht
phn tch vo mu.
Dung mi chit phi ho tan tt cc cht phn tch, nhng li khng ho tan
tt vi cc cht khc c trong mu.
H s phn b ca h chit phi ln, cho s chit c trit .
Cn bng chit nhanh t c v thun nghch, gii chit c tt.
S phn lp khi chit phi r rng, nhanh v d tch ra ring bit cc pha.
Phi chn mi trng axit, pH, loi axit thch hp,
Phi thc hin trong nhit ph hp v gi khng i trong c qu trnh.
Phi lc hay trn u mnh qu trnh chit xy ra c tt.

5.2. Cc kiu chit dng trong x l mu phn tch

5.2.1. K thut chit lng-lng
5.2.1.1. Nguyn tc v iu kin
Nguyn tc: Nguyn tc ca k thut chit ny l da trn c s s phn
b ca cht phn tch vo hai pha lng (2 dung mi) khng trn ln c
vo nhau (trong hai dung mi ny, c th mt dung mi c cha cht phn
tch) c trong mt dng c chit, nh phu chit, bnh chit. V th h
s phn b nhit ng Kb ca cn bng chit l mt yu t quyt nh

24/44

Ti liu ging mn k thut x l mu phn tch ha

hiu qu ca s chit v tip n l s nh hng ca nhit , mi trng

axit. V Kpb l hng s nhit ng. Chit theo kiu ny c hai cch l chit
tnh v chit theo dng chy lin tc. Trong phn tch, kiu tnh c ng
dng nhiu hn, v s n gin ca n.
iu kin chit: qu trnh chit t hiu qu tt, phi c cc iu kin
chit nh c m t trong mc 5.4.1C trn.
5.2.1.2. Cc cch chit v v d
* Phng php chit tnh
Phng php chit ny n gin, khng cn my mc phc tp, m ch cn
mt s phu chit (dung tch 100, 250, 500 mL), l c th tin hnh c
mi phng th nghim. Vic lc chit c th thc hin bng tay, hay bng
my lc nh. Tt nhin khi phi lm hng lot mu th mt nhiu thi gian.
Hin nay ngi ta cung cp cc h chit n gin c 6, 9 hay 12 phu vi
my lc nh, nn vic thc hin chit cng d dng v d ng nht iu
kin.
V d: Chit ly cc Retinoit (cc Vitamin A) t mu thc phm.
Loi mu thc phm c th cc dng sau:
a). Thc phm lng: V d sa ti.
Cch 1: Ly 10 mL mu vo bnh chit, thm 20 mL ru etylic tuyt i,
5-8 gam Na2SO4 khan, trn u, thm 10 mL dung mi n-Hexan, lc mnh
trong 5 pht, trong t lnh 2 pht cho phn lp, tch ly lp n-Hexan c
cha cc Retinoit, lm kh pha chit bng Na2SO4 khan v phn tch cc
Retinoit (h Vitamin A) trong n-Hexan bng HPLC hay MEKC.
Cch 2: Ly 10 mL mu vo bnh chit, thm 15 mL nc ct, 10 mL ru
etylic tuyt i, trn u, thm 10 mL dung mi n-Hexan, lc mnh trong 5
pht, trong t lnh 2 pht cho phn lp, tch ly lp n-Hexan c cha cc
Retinoit, lm kh dch chit n-Hexan bng Na2SO4 khan v phn
25/44

Ti liu ging mn k thut x l mu phn tch ha

tch cc Retinoit trong n-Hexan bng HPLC hay MEKC. Cch ny p dng
cho cc loi sa hp c snh.
b). Cc loi rn, bt, rau qu, trng tht:
Trc tin phi nghin hay xay mu thnh bt v bo qun -15 oC.
x l: Ly 5,00 gam mu xay mn vo bnh x l, thm 15-20 gam
Na2SO4 khan, trn u, thm 20 mL cn tuyt i, lc mnh 5 pht, thm
tip 10 mL dung mi n-Hexan, lc mnh 5 pht, t vo t lnh 4 pht cho
phn lp, tch ly lp n-Hexan c cha cc Retinoit, lm kh bng Na 2SO4
khan, ly dch chit phn tch chng bng HPLC hay MEKC.
V d: Chit alpha-v beta-Caroten t cc loi mu rau qu.
+ Trc ht mu c chn v xay thnh bt, bo qun -15 oC.
+ Ly 5,00 gam mu xay mn vo bnh chit, thm 15-20 gam Na 2SO4
khan, 1 gam MgCO3 khan, trn u, thm 20 mL dung mi THF, khuy u
trong 5 pht, lc ht chn khng ly pha hu c THF c cha cc Caroten
vo bnh ct quay chn khng, ct quay cho n cn khong 1 mL, yn
tip 1 pht cho kh, ho tan b v nh mc mu thnh 5 mL bng THF, v
ly tm b cn. y l dung dch xc nh cc - v -Caroten bng
phng php HPLC hay phng php HPCEC.
* Phng php chit dng chy lin tc
Trong phng php chit ny, khi thc hin chit, hai pha lng khng trn
c vo nhau (hai dung mi, c mt dung mi c cha cht phn tch)
c bm lin tc v i ngc chiu nhau vi tc nht nh trong h
chit, nh phu chit, hay bnh chit lin hon ng kn chng tip xc
vi nhau. Hoc cng c th ch mt dung mi chuyn ng, cn mt pha
ng yn trong bnh. Khi , cht phn tch s c phn b vo hai dung
mi theo tnh cht ca chng, t n trng thi cn bng. Chit theo cch

