QUY TC LM VIC TRONG PHNG TH NGHIM HA HC

I. An ton khi lm vic vi axit v kim

1. An ton khi lm vic vi axit:
- Phi lm vic trong t ht bt c khi no un nng axit hoc thc hin phn ng vi cc hi axit
t do.
- Khi pha long, lun phi cho axit vo nc tr phi c dng trc tip.
- Gi axit khng bn vo da hoc mt bng cch eo khu trang, gng tay v knh bo v mt.
Nu lm vng ln da, lp tc ra ngay bng mt lng nc ln.
- Lun phi c k nhn ca chai ng v tnh cht ca chng.
- Ly axit ng lng ghi trong ti liu, mi axit phi c mung hoc ng ht ring..
- Axit ri ra ngoi phi dn ngay, cc axit thi ng ni quy nh.
2. An ton khi lm vic vi kim
- Kim c th lm chy da, mt gy hi nghim trng cho h h hp.
- Mang gng tay cao su, khu trang khi lm vic vi dung dch kim m c.
- Thao tc trong t ht, mang mt n chng c phng nga bi v hi kim.
- Dung dch amoniac: l mt cht lng v kh amoniac rt n da, mang gng tay cao su, khu trang,
thit b bo v h thng h hp. Hi amoniac d phn ng mnh vi cht oxi ho, halogen, axit mnh.
- Kim loi Na, K, Li, Ca: phn ng cc mnh vi nc, m, CO
2
, halogen, axit mnh, dn xut clo
ca hydrocacbon. To hi n mn khi chy. Cn mang dng c bo v da mt.
- Canxioxit rt n da, phn ng cc mnh vi nc, cn bo v da mt, ng h hp do d nhim
bi oxit.
- Natri hiroxit v kali hiroxit: rt n da, ta nhit ln khi tan trong nc. Cc bin php an ton
nh trn, cho tng vin hoc t bt vo nc ch khng c lm ngc li.
- Ly kim ng lng ghi trong ti liu, mi loi kim phi c mung hoc ng ht ring..
- Kim ri ra ngoi phi dn ngay, cc kim thi ng ni quy nh.
II. Quy tc lm vic vi ha cht th nghim
1. Ho cht th nghim:
Cc ho cht dng phn tch, lm th nghim, tin hnh phn ng, ... trong phng th nghim c
gi l ha cht th nghim. Ho cht c th dng rn (Na, MgO, NaOH, KCl, (C
6
H
5
COOH) ...; lng
(H
2
SO
4
, aceton, ethanol, chloroform, ...) hoc kh (Cl
2
, NH
3
, N
2
, C
2
H
2
...) v mc tinh khit khc
nhau:
- Sch k thut (P): sch > 90%
- Sch phn tch (PA): sch < 99%
- Sch ha hc (PC): sch > 99%
2. Cch s dng v bo qun ho cht:
- Chai l ha cht phi c np. Trc khi m chai ha cht phi lau sch np, c chai, trnh bi bn
lt vo lm hng ha cht ng trong chai.
- Cc loi ha cht d b thay i ngoi nh sng cn phi c gi trong chai l mu vng hoc
nu v bo qun vo ch ti.
- Dng c dng ly ha cht phi tht sch v dng xong phi ra ngay, khng dng ln np y
v dng c ly ha cht.
- Khi lm vic vi cht d n, d chy khng c gn ni d bt la. Khi cn s dng cc ha
cht d bc hi, c mi,... phi a vo t ht, ch y kn np sau khi ly ha cht xong.
- Khng ht bng pipet khi ch cn t ha cht trong l, khng ngi hay nm th ha cht.
- Khi lm vic vi axit hay baz mnh: Bao gi cng axit hay baz vo nc khi pha long
(khng c nc vo axit hay baz); Khng ht axit hay baz bng ming m phi dng cc
dng c ring nh qu bp cao su, pipet my. Trng hp b bng vi axit hay baz ra ngay vi
nc lnh ri bi ln vt bng NaHCO
3
1% (trng hp bng axit) hoc CH
3
COOH 1% (nu bng
baz). Nu b bn vo mt, di mnh vi nc lnh hoc NaCl 1%.
Trng hp b ha cht vo ming hay d dy, nu l axit phi sc ming v ung nc lnh c
NaHCO
3
, nu l baz phi sc ming v ung nc lnh c CH
3
COOH 1%.



