CNG N THI THC TP HA DC

(c p n)
Lp H Dc
Ni dung 1. Trnh by l thuyt thc hnh
- nh tnh:
1. C ch phn ng to mui ca vitamin C vi st (II) sulfat ?
2. C ch phn ng xc nh acid salicylic trong aspirin ?
3. C ch phn ng to phm mu nit ca paracetamol ?
4. Xc nh h s hp th ring E (1%, 1 cm) ca acid ascorbic ?
- TTK:
5. Nguyn tc xc nh gii hn tp cht sulfat (SO42-) ?
6. Nguyn tc xc nh gii hn tp cht clorid (Cl-) ?
7. Nguyn tc xc nh tp cht iodid (I-) trong natri clorid dc dng ?
- nh lng:
8. Nguyn tc nh lng natri clorid dc dng, phng php I ?
9. Nguyn tc nh lng paracetamol bng quang ph UV ?
10. Nguyn tc nh lng vitamin C bng php o Iod ?
Ni dung 2. Thc hnh thc nghim
(Thc nghim, khng trnh by l thuyt php th)
- nh tnh:
1. Thc hin phn ng paracetamol vi FeCl3 ?
2. Thc hin phn ng to phm mu nit ca paracetamol ?
3. Thc hin phn ng nh tnh ion clorid (Cl-) trong natri clorid ?
4. Thc hin phn ng acid ascorbic vi st (II) sulfat ?
5. Thc hin phn ng acid ascorbic vi AgNO 3 ?
6. Thc hin phn ng nh tnh acid salicylic trong aspirin ?
7. Thc hin phn ng to methyl salicylat ca aspirin ?
8. Thc hin phn ng to thiocrom ca vitamin B1 ?
9. Thc hin phn ng pyridoxin hydroclorid vi FeCl3 ?
10. Thc hin phn ng mu Murexit ca cafein ?
11. Xc nh tr s E (1%, 1 cm) ca acid ascorbic ?
- Th TK:
12. Tin hnh pht hin gii hn tp sulfat trong natri clorid dc dng.?
13. Tin hnh xc nh tp iodid trong natri clorid dc dng ?
14. Tin hnh pht hin gii hn tp Cl- trong paracetamol ?
15. Tin hnh pht hin gii hn tp SO42- trong paracetamol ?
16. Xc nh Mg++ v kim loi kim th trong natri clorid dc dng ?
17. Xc nh tp Ba++ trong natri clorid dc dng ?
- nh lng:
18. Tin hnh nh lng NaCl dc dng ?
19. Tin hnh nh lng vitamin C bng php o iod ?
20. Tin hnh nh lng paracetamol bng quang ph UV ?
1

P N L THUYT THC HNH

1. C ch phn ng to mui ca vitamin C vi st (II) sulfat ?
Acid ascorbic (vitamin C) l acid nn to mui vi kim loi nh Fe 2+,
Cu2+,V l acid yu kh phn ly trong nc nn phi qua dng mui natri:
R

R
O
+

HO
OH
acid ascorbic

NaOH
H2O

NaO

FeSO4

ONa

O
Fe
ascorbat Fe

Dung dch ascorbat natri to ascorbat st mu xanh vi FeSO4.

2. C ch phn ng xc nh acid salicylic trong aspirin ?
Aspirin l ester ca acid salicylic vi acid acetic.
Pht hin acid salicylic trong aspirin cn qua thy phn aspirin trong mi
trng kim v un nng:
COOH

COONa
OCO CH3

OH

H2O

COOH
OH

HCl

NaOH

Aspirin

Acid salicylic

Sau thy phn acid salicylic dng mui natri, acid ha bng HCl s kt
ta mu trng. Ta ny sau ra sch cho mu tm- vi FeCl3.
3. C ch phn ng to phm mu nit ca paracetamol ?
Sau thy phn paracetamol trong mi trng HCl 10% gii phng hp
cht amin thm I l p-hydroxyanilin:
HO