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Ti liu ging mn k thut x l mu phn tch ha

ny hiu sut cao. y l phng php chit c ng dng trong chit sn

xut cng ngh.
thc hin cch chit ny, phi c h thng my chit, ct chit hay bnh
chit, c bm bm cc cht theo dng chy ngc chiu nhau vi tc
nht nh thch hp, hoc ch mt cht, hay c 2 cht chuyn ng ngc
chiu nhau, v phi c b tch pha, tch cc cht ngay trong qu trnh
chit, ly cht c chit ra lin tc, hay theo tng thi im (chu k)
nht nh, m cn bng chit t c (dng c chit cui chng).
5.2.2. Cc u nhc im v phm vi ng dng
Phng php chit tnh n gin, d thc hin, v ang c ng
dng ph bin v rt c hiu qu trong lnh vc tch chit phn tch v lm
giu cc cht phn tch phc v cho vic xc nh hm lng vt. Nht l
tch v lm giu cc kim loi, cc cht hu c, HCBVTV c hi trong cc
mu nc, nc thi, nc bin, v.v.
Cc u v nhc im chung ca k thut chit l:
+ Dng c cho c chit phn tch v sn xut tch chit lng ln,
+ Ly ring cht PT, loi c cc cht nh hng, nht l cht nn ca
mu,
+ Thch hp cho lm giu lng nh cht phn tch (c th 10-50 ln),
+ Phc v cho chit c c cc cht v c v cc cht hu c,
+ Sn phm chit ph hp c cho nhiu phng php phn tch.
5.3. K thut chit pha rn (SPE)
5.3.1. Nguyn tc v iu kin
5.3.1.1. Nguyn tc chung
Chit pha rn cng l qu trnh phn b ca cc cht gia 2 pha, trong
lc u cht mu dng lng (pha nc, hay hu c), cn cht chit dng

27/44

Ti liu ging mn k thut x l mu phn tch ha

rn, dng ht nh v xp ng knh 25 - 70 m. V th nn c tn l chit

pha rn (Solid Phase Extraction ), hay chit rn-lng.
Cht chit c gi l pha tnh, v c nhi vo mt ct chit nh, ct
chit kch thc: 6 x 1 cm, hay dung lng chit 100-600 mg, hoc dng a
chit c kch thc dy 1-2 mm v ng knh 3-4 cm. Cht chit l cc ht
Silica trung tnh, cc ht xit nhm, hay cc Silicagen trung tnh b alkyl
ho nhm -OH bng nhm mch carbon thng -C2, -C4, -C8, -C18,.. , hay
nhn phenyl. N c ch to trong iu kin ging nh pha tnh ca sc k
HPLC, v cc ht ny c xp ln, vi din tch b mt xp thng t 50 300 m2/gam.
Khi x l mu, dung dch cht mu c di ln ct chit. Lc ny pha
tnh s tng tc vi cc cht v gi mt nhm cht phn tch li trn ct
(trn pha tnh), cn cc nhm cht khc s i ra khi ct cng vi dung mi
ho tan mu. Nh th l chng ta thu c nhm cht cn phn tch trn
pha tnh (cht chit rn).
Sau dng mt dung mi thch hp ho tan tt cc cht phn tch ra
gii chng ra khi pha tnh (ct chit), v chng ta thu c dung dch c
cht phn tch xc nh chng theo mt cch chn.
5.3.1.2. Cc loi cht chit pha rn
Theo c im v bn cht ca s chit, cc cht chit pha rn c
ch to v phn chia theo cc loi cht:
Loi hp ph pha thng. l cc Silica trung tnh v xit nhm,
Hp ph pha ngc. l cc Silica thng c alkyl ho nhm-OH,
Loi cht trao i in ( tch Cation v Anion),
Cht ry hay sng lc phn t theo ln, kch thc ca phn t cht,
Loi cht hp ph kh (purge and trap Extraction), hp th cht kh.
5.3.1.3. Cc kiu v c ch chit pha rn
28/44