MT S K NNG V THAO TC C BN V CHUN
TRONG TH NGHIM THC HNH HA HC
1. Cch s dng Pipet: dng ly chnh xc th tch dung dch. Khi thao tc vi pipet trnh nm
c tay vo pipet v nhit t tay s lm thay i th tch ca cht lng trong pipet. Khi ly dung dch
bng pipet, tay cm u trn ca pipet bng ngn ci v ngn gia ca tay thun ri nhng u di
ca pipet vo dung dch (gn y bnh). Tay kia cm qu bp cao su, bp li ri a vo u trn ca
pipet ht dung dch vo pipet n khi dung dch trong pipet cao hn vch mc 2-3 cm. Dng ngn
tay tr bt nhanh u trn ca pipet li cht lng khng chy khi pipet. Dng tay khng thun
nng bnh ng dung dch ln, iu chnh nh ngn tay tr cht lng chy t t ra khi pipet cho
n khi mt cong pha di ca cht lng trng vi vch ca pipet th dng ngn tay tr bt cht u
trn ca pipet l v chuyn pipet c cha mt th tch chnh xc cht lng sang bnh chun . Khi
ly dung dch v khi cho cht lng chy khi pipet cn gi cho pipet v tr thng ng. Khi cht
lng chy xong cn chm nh pipet vo phn bnh khng c dung dch (hnh 3) nhng tuyt i
khng thi git dung dch cn li trong pipet (nu thnh pipet c ch thch l loi TD).
Khi c th tch trn pipet ch ly 02 ch s c ngha sau du phy.
2. Cch s dng Buret: Khi lm vic vi buret cn kim tra cu kha buret c m bo kn v trn,
nu cn th bi kha vi mt lp mng vaselin tng kn v trn. Kp buret vo gi buret v tr
thng ng. Trc mi ln chun cn trng buret bng chnh dung dch s ng trong buret
v phi dung dch vo buret ti vch 0 pha trn v ch lm y c phn cui v c kha buret.
Khi c th tch buret, mt phi v tr ngang mt cong pha di dung dch trong sut hoc
phn trn mt li vi dung dch khng mu v ch ly 01 ch s c ngha sau du phy. Khi tin
hnh chun phi cho dung dch chy khi buret t t tt c cht lng chy ra ht khi buret
v sau 30 giy k t khi kha dung dch mi c kt qa. Cui qu trnh chun phi nh tng
git dung dch v lm vi ln ly gi tr trung bnh. Php chun c coi l kt thc khi hiu
th tch gia cc ln chun song song khng qu 0,1 ml.


(a) np dung dch
vo buret
(b) Kim tra xem c
cn bt kh kha
van khng
(c) ra u buret
bng nc ct
(d) lm sch v kh
buret trc khi
chun


3. Cch ly dung dch chun :(ch dng nc ct trng, khng c dng dung dch cn ly
trng bnh nn). s dng pipet ly dung dch chun hoc dung dch phn tch vo bnh nn
(hnh 12).