NHCO CH 3

+ H 2O

HO

HCl , t o

Paracetamol

NH 2 . HCl

p-hydroxyanilin

Cho dch thy phn phn ng vi NaNO 2 to mui diazoni, ngng t vi

2-naphtol /NaOH 10% to phm mu (phm mu nit).
Ar-NH2 + NaNO2 + 2HCl [Ar-N N +] Cl- + NaCl + 2H2O
[Ar-N N +] Cl- + 2-naphtol /NaOH
Ar N N
HO
Mu gc phm mu l mu .
Tuy nhin c th xy ra phn ng oxy ha kh gia p-hydroxyanilin cha
nhm OH phenol, vi NO2- to mu xanh tm. V vy mu cui cng ca phn
ng ngng t cn l mu vang.
4. Xc nh h s hp th ring E (1%, 1 cm) ca acid ascorbic ?
Acid ascorbic (vitamin C) hp th UV c MAX 243 nm.

Tr s hp th ring E (1%, 1 cm) ca acid ascorbic dc dng qui nh

nm trong khong 545-585.
Xc nh tr s E (1%, 1 cm) ca acid ascorbic theo phng trnh (1):
E (1%, 1 cm) = E / C
(1)
E = hp th ca dung dch acid ascorbic o c.
C = Nng (%) dung dch acid ascorbic dng o trn my.
Nguyn tc tin hnh:
- Pha dung dch acid ascorbic th sao cho hp th ca dung dch trong
khong 0,5-0,6; o hp th E ca dung dch trn my quang ph UV-VIS,
bc sng 243 nm.
- Tnh nng acid ascorbic C (%) ca dung dch o.
Theo phng trnh (1) tnh c tr s E (1%, 1 cm).
5. Nguyn tc xc nh gii hn tp cht sulfat (SO42-) ?
Nguyn tc: Dng phn ng ion Ba++ vi ion SO42- tao c ca ta BaSO4:
Ba++ + SO42- BaSO4
So snh c ng th vi ng i chiu ion sulfat:
Tin hnh theo cc bc:
- Chn 2 ng nghim ging nhau theo qui nh ca dc in VN v cht
liu thy tinh, kch thc. nh du qui nh ng th v ng i chiu.
- Tin hnh ng thi phn ng to c cho ng th v ng i chiu.
- yn cc ng khong 5 pht. So snh c ca 2 ng, nhn theo trc
ng nghim, trn nn mu en, trong nh sng khuych tn ban ngy.
Nhn nh kt qu:
- Nu ng th c hn ng i chiu: Khng t.
- Nu c ng th bng hoc km hn c ng i chiu: t.
Ghi ch: Sinh vin trnh by c th hn s cho tng im.
6. Nguyn tc xc nh gii hn tp cht clorid (Cl -) ?
Nguyn tc: Dng phn ng ion Ag+ vi ion Cl - tao c ca ta AgCl
Ag+ + Cl - AgCl
So snh c ng th vi ng i chiu ion sulfat:
Tin hnh theo cc bc:
- Chn 2 ng nghim ging nhau theo qui nh ca dc in VN v cht
liu thy tinh, kch thc. nh du qui nh ng th v ng i chiu.
- Tin hnh ng thi phn ng to c cho ng th v ng i chiu.
- yn cc ng khong 5 pht. So snh c ca 2 ng, nhn theo trc
ng nghim, trn nn mu en, trong nh sng khuych tn ban ngy.
Nhn nh kt qu:
- Nu ng th c hn ng i chiu: Khng t.
- Nu c ng th bng hoc km hn c ng i chiu: t.
7. Nguyn tc xc nh tp cht iodid (I-) trong natri clorid dc dng ?
Nguyn tc:
Khi trn natri clorid th vi vi hn hp NaNO 2 v acid sufuric, tp I
phn ng vi NO2-, gii phng iod:
2I- + 2NO2- + 4H+ I2 + 2NO + 2H2O
Iod gii phng gp h tinh bt s cho mu xanh.
3