Ti liu ging mn k thut x l mu phn tch ha

Chnh v c nhiu loi cht chit pha rn, cho nn k thut chit pha rn
cng c nhiu c ch v qu trnh ng hc khc nhau, theo bn cht ca
mi loi cht chit (pha chit). Ni chung, cc cht chit pha rn ny cng
tng t nh cc pha tnh trong sc l lng hiu nng cao (HPLC). N c
th l dng ct chit (1x6 cm c th tch 4-6 mL) hay dng a chit (dy 1-2
mm v ng knh 3-4 cm). Do chit pha rn cng c 3 loi c ch chnh
l:
1. Hp ph pha thng (loi NP), v Hp ph pha ngc (loi RP),
2. Trao i ion v cp ion i vi cc cht dng ion (loi IEx),
3. Ry phn t theo ln ca cht phn tch (Gel).
5.3.2. Cc iu kin ca chit pha rn
Qu trnh chit y thc cht cng l s phn b ca cht phn tch
gia 2 pha, pha rn (cht chit) v pha lng (dung dch cha cht phn tch)
khng trn ln vo nhau trong nhng iu kin nht nh, nh pH, dung
mi, nhit , tc chy ca mu qua ct chit. Trong h s phn b
nhit ng Kb ca cht phn tch gia hai pha (rn v lng cha mu) cng l
mt yu t quyt nh hiu qu ca s chit. N cng tng t nh trong h
sc k ct lng-rn (ca cc h HPLC).
V th mun thc hin chit pha rn tt phi c cc iu kin sau y
Pha rn hay cht chit (dng ct chit hay a chit) phi c tnh cht hp
th hay trao i chn lc vi mt cht, hay mt nhm cht phn tch nht
nh, tc l tnh chn lc ca pha tnh chit.
Cc cht chit v dung mi ra gii phi c sch cao theo yu cu ca
cp hm lng phn tch.
H s phn b nhit ng K fb ca cn bng chit phi ln, c c hiu
sut chit cao.

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Ti liu ging mn k thut x l mu phn tch ha

Qu trnh chit phi xy ra nhanh v nhanh t cn bng, nhng khng c

tng tc phn ng ho hc lm mt hay hng pha rn v cht phn tch.
Qu trnh chit phi c tnh thun nghch, cn c th ra gii c tt
cht phn tch ra khi pha chit bng mt pha ng ph hp.
Khng lm nhim bn thm cht phn tch trong qu trnh chit bi bt k
t ngun no.
S chit phi c thc hin trong iu kin nht nh ph hp, phi lp
li c tt v tt nhin l cng n gin d thc hin th cng tt.
5.3.3. Cc kiu chit v c ch chit pha rn
5.3.3.1. Chit theo c ch hp ph pha thng
Trong kiu ny, cht chit (pha tnh) l cc Silica trung tnh, c b mt
xp phn cc. N tc dng tt vi cc cht mu khng phn cc v t phn
cc. l s tng tc hp ph. Tu theo bn cht v cu trc phn t ca
mi nhm cht phn tch, bn cht hp ph ca Silica trung tnh v cc iu
kin thc hin chit, m nhm cht phn tch no b pha tnh hp ph v gi
li trn ct chit v hon ton tng t nh s tng tc hp ph trong ct
sc k NP-HPLC.
Dung mi gii chit cht phn tch trong loi ny thng l cc dung mi
hu c khng phn cc hay t phn cc v k nc (khng tan vo nc ),
hay hn hp ca chng vi nhau theo t l thch hp. V d n-Hexane, nHeptane, CCl4, CHCl3, Benzen, Diclo-Etan, Ethyaxetat, v.v. Cc dung mi
ny c gi l pha ng (MP) v n phi ho tan tt cht phn tch, ly
c cc cht phn tch ra khi pha tnh (cht chit rn).
V d 1: Chit x l mu xc nh nhm hp cht Clo-phenol trong
nc. Ly 250 mL mu vo phu chit, axit ho n pH=2 bng H2SO4 2%,
lc b cn (nu c) sau di dung dch mu ny qua ct chit ( loi LASi5) vi tc 2-4 mL/pht cho n khi mu chy ht qua ct chit. Di qua
30/44

Ti liu ging mn k thut x l mu phn tch ha

ct chit 5 ml nc ct, yu 5 pht. Sau gii chit ly cht phn tch

bng 10 mL dung mi acetonitril (hay dichlomethane) v xc nh cht phn
tch trong pha hu c ny bng HPLC hay GC.
5.3.3.2. Chit theo c ch hp ph pha ngc
Trong kiu chit ny, cht chit (pha tnh) l cc Silica pha ngc, c
b mt hu nh khng phn cc. N tc dng tt vi cc cht mu khng
phn cc v phn cc. l s tng tc hp ph ca pha tnh (cht chit ).
Tu theo bn cht v cu trc phn t mi nhm cht phn tch v cc iu
kin thc hin chit, m nhm cht phn tch no b pha tnh hp ph v gi
li trn ct tch chit.
C ch chit y l s tng tc hon ton tng t nh s tng tc hp
ph trong ct sc k lng hiu nng cao hp th pha ngc (RP-HPLC ).
Kiu chit ny d thc hin, n gin v c ng dng nhiu. V do tnh
tin li ca h dung mi ra gii tan trong nc, dung mi cha cht phn
tch. Chng ta c minh ho s tng tc ny nh m hnh sau.
V d: Chit x l mu xc nh mt s ho cht BVTV trong
nc. Ly 250 mL mu nc, chnh pH=5, lc b cn. Ly dung dch di
qua ct chit (loi LR-C18 ) vi tc 2-4 mL/pht. Sau ra ct bng 5
mL nc ct, ht chn khng cho ct 3 pht. Ra gii cht BVTV trong ct
bng 20 mL dung mi Etyl-axetat. Ly dung dch ra gii ny di qua ct
hp ph th hai ( ct c: Na2SO4+ Al2O3 + than hot tnh) lm sch v lm
kh mu. Sau li ra gii cht BVTV trong ct ny bng 10 mL EtylAxtat. Thu dung dch, lm bay hi bng dng kh nit sch ( tc 0,8
mL/pht) n cn dung dch snh, nh mc thnh 2 mL bng Etyl-Axetat,
lm kh bng Na2SO4 khan. Ly dung dch mu ny xc nh cc ho cht
BVTV (Metyl-parathion, Diazinon & Sumithion) bng phng php
GC/ECD, hay GC-MS.
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Ti liu ging mn k thut x l mu phn tch ha

