BI 1: NH TNH PHM MU HU C TNG HP TRONG CM CANXI BNG SC K GIY

I. NGUYN TC
Sc k giy l loi sc k dng giy lm gi mang pha tnh. Trong loi sc k ny pha ng v pha tnh u l cht lng. Pha tnh c hp ph trong cc l xp ca gi mang. Nh vy sc k giy l sc k phn b lng-lng, da vo h s phn b khc nhau ca cc cu t trong hn hp 2 cht lng khng ha tan vo nhau tch cc cu t ny. Trong sc k giy pha tnh thng dng l nc. Ngoi ra cng c th dung mt s dung mi khc lm tng tnh tm ln giy nh du silicon, du paraffin Sau khi chm hn hp ln giy, cho dung mi th 2 (pha ng) i qua, cc cu t hn hp s tch ra trn giy. Trong bi ny pha ng s l hn hp dung mi: etanol-amoniac-nc (12,5:2,5:85).

II. KT QU

10.5 (cm)

8.9 7.7 5.8 4.8 3.8 5.0 7.7 7.9

2.3

SY

M1

DE

DP

M2

GT

M3

VT

XB

Tnh Rf v nh tnh cc phm mu: b (cm) 10.5 a (cm) SY DE Mu chun DP GT VT XB M1 Mu phn tch M2 M3

Rf

3.8 0.36 Kt qu:

2.3 0.22

5.0 0.48

5.8 0.55

7.9 0.75

9.0 0.86

4.8 0.46

7.7 0.73

7.7 0.73

8.9 0.85

Mu 1: DP ( Poceur) Mu 2: VT (vng Tartazin) Mu 3: VT v XB (xanh Brillant)

III. TR LI CU HI
1. Nguyn tc v c ch chnh trong sc k giy:

Sc k giy l loi sc k dng giy lm gi mang pha tnh. Trong loi sc k ny pha ng v pha tnh u l cht lng. Pha tnh c hp ph trong cc l xp ca gi mang. Nh vy sc k giy l sc k phn b lng - lng, da vo h s phn b khc nhau ca cc cu t trong hn hp 2 cht lng khng ha tan vo nhau tch cc cu t ny. Trong sc k giy pha tnh thng dng l nc. Ngoi ra c th dng 1 s dung mi khc lm tng tnh tm ln giy nh du Silicon, du parafin.. Sau khi chm hn hp ln giy, cho dung mi th 2 (pha ng) i qua, cc cu t ca hn hp s c tch ra trn giy.
2. ng dng v u nhc im ca sc k giy:

ng dng: - nh tnh v th tinh khit: Thung sc k so snh vi cc cht chun nh tnh (da vo gi tr Rf ). nh tnh mt cht tng i chc chn cn tin hnh sc k vi t nht vi h dung mi khc nhau. V cht th c coi l tinh khit khi sc k khng c vt l. - Bn nh lng v nh lng: C nhiu phng php nh lng cc cht sau khi tch v pht hin vt ca chng nh o chiu di vt, o chiu di vt, o in tch vt, o cng mu ca vt.Phng php thng dng nht l phng php ra.

 u v nhc im ca phng php sc k giy: u im: - K thut v dng c n gin, d thc hin. - L phng php vi phn tch v lng mu cn dng nh (1g). - C th ng dng xc nh nhiu ch tiu nh nh tnh, nh lng, xc nh tp lin quanHin l phng php n gin nht tch v pht hin cc hp cht c cha nguyn t phng x. - R tin. Nhc im: - Khng lm sc k ch ha bng sc k giy. - Khng dng c cc ha cht c tnh n mn trong pht hin vt. - Thi gian khai trin lu t 4 - 5 gi (mt s mu khai trin t 2 3 ngy). - Giy d hp th cc cht khc c trong mi trng nn phi bo qun giy sc k tht k.
3. Vi cc bc tin hnh trong sc k giy, giai on c th gy sai s nhiu

nht cho kt qu phn tch l giai on chun b mu. Cht th cn phi loi tp hon ton. Nu nh trong mu cn ln nhiu tp cht th nh hng n kh nng phn b ca cht th (Rf). Bn cnh cht th phi c ho tan hon ton vi lng dung mi thch hp

BI 2: TCH V NH TNH CC SULFONAMIDE BNG SC K LP MNG

I. TIN HNH TH NGHIM:
1. Chun b vt liu: -Ly 2 ming bng mng kch thc 13cm x 5cm. K ng gii hn, cch mi cnh bn 0.5cm, chia u v chm 6 im