(a) trng pipet bng
chnh dung dch
cn ly
(b) lau pha ngoi
pipet bng giy
thm
(c) pipet thng
ng v nghing
bnh nn dung
dch chy vo
(d) Tia nc ct
xung quang bnh
nn m bo tt
c th tch chnh xc
dung dch ly
c phn ng vi
cht chun
Hnh 3. Cc thao tc ly dung dch vo bnh nn bng pipet
4. pha dung dch chun t cht gc, ngi ta cn mt lng xc nh ph hp cht gc trn cn
phn tch c chnh xc 0,0001 hoc 0,00001g, ho tan nh lng lng cn trong bnh nh mc
c dung tch thch hp ri pha long bng nc ct hoc dung mi thch hp ti vch mc.
Th d: pha dung dch chun NaOH 0,0500 M (M = 40), trc tin cn tnh khi lng NaOH cn
thit pha ch c 250 ml dung dch NaOH nng 0,0500M theo cng thc:
m= 0,2500,0540 = 0,50 gam.
Cn 0,50 gam NaOH c tinh khit phn tch trong cc cn trn cn phn tch, chuyn cht rn qua
phu vo bnh nh mc 250,0 ml. Trng cc cn 3 ln bng nc ct vo bnh nh mc. Thm
khong 150ml nc ct na v lc k cho tan ht sau thm nc ct n vch mc, lc k trn
u, ta c dung dch chun NaOH 0,0500M.
5. Cch tin hnh chun :
- Tay khng thun cm kha van (hnh 13a)
- Tay thun cm bnh nn (hnh 13b)
- Chun vi tc nhanh trc im tng ng mt vi ml
- u buret chm vo bnh nn (hnh 13c)
- Tia nc ct xung quanh dung dch ca cht chun nu c bm trn thnh ca bnh nn s
c i xung (hnh 13d)
- Khi gn n im tng ng chun vi tc chm
- Du hiu kt thc chun l khi dung dch va chuyn t mu A sang mu B


(a) (b) (c) (d)
Hnh 4. Cc thao tc trong qu trnh chun

Phn 2. Mt s bi th nghim thc hnh mn ha hc
Bi 1. CHUN AXIT BAZ
I. Cc bc tin hnh th nghim
1. Cch pha dung dch chun t cht gc, ngi ta cn mt lng xc nh ph hp cht gc trn
cn phn tch c chnh xc 0,0001 hoc 0,00001g, ho tan nh lng lng cn trong bnh nh
mc c dung tch thch hp ri pha long bng nc ct hoc dung mi thch hp ti vch mc.
Th d: pha dung dch chun NaOH 0,0500 M (M = 40), trc tin cn tnh khi lng NaOH cn
thit pha ch c 250 ml dung dch NaOH nng 0,0500M theo cng thc:
m= 0,2500,0540 = 0,50 gam.
Cn 0,50 gam NaOH c tinh khit phn tch trong cc cn trn cn phn tch, chuyn cht rn qua
phu vo bnh nh mc 250,0 ml. Trng cc cn 3 ln bng nc ct vo bnh nh mc. Thm
khong 150ml nc ct na v lc k cho tan ht sau thm nc ct n vch mc, lc k trn
u, ta c dung dch chun NaOH 0,0500M.
Vic pha NaOH gp nhiu kh khn nh sau:
1/ NaOH dng rn l cht cc k d ht m, do lng NaOH thc t ko ng bng lng NaOH
bn em cn m ln t nc.
2/ Trong qu trnh bo qun NaOH trong bnh, nng NaOH cng b gim theo thi gian. Do trong
khng kh ca chng ta c kh CO
2
, l mt acid yu khi tan trong nc ---> tc dng vi NaOH to
NaHCO
3
v Na
2
CO
3
gy gim nng ca cht chun NaOH.
V vy, khi pha dung dch NaOH, ta phi lm tht nhanh v y kn bnh cha trnh CO
2
tc
dng vi NaOH gy gim nng NaOH.
2. Cch chun : Ly dung dch chun NaOH vo buret. Ly dung dch HCl cn xc nh nng
vo bnh tam gic sch (dng pipet). Thm vo
1 - 2 git cht ch th, th d phenolphtalein. Thm t t dung dch chun vo bnh (va thm va lc
trn) n khi dung dch cht ch th chuyn mu t khng mu sang mu hng nht bn trong
khong 30 giy th kt thc. c th tch dung dch chun tiu tn.
Tin hnh chun t 2 n 3 ln, ghi cc kt qu v tnh gi tr trung bnh.
II. Mt s lu th nghim thc hin thnh cng
Pha dung dch chun cn thn
Cc thao tc s dng pipet v buret phi thnh tho, nn s dng trc khi chun chnh thc
(nu kha buret b kt cn nh 1 -2 git glyxerol)
Khi cht ch th nhum mu hng, cn lc k, nu mu hng bin mt th thm cn thn tng git
nh dung dch chun ng thi lc bnh n khi mu hng khng bin mt trong 30 giy th kt thc.