5.3.3.3. Chit theo c ch trao i in v cp ion

Chit theo c ch trao i ion
Nguyn tc: Da trn c s ca qu trnh trao i ion ca cht phn tch
vi ion i (ion trao i) ca cht chit (pha tnh trao i in) hp thu
(gi) cht phn tch li trn pha tnh (ct chit). Sau dng mt pha ng
(dung dch) ph hp ra gii cht phn tch vo dung mi v sau
tin hnh xc nh n theo mt phng php phn tch thch hp chn.
Dung mi ra gii y l dung dch nc ca cc mui tan ca kim loi
kim, amoni c pH ph hp, hay dung dch axit long v c th c thm cht
to phc.
Cht trao i in ca kiu chit ny c th l hai loi sau v ang c
s dng hin nay, l:
+ Trao i Cation axit mnh (R-SO3Na) v axit yu (R-COONa).
+ Trao i Anion Baz mnh (R-N+(-OH)), baz yu (R-NH2OH), v.v.
C ch ca s trao i in
a) Loi trao i Cation
Tng qut qu trnh trao i Cation:
nMat-SO3Na + Men+ (Mat-SO3)n-Me + nNa+
( Cht chit ) ( cht PT )

Trong : Mat: Mng rn ca cht trao i ion; Men+: Cation ca cht phn
tch. Na+: Cation trao i ca cht chit. -SO3Na: Nhm chc trao i ion.
b). Loi trao i Anion
Tng qut qu trnh trao i Anion:
nMat-OH + Xn- (Mat)n-X + nOHhay nMat-Cl + Xn- (Mat)n-X + nCl( cht chit ) ( Cht PT )

32/44

Ti liu ging mn k thut x l mu phn tch ha

Trong : Mat: L mng rn ca cht trao i ion; Xn- : Anion ca cht phn
tch. OH- v Cl- l anion trao i.
Trong qu trnh trao i ion, tu thuc vo mi loi cht phn tch v cht
pha tnh (ch yu l nhm chc trao i ion thuc loi axit yu hay mnh,
hoc baz mnh hay yu) , m qu trnh c th c thc hin tt trong mt
vng pH (mi trng axit) nht nh. V th s chit theo c ch ny cn
phi c thc hin trong mi trng pH (hay axit) ph hp.
Chit theo c ch trao i cp ion
Cng vi s trao i cation v anion, trong s chit pha rn cn c c ch
chit theo kiu cp ion. y cng l bn cht trao i ca ion ca cht phn
tch thng qua cht trung gian- cht to cp ion, n cho ion trao i vi cht
phn tch. N cng hon ton tng t nh sc k cp in ca h pha ngc
hp ph (h RP-HPLC). Cht chit y thng l cht hp ph pha
ngc.V d Silica LiChrosorb RP-8, RP- 18 hay l Hypersil ODS. V y
cng c hai kiu trao i cp ion.
5.3.3.4. Cc u nhc im v phm vi ng dng
Chit pha rn l mt k thut chit mi ra i, ang pht trin v c ng
dng trong khong chc nm tr li y, nht l cc nc tin tin v n
mi vo Vit nam ta t nm 1997. Hin nay c mt s hng sn xut v
cung cp ra th trng nhiu loi cht chit v dng c chit khc nhau cho
nhiu i tng rt tin dng. Cht chit thng l cc cht Silica c hot
ho chng c kh nng hp th cao v chn lc cc cht theo tng nhm.
K thut chit ny c cc u v nhc chnh im sau y:
C tnh chn lc i vi mt nhm hp cht phn tch,
Cn bng chit nhanh t c v c tnh thun nghch,
Thch hp cho mu lng nh v phn tch lng vt cc cht,
Thao tc n gin v nhanh hn cc k thut chit khc,
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Ti liu ging mn k thut x l mu phn tch ha