Nhn nh kt qu:
Sau khi tm t NaCl th vi hn hp NaNO2, H2SO4 v h tinh bt:
- Mu th xut hin mu xanh: Khng t.
- Mu th khng xut hin mu xanh: t.
8. Nguyn tc nh lng natri clorid dc dng, phng php I ?
Natri clorid l mui halogen nh lng bng phng php o bc:
AgNO3 + NaCl AgCl + NaNO3
Phn ng trong mi trng trung tnh, ch th l kali cromat K2CrO4
Ht Cl-, ion Ag+ phn ng vi ion cromat to mu bo im kt thc:
2Ag+ + CrO42-
Ag2CrO4
Tnh hm lng H (%) ca NaCl trong mu th theo cng thc:
V . E . F . 100
H (%) =
m (g)
V (ml): Th tch AgNO3 0,1 M tiu th trong php nh lng.
E: Tr s 1 ml AgNO3 0,1 M tng ng 5,844 mg NaCl.
V hm lng tnh ra % nn i E sang n v g
E = 0,005844 g
F: H s hiu chnh ca dung dch AgNO 3 0,1 M. V pha t ng
chun nn ly F = 1,00
m (g): Khi lng NaCl cn nh lng, tnh ra g
9. Nguyn tc nh lng paracetamol bng quang ph UV:
Paracetamol hp thu bc x UV, MAX 257 nm, dung mi NaOH 0,1 M.
Tr s hp th ring E (1%, 1cm) 257 nm bng 715.
Pha dung dch o paracetamol trong NaOH 0,1 M qua 2 bc (2 d.d.)
- d.d. 1: 40 mg paracetamol pha trong NaOH 10% va 250 ml.
- d.d. 2: Pha long 5 ml d.d. 1 thnh 100 ml bng NaOH 0,1 M v nc.
Ly d.d. 2 lm dung dch o.
o hp th ca d.d. 2 c tr s hp th E.
Tnh hm lng (%) paracetamol trong ch phm nh sau:
E
1). Tnh nng (%) d.d. 2: C (%) =
E (1%, 1 cm)
2). Tnh hm lng H (%) paracetamol theo cng thc:
C . F . 100
H (%) =
m (g)
m (g) = khi lng paracetamol cn nh lng ( 0,040 g)
F = pha long, tnh theo cng thc: F = (f1 f2) / 100
Trng hp paracetamol:
f1: Pha long ln 1: (40 mg/ 250 ml), f1 = 250
f2: Pha long ln 2: (5 ml thnh 100 ml), f2 = 20
100: Ly 100 ml lm n v (C tnh bng nng phn trm).
F = (250 20) / 100 = 50
4

10. Nguyn tc nh lng vitamin C (acid ascorbic) bng o Iod:

Acid ascorbic cha cu trc endiol c tnh kh, nh lng bng o iod:
R

R
O

+ I2
HO

+ 2 HI
O

OH

- Dung dch chun: Dung dch iod 0,1 N (biu kin).

- Ch th: H tinh bt.
Khi ht vitamin C, iod gp tinh bt cho mu xanh, bo im kt thc.
Tin hnh theo cc bc:
a. Mu th: Cn m (g) acid ascorbic cho vo bnh nn, thm ch th h tinh bt;
chun bng dung dch iod 0,1 N ti xut hin mu xanh nht, bn.
Tiu th ht V ml dung dch iod 0,1 N.
b. Xc nh h s hiu chnh F ca dung dch iod 0,1 N:
V dung dch chun iod 0,1 N khng n nh nn cn xc nh h s hiu
chnh F cng thi im nh lng mu th.
Ly chnh xc 10 ml dung dch iod 0,1 N vo bnh nn, chun bng
dung dch natri thiosulfat 0,1 N vi ch th h tinh bt.
Tiu th ht V1 ml dung dch natri thiosulfat 0,1 N.
H s hiu chnh: F = V1 / 10
Hm lng H (%) acid ascorbic trong mu th tnh theo cng thc:
V . F . E . 100
H (%) =
m (g)
E: Tr s ly t 1 ml iod 0,1 N tng ng 8,806 mg acid ascorbic.
V hm lng tnh theo % nn E tnh bng n v g
E = 0,008806 g