-Bnh khai trin: Cho dung mi (24 ml chloroform v 8 ml eter) vo bnh khai trin, chiu cao dung mi 1 cm ( bo ho dung mi trong 30 pht) 2. Chit sulfonamide -Ly 3 l ng cc mu sulfamide A, B, C, nghin mn, chit tng mu bng cn etylic 2 ln mi ln 10 ml. Lc vo cc thu tinh, lm bay hi trn bp cch thu cn khong 3 ml. Cc dung dch ny dng chm ln bng mng 3. Trin khai sc k: -Chun b bng mng v cc ng mao qun -Chm cc vt: chm 3 vt mu sulfonamide chun bit tn v 3 vt hn hp mu -t bn vo bnh khai trin, nhng vt ny phi nm trn mc dung mi 1 cm. y bnh v trin khai n khong 10 cm trn vt chm, ly bn ra khi bnh v vch chnh xc ng dung mi 4. Pht hin: - kh bn khai trin ngoi khng kh sau phun thuc th PDAB thy c vt mu vng -Tnh Rf

II. KT QU:
Sc k
6.2 cm

0.
1.6 0.9 1 A 2 1.0 B 3 1.6 C

Vi: 1: sulfanilamide 2: sulfamethoxazon 3: sulfaguanidin

Vy: A: sulfaguanidin B: sulfanilamide C: sulfamethoxazon

Bng gi tr Rf

a (cm) 5.5 Rf

b (cm) Mu chun 1 2 0.9 1.6 0.145 0.258

3 0.0 0.0

Mu phn tch A B 0.0 1.0 0.0 0.161

C 1.6 0.258

III. TR LI CU HI

1. C ch to mu ca sulfonamide v PDAB: Sulfonamide l cc dn xut ca Sulfoanilin c cu to:

NH2

S X

Nu X l: NH2 Nu X l:- HN
N
- NH

Sulfanilamid

Sulfamethoxazone O CH3 NH2 NH Sunfaguanidine

Nu X l:

- C ch to mu ca sulfonamid vi PDAB:
H :N H SO2X

O Me2N CH Me2N

CH

H Me2N C

H N
+

H H SO2X Me2N C N :OH H

+

SO2X

O- H

H H Me2N C H
+

SO2X

-H O 2

H H Me2N C
+

N ..

SO2X

OH2

H Me2N C N SO2X

Hp cht Imin c mu vng

2. Silicagel dng trong sc k lp mng: - L Kieselgel Gel ca acid Silicic, l cht hp ph c s dng rng ri nht hin nay.
-

Kch thc ht: 10 - 40m. Din tch b mt 200 400m2/g.

- Silicagel loi ny c loi st bng cch un vi HCl m c, sau dng

nc ra sch ion Cl- v lng gn loi cc ht nh l lng, cui cng sy 120oC trong 48 gi. - Hot tnh hp ph ca n do nhm OH trn b mt quyt nh. Do hm lng m tng s lm gim hot ca silicagel. Cu trc silicagel
HO OH HO

Si :
O

OH HO

Si
O

Si

OH

BI 3. SC K CT
I. NGUYN TC
- Da trn kh nng trao i ion ca nha cationid, tin hnh xc nh hm lng ion Ca2+ trong mu nc cng trc v sau khi qua ct sc k bng phng php nh phn vi dung dch EDTA chun dng ch th Murexide. T xc nh dung lng trao i ca nha i vi ion Ca2+ .

- Da trn kh nng hp ph ca Al2O3 tin hnh tch hn hp mu Methyl orange v Methylene blue bng sc k ct vi dung mi ra gii ln lt l cn tuyt i v nc ct.

II. KT QU TH NGHIM
1. nh lng ion Ca2+ trong mu nc cng trc v sau khi qua ct trao i cation

Phn ng nh tnh ion Ca2+ : 2C12H25SO3Na + Ca2+ (C12H25SO3)2Ca + 2Na+

Phn ng nh lng ion Ca2+ bng phng php Complexon: Phn ng chun : Ca2+ + Y4- CaY21(mol) 1(mol) 1(mol) Gi V1 l th tch EDTA vi C(M) dng (ml). V l th tch mu nc ly lm th nghim (ml).