Trong qu trnh chit lun lun c c s lm giu cht phn tch,

Cht chit pha rn khng t (khong 50.000 .VN/1ct chit).
Chnh v th m n ang c s dng rt ph bin trong phn tch, c bit
l phn tch i tng mi trng cc cht vi lng c hi.
5.4. K thut chit hp ph pha kh (rn-kh)
5.4.1. Nguyn tc chung
K thut ny da trn c s l mt nhit nht nh thch hp, khi thi
mt dng kh tr nng (argon hay hli) dn mu dng kh vo ct chit, th
mt nhm cc cht phn tch b pha tnh rn trong ct hp ph gi li, cn
cc cht khc th i qua. V th v bn cht n cng l s chit gia hai pha
kh v rn (pha chit l rn, cht phn tch c chit dng kh) khng tan
vo nhau. S chit y l theo c ch hp ph. Sau c th:
Ngi ta li lm nng ct hp ph v cng dng dng kh tr nng gii
hp cc cht phn tch a trc tip chng vo h ct ca my GC hay cho
chng tan vo mt dung mi hu c ph hp xc nh bng cch khc,
nh HPLC hay ph UV-VIS.
Hay cng c th gii chit cht phn tch ra khi ct chit bng mt dung
mi hu c thch hp ho tan tt cht v xc nh chng bng HPLC hay IR.
Phng php chit ny c ng dng cho c mu rn v lng, hay bn, hay
b thi, nhng ch cho cc cht phn tch l cc hp cht hu c c nhit
bay hi thp (di 150 oC) v d bay hi. Cch ny rt thch hp cho vic
chit cc cht hu c trong mi trng kh, hay cc mu rn, mu bt, hay
mu bn v mu nho. Tt nhin, vic trc tin l phi nh ho cc mu ny
bng mt dung mi thch hp, nh nc hay dung mi hu c c nhit
si cao. Cn cht hp ph y l cc ht silica rn xp c nhi vo ct
chit ng kn. N cng thng l cc silica trung tnh xp hay silica

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Ti liu ging mn k thut x l mu phn tch ha

c th ho (alkyl ho), tng t nh trong h chit NP-HPLC v RPHPLC.

K thut chit ny rt thch hp cho vic x l cc loi mu xc nh cc
cht hu c c nhit si thp (di 150 oC) v d bay hi trong cc loi
mu rn, mu bn, cc mu b thi v cc mu kh. N c u im l chn
lc cao, thch hp cho cc phng php phn tch HPLC, GC, hay GC-MS,
xc nh lng nh cc cht hu c, mt s hp cht c kim v mt s
cht v c, nh H2S, HCN, v.v.
5.4.2. Cc kiu trang thit b v mt s v d
Theo k thut ny trang thit b cng c hai loi l cc h n gin v h
hon chnh t ng theo chng trnh. Kh mang tr y l kh argon, hli
hay nit tnh khit (> 99,9%). C th trang b l gm cc b phn:
+ H ct chit kn v bung ct chit c gia nhit c,
+ Kh tr mang mu, cng nh ra gii cht phn tch (Ar, N2, hay He).
+ H my bm kh v nn kh mu vo ct chit.
Cc loi trang b ny hin nay u c cung cp trn th trng do cc
hng sn xut cc dng c phn tch.
V d 2: Chit ly mt s hp cht pesticide d bay hi trong cc loi
nc hay mu rn, bn (Method 502.2b. EPA). Ct hp ph l cht chit
pha rn loi LC2-25x1 cm. Mu c gi 150oC v dng kh tr Argon
thi qua bnh mu vi tc 0,8-1,0 mL/pht a cht phn tch vo ct
hp ph. Cc cht phn tch s c hp ph vo ct ny. Sau cng gii
hp cc cht trong ct hp ph bng dng kh tr nhng 200 oC, dn
vo my GC/MS tch v xc nh cc cht.

5.5. K thut vi chit pha rn (SPME)

K thut ny cng vn da trn c s s phn b ca cht phn tch X gia
hai pha khng ho tan vo nhau, trong pha mu cha cht X l lng, cn
35/44

Ti liu ging mn k thut x l mu phn tch ha

pha chit l cht rn. Song y pha chit (que chit) l cc ht cht rn xp
c ht vi micromet (m) c tm ln thanh que nh kim loi hay PE (1x4
mm) to thnh lp mng cht chit dy khong 0,3-0,5 mm bao xung quanh
to ra que chit. Que chit c trong h xy lanh v kim tim, c th
cm qua chit vo qua nt cao su ca bnh cha mu cn chit.
Qu trnh chit xy ra khi ta nhng que chit vo trong bnh mu theo mt
trong hai kiu:
+ Khng gian mu (cht dng lng). Vi cch ny pha mu phi c lc
u (hay khuy) lin tc khi chit v qua chit chm trong pha mu.
+ Khng gian hi (cht d ho hi). Vi cch ny, pha mu l hi, que chit
nm trong khng gian hi ca bnh mu, v mu phi c gia nhit ph
hp, cho cc cht bay hi t n trng thi cn bng gia pha mu ban
u (lng hay huyn ph) v pha hi ca mu.
Thi gian chit: 20- 30 pht.
Trang b ca k thut chit ny:
Bao gm (hnh ):
+ Bnh cha mu chit (dung tch 50 mL, nt cao su),
+ B Xylanh, kim tim v que chit,
+ My khuy v gia nhit cho bnh mu.
C ch ca s chit:
Ch c hai kiu l:
+ Hp ph pha thng (cht chit pha thng),
+ Hp ph pha ngc (cht chit pha ngc),
Vn ny xem trong mc chit pha rn trnh by trn.
u nhc im v ng dng
K thut chit ny:
+ n gin, d thc hin,
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Ti liu ging mn k thut x l mu phn tch ha

+ Thch hp cho xc nh cc cht vi lng,

+ Lm giu c cht,
+ Ch yu cho xc nh cc cht hu c v mt s kim loi nng.
K thut ny mi ra i v cn ang pht trin. Song cng c ng dng
c hiu qu, nht l trong lnh vc phn tch cc ho cht bo v thc vt v
thuc tr su.