Bi 2. XC NH HM LNG AXIT AXETYLSALIXYLIC
TRONG ASPIRIN BNG PHNG PHP CHUN AXIT BAZ
I. C s l thuyt
Aspirin (axit axetylsalixylic) l mt axit hu c c cha c este hu c. N c s dng rng ri
trong y hc nh mt loi thuc gim au v nh mt loi thuc gim st. N thng c iu ch
bng phn ng ca axit salixylic vi anhydrit axetic theo phn ng sau:

axit Salixylic anhydrit axetic axit axetyl salixylic axit axetic
Mt lng axit axetylsalixylic c th c xc nh bi s chun vi mt baz mnh nh Natri
hiroxit
CH
3
COO-C
6
H
4
COOH(aq) + OH
-
(aq) CH
3
COOC
6
H
4
COO
-
(aq) + H
2
O(l)
Khi x l vi mt dung dch natri hidroxit, aspirin b thy phn v hai axit sinh ra cng c trung
ha ngay.
CH
3
COOC
6
H
4
COOH + 2NaOH CH
3
COO Na + HOC
6
H
4
COONa + H
2
O
Nu dng mt lng d dung dch NaOH trong phn ng ny, th lng NaOH d c xc nh
bng php chun vi dung dch axit. Tuy nhin, iu cn thit l axit dng chun phi
khng tc dng vi natri axetat v natri salicylat (c hai cht ny u cha nhng anion baz). C
th trnh iu ny bng cch chn cht ch th l phenol (khong chuyn mu pH t 6,8 n 8,4)
hoc phenolphatalein (khong chuyn mu pH t 8,3 n 10,0).
Tuy nhin, axit axetylsalixylic cng l mt este nn d dng b thy phn khi chun vi mt baz
mnh, do trong mi trng kim n b phn hy dn n sai st trong s phn tch. Nh vy, khi
p dng phng php chun th tt c axit c mt trong dung dch s thy phn hon ton trong
NaOH d. Mt mol axit trong aspirin phn ng va vi mt mol NaOH, mt mol este trong
aspirin phn ng va vi mt mol NaOH. Nh vy s mol NaOH phn ng s gp i s mol
aspirin, sau lng NaOH tha s c chun vi dung dch axit chun. Trong th nghim ny,
axit acetylsalicylic s c chun b, tng lng acid c mt s c xc nh bng cch s dng mt
phng php chun li.
II. Cc bc tin hnh th nghim
1. Cn cc vin aspirin c lng khong 0,5 g. Ghi li s vin v khi lng. Ha tan cc vin
aspirin cn c vo 15 ml etanol trong mt bnh tam gic 250 ml.
2. Thm 20 mL dung dch NaOH 0.50 mol.L
-1
.
3. tng tc phn ng thy phn, un nng cc mu trong mt cc nc khong 15 pht.
4. Lm lnh mu n nhit phng v cn thn tt c vo mt bnh nh mc 250 mL. Ra
bnh phn ng vi ln vi nc, thm phn ra vo bnh nh mc. Lm long dung dch n vch
mc v lc k hn hp.
Ly 25 mL hn hp phn ng pha long v n vo mt bnh nn sch, thm 2- 4 git ch th
phenolphtalein vo bnh. Mu sc ca dung dch l mu hng nht. Nu