Ti im tng ng: nCa = nY = C x V (mmol)

2+ 4

Khi lng Ca2+ trong mu nc cng ban u: mCa 2 + = nCa 2 + 40 = C V 40 (mg)

Trong V1 (ml) mu nc ban u c C V 40 (mg) Ca2+ Vy trong 1lt mu nc c X(mg) Ca2+ Do : X =

C V1 40 1000 C V1 4.10 4 = (mgCa 2+ / lit ) V' V'

kt qu phn tch c chnh xc ta tin hnh chun mu trng. Gi s th tch EDTA dng chun mu trng l Vo (ml) th:
(V V0 ) (mgCa 2+ / lit ) ' V

X = 4.10 4 C

Th tch EDTA (ml) Mu trng (Vo) Mu nc cng ban u (V1) Mu nc cng sau (V2)

11

4.5

Hm lng ion Ca2+ trong mu nc cng ban u: Vi: V= 10 ml V1= 11 ml Vo= 0 ml C= 0.01M
(11 0) = 440(mgCa 2+ / lit ) 10

X = 4.10 4 0.01

Hm lng Ca2+ trong mu nc cng sau khi qua ct trao i Ion:

(4.5 0) = 180(mgCa2 + / lit ) 10

X ' = 4.10 4 0.01

2. Tch hn hp Methyl orange v Methylene Blue bng sc k ct (Al2O3) Chun b ct: nhi ct bng 5g Al2O3 cng vi nc.

Ly 2ml dung dch cn phn tch rt vo ct. Ra gii tng phn trn ct: phn methyl orange c ra bng nc, phn methylene blue c ra bng etanol.

III. TR LI CU HI
1. Tnh dung lng trao i Ion ca nha i vi Ion Ca2+: S mmol ion Ca2+ Dung lng trao i ion = S gam nha Cationid S mmol Ca2+ ban u:
nCa 2 + = C (V1 V0 )(mmol )

(mmol Ca2+/g)

S mmol Ca2+ sau khi qua ct trao i:

nCa 2 + = C (V2 V0 )( mmol ) S mmol Ca2+ trao i: nCa 2 + = C (V1 V0 ) C (V2 V0 )

Hay:
nCa 2 + = C (V1 V2 )( mmol )

Do :
C (V1 V2 ) 0.01 (11 4.5) = = 13 10 3 (mmolCa 2+ / g ) mcationid 5

DLT ION =

Vy: Dung lng trao i Ion ca nha i vi Ca2+ bng 13 10 3 (mmolCa 2+ / g ) . 2. Methyl orange v Methylene Blue: a) Methyl orange:

Cng thc phn t: C14H14O3N3SNa.

Danh php: p-(p-dimetyl aminophenylazo)-benzensulfonate Natri; 4-

dimetylaminoazobenzen-4-sulfonate Natri; Dacan III. Cng thc cu to:

H3C H3C N N N SO3Na

Tnh cht: - Dng rn l nh hoc ht mu da cam vng. - Tan t trong nc lnh ( tan 0,2g) to dung dch mu vng. - Khng tan trong ru Etylic. - Metyl da cam i mu t hng trong mi trng acid sang vng nht

trong mi trng baz. ng dng:

- Lm ch th pH, chuyn mu t sang vng trong khong pH = 3.04.0. - Xc nh Sn2+ bng phng php phn tch th tch (un nng lm mt mu thuc th). - Pht hin cc cht kh mnh (Ti3+, Cr2+,...) v cht oxy ha mnh (Cl2, Br2) do cc cht ny lm cht mu ch th. b) Methylene Blue:

Cng thc phn t: C16H18N3SCl.3H2O

Danhphp:3,9-bis-Dimetylaminophenazothioninclorua;Tetrametylen-

Thioninclorua trihydrat. Cng thc cu to:

N (CH3)2N S N(CH3)2
+ Cl . 3 H2O

Tnh cht: - Tinh th mu xanh l cy thm c nh ng hoc l bt nh mu

xanh l cy thm. - Kh tan trong nc lnh v ru Etylic, khi un nng d tan hn to dung dch mu xanh. - Khng tan trong Eter, Benzen, CH3Cl. Tan trong H2SO4 m c cho dung dch vng nht. - Xanh l cy khi pha long bng nc th chuyn sang mu xanh lam. - Mt mu xanh khi phn ng vi Zn bt hoc dung dch Iod. - Dung dch NaOH lm dung dch t mu xanh chuyn sang tm. ng dng: - Lm ch th oxy ha -kh. - Dng trong phn tch th tch, phng php o mu xc nh th oxy ha kh.

- Dng trong php soi knh hin vi v lm cht nhum mu trong vi sinh vt hc.