5.6. K thut chit Soxhlet

5.6.1. Nguyn tc chung
Chit Soxhlet l mt kiu chit lin tc c bit c thc hin nh mt loi
trang b chit ring. Kiu chit ny cng nh kiu chit lng lng, nn v
bn cht ca s chit n vn l da trn c s quy lut phn b cht trong
hai pha khng trn vo nhau. Song y pha mu l trng thi lng, bt,
ht hay dng mnh, hay dng l u c c. Cn dung mi chit (cht hu
c) l dng lng. V d nh chit ly du melton t l cy bc h bng
dung mi hu c n-Hexan, hay benzen. Chit cc thuc tr su hay
HCBVTV trong mu rau qu, mu t bng n-Hexan.
V th y l kiu chit ca h chit c th c ng th v d th. Trong thc
t c dng ch yu l h d th, m cht phn tch trong mu rn, bt, l,
si, v.v m cc k thut chit nu trn khng lm c tt, c bit l
chit cc cht hu c trong cc mu khng dng lng (h chit d th).
5.6.2. Cc trang thit b v v d
Trang thit b ca k thut chit ny c hai loi l:
1 1. Cc h chit Soxhlet thng v n gin.
2 2. Cc h chit Soxhlet t ng (Auto-Soxhlet).
Cch chit theo h loi 1 l n gin, vn hnh bng tay, cn cch chit theo
h my loi 2 l vn hnh mt cch t ng theo chng trnh. K thut
chit ny ch yu c s dng chit tch cc cht hu c nm trong mu
37/44

Ti liu ging mn k thut x l mu phn tch ha

dng rn, hay dng bt, hay mnh nh, hay cc vt liu mu kh (nh l
cy, dc liu,..). V th n l cc h chit d th.
V d 1: Chit Soxhlet thng ly mt s ho cht BVTV t mu rau
qu. Ly 10 g. mu c nghin nh v trn u vo cc ng mu ca
h chit, thm 25-30 g. Na2SO4 khan, trn u, 50 mL dung mi chit nHexan c 20 % Cl2CH2. Sau tin hnh chit trong vng 5-6 gi lin tc,
yn 10 pht, tch ly pha hu c n-Hexan c cha cht phn tch v xc
nh chng trong pha hu c ny bng phng php ph hp chn.
5.6.3. Cc u nhc im v phm vi ng dng
K thut chit ny c u im l chit trit , song cc iu kin chit phi
nghim ngt v thi gian chit cng di, th mi c kt qu chit tt. V th
h thng vn hnh t ng (auto-Soxlet) cho kt qu tt hn. N thch hp
cho vic chit lng vt cc cht hu c, nht l cc cht c hi t cc i
tng mu khc nhau, cht phn tch c trong mu trng thi rn, bt, vt
mu xp kh (l cy), v.v. K thut chit ny c ng dng ch yu
chit cc HCBVTB t cc mu cy, l, rau qu, thc phm, mu t.

5.7. K thut chit Siu m

5.7.1. Nguyn tc chung
Qu trnh chit siu m cng vn da trn c s chung ca s chit l
s phn b ca cht vo hai pha khng trn ln vo nhau, ch c khc l
c thc hin trong mi trng c thm tc dng ca nng lng sng
siu m (nng lng tia Vi sng). Pha cha mu phn tch cn chit l pha
nc v pha lng chit cht phn tch l dung mi hu c (pha th hai)
u

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Ti liu ging mn k thut x l mu phn tch ha - Vin KNATVSTP quc gia

c cho vo bnh chit, sau c t vo trong hp chit ca h chit vi

sng v tin hnh chit di tc dng ca sng siu m thch hp trong mt
thi gian nht nh (1,5- 2 gi). Cch chit ny c th c thc hin hai
trng thi mu ng th v d th.
a)H chit ng th (h lng-lng), y cht mu phn tch tan trong
dung mi lng, nh nc v dung mi chit cng l cht lng, thng l cc
dung mi hu c khng tan trong nc. V d nh chit cc ion kim loi
nng (Cd, Cu, Fe, Mn, Ni, Pb, Zn,..) t nc bin mi trng pH=4 bng
dung mi MIBK c cha thuc th APDC 0,1%. Sau xc nh cc kim
loi ny bng php o ph F-AAS.
b)H chit d th (h rn-lng), trng hp ny, mu phn tch l trng
thi rn, thng c nghin thnh bt, hay c bm nh v b vo trong
bnh chit c dung mi chit. Dung mi chit l cc dung mi hu c. V d
chit ly du Menton t l bc h bng dung mi chit Benzen.
Khi chit, di tc dng ca nng lng sng siu m c tn s cao, mng
cu trc ca cc phn t cht mu b ph v, cht phn tch c gii phng
v phn b (hay tan) vo trong dung mi chit theo tnh cht ca n dng
phn t hay dng hp cht phc v y h s phn b K pb ca cht gia hai
pha khng trn ln vo nhau cng l yu t quyt nh hiu qu chit. Cn
nng lng siu m c tc dng chnh l ph v cu trc ban u ca mu,
xo trn hn hp chit, to iu kin tt cho cn bng chit xy ra d dng,
nhanh hn v trit hn.
5.7.2. Cc kiu chit v trang thit b
thc hin chit theo k thut ny chng ta phi c h thng bnh chit
kn v h bung chit to siu m. Cc thit b ny, hin nay u c bn trn
th trng theo cc quy m to nh v mc chit khc nhau, chit phn
tch hay chit bn sn xut. V nguyn tc n gm hai b phn chnh l:
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Ti liu ging mn k thut x l mu phn tch ha - Vin KNATVSTP quc gia

1. Bung chit siu m khng ch c nng lng siu m.

2. Cc rotor cha bnh ng mu chit (loi 6 bnh, 9 bnh hay 12 bnh)
vi dung tch mi bnh l 200, 150, 100, v 50 mL.
V d : Chit tch ly mt s ho cht BVTV t mu t hay mu rau
qu. (nh Metyl-parathion,Sumithion,Diazinon). Ly 10 g. mu t c
nghin nh cho vo bnh chit, thm 40 mL etyl-axetat, trn u, t bnh
mu vo h my chit, tin hnh chit trong 90 pht, ngui yn 10 pht,
tch ly pha hu c etyl-axetat c cha mt s ho cht BVTV. Di pha hu
c ny qua ct sc k hp ph (c cha Al 2O3+than hot tnh+Na2SO4 khan )
lm sch cht v lm kh. Sau ra gii ct ny bng 10 mL etyl-axetat,
thu ly dung dch ra gii ny xc nh cc ho cht BVTV (nh Metylparathion, Sumithion, Diazinon,v.v.) bng GC/ECD, HPLC/MS, hay
GC/MS.
K thut chit ny c u im l trit v hiu sut cao, nhng i hi
phi c h trang b chit siu m, c cc rotor chit cho mi cch chit khc
nhau v mi loi mu khc nhau. K thut chit ny cha c ng dng
ph bin. Ch mt s vin nghin cu mi c trang b ny. Nn hin nay
nc ta cn t c dng v cha ph bin, nn nhiu ngi cha bit.

5.8. K thut sc k trong x l mu

Hin nay, sc k l mt loi phng php tch v xc nh ng thi cc
cht trong mt hn hp, song n cng l mt k thut x l mu phn tch tt
cho nhiu trng hp tch v lm giu ly cc cht cn phn tch. Trong
phn tch c ng dng x l mu phn tch ch yu l 2 loi l: a). sc
k ct v b). sc k phng (sc k lp mng v sc k giy).

5.8.1. K thut sc k ct
5.8.1.1. Nguyn tc v iu kin

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Ti liu ging mn k thut x l mu phn tch ha - Vin KNATVSTP quc gia

Nguyn tc chung
+ K thut x l mu ny da trn c s tnh cht hp ph hay trao i ion
ca cc cht phn tch hp thu cht phn tch ln cht nhi (pha
tnh) trong ct sc k, gi v tch chng ra khi cc cht khc c
trong mu ban u. Sau dng mt dung mi thch hp (pha ng)
ra gii v tch n ra khi ct sc k, ri xc nh chng trong pha ng
ny bng mt phng php ph hp. V d nh AES, AAS, UV-VIS, HPLC,
GC, EC, CEC,.. V th trc ht phi a mu phn tch v dng dung dch,
c th np cht mu vo ct sc k c.
S tch y l da trn s phn b ca mt nhm cht phn tch gia hai
pha khng trn vo nhau, pha tnh (cht rn sc k), pha ng (cht lng,
dung mi ra gii). V th n cng tng t nh k thut chit pha rn. Ch
yu c s dng cho x l mu l:
Trc tin l sc k ct hp ph (pha thng v pha ngc) dng pha tnh
l cc Silica hay nhm xit xp, c c ht 25-70 m.
Tip n l sc k trao i ion trn ct ca pha tnh trao i ion (trao i
Cation v Anion).
5.8.2. Cc iu kin sc k
i vi sc k ct c c s tch tt cc cht phn tch, cn phi:
Chn pha tnh c tnh cht chn lc cho mt nhm cht phn tch,
Dung mi lm pha ng sc k phi c tinh khit t yu cu,
Chn pha ng ph hp cho cht cn x l, thu c s tch tt.
Cn bng trong qu trnh sc k xy ra nhanh v c tnh thun nghch.
Chn iu kin sc k thch hp (pH, T,..) gp c cht phn tch vo
mt nhm hay tch ra thnh tng cht th cng tt, cng nh lm giu chng.
5.8.3. Trang b v cch x l

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Ti liu ging mn k thut x l mu phn tch ha - Vin KNATVSTP quc gia

Mun thc hin tch cht theo kiu ny chng ta phi c cc h trang b sc
k ph hp. C th ch l cc ct tch n gin v cng c th l cc h
thng t ng hon chnh. Tu loi cht phn tch, m chng ta c th chn
h pha sc k hp ph, hay h pha trao i ion tch ly cc cht cn phn
tch. N bao gm cc b phn:
Trc ht l h ct sc k cha cc cht sc k, n l cc cht Silica, hay
oxit Al xp c kh nng sc k hp ph, hay cht trao i ion (cation hay
anion) vi mt nhm cc cht phn tch nht nh c trong mu. Khi cn ct
sc k cn phi t trong bung iu nhit, khng ch nhit thch hp.
Cc dng c np dung dch mu ln ct sc k, khng ch tc np v
ra gii cht phn tch ra khi ct.
Th ba l cc dung mi ho tan mu phn tch thnh dung dch c c
th np c mu ln ct sc k.
Th t l cc dung mi pha ch pha ng phc v cho vic ra gii cc
cht phn tch ra khi ct sc k.
5.8.4. V d ng dng
V d 3: X l mu xc nh mt s anion trong mu nc v d:
Cl-, Br-,I-, NO3-, SO42-,, v.v). Trc ht mu nc (250 mL) phi chnh pH=8,
v lc b cn. Sau np ln ct sc k pha tnh trao i in loi Dowex50A12-OH (150 x 8 mm) vi tc chy 1-2 mL/pht, cc anion c
gi li trn ct sc k. Khi mu chy ht, di qua ct 5 mL nc ct hai ln.
Sau dng 20 mL dung dch NaOH 0,5M ra gii cht phn tch ra khi
ct sc k vi tc 1-1,5 mL/pht. Nh vy cht phn tch s tan vo pha
ng ra gii, v tin hnh xc nh n trong pha ng ra gii ny bng
mt trong cc phng php AES, AAS, UV-VIS. Cch ny c th dng
x l mu cho xc nh mt s anion trong cc loi nc thi, nc sng h,
v.v.
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Ti liu ging mn k thut x l mu phn tch ha - Vin KNATVSTP quc gia

5.8.5. K thut sc k phng (sc k giy v sc k bn mng)

5.8.5.1. Nguyn tc chung
Qu trnh sc k y l da trn c s trong mt h pha dung mi nht
nh, th s di chuyn v phn b ca cc cht phn tch trn mng phng
(lp mng phng) silicagel xp c trng trn bn thu tinh hay polyme
cng, hoc l s phn b ca cht trn bn giy xp sc k l khc nhau
to ra s tch sc k ca cc cht. Trong qu trnh sc k cc cht s di
chuyn khc nhau to ra mi cht s c mt vng ring trn bn mng v
tch khi nhau. V th mi c tn l sc k phng (sc k bn mng v sc
k giy). V qu trnh sc k xy ra trn mt mt phng nh (v d 4x20 cm)
ca nguyn liu c tnh cht sc k, l bn giy sc k hay bn mng
Silicagel.
c trng cho qu trnh sc k ca cc cht phn tch y l h s chy Rf
ca cht trn mt phng tch (tm giy hay bn mng Silicagen). Trong mt
h pha sc k v trong mt iu kin nht nh ph hp, mi cht phn tch
s c h s Rf ny khc nhau v to ra s sc k ca cc cht trong mt hn
hp mu. H s Rf ny c xc nh bi:
+ Bn cht ca cc cht sc k (giy sc k hay Silica gel),
+ Bn cht ca cc cht phn tch trong mu,
+ Bn cht v tnh cht ca h pha ng chy (hay khai trin) sc k,
+ iu kin chy sc k, ch yu l nhit v p sut hi pha ng trong
bnh trin khai sc k.
5.8.5.2. Cc trang b, cch tin hnh v v d
Mun thc hin tch cht theo kiu ny chng ta phi c cc h trang b sc
k phng, n bao gm:
Cc loi bn mng sc k, c th l:
+ Bn mng Silicagel hay oxit Al trn tm thu tinh hay PE
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Ti liu ging mn k thut x l mu phn tch ha - Vin KNATVSTP quc gia

+ Bn giy sc k xp c kh nng hp ph cc cht phn tch.

Cc h dung mi ho tan mu phn tch,
Cc bnh hay hp chy sc k (trin khi sc k).
Pha ng hay h dung mi chy sc k (pht trin sc k).
B trang b pht hin cc cht sau khi tch trn bn mng.
Tu loi cht phn tch, m chng ta c th chn h pha sc k giy hay sc
k lp mng Silicagel hoc oxit nhm. Bn mng hay giy sc k sau khi
chm mu (nh mu) ln c lm kh v ngm vo dung mi (pha ng)
trong bnh chy sc k. Lc ny cc cht phn tch s chy theo dung mi t
di ln trn, v to thnh tng vng cht sau mt thi gian nht nh. Sau
khi chy sc k, lm kh bn sc k, phun cht hin mu nhn bit cc
vng cht v tch cc vng mu ho tan vo dung mi ph hp v xc
nh cc cht bng cc phng php ph phn t (hp th UV-VIS ), HPLC,
hay GC. Cng c th o trc tip cng mu trn vng mu bng my
ph phn x UV-VIS, hay cc my Densitometer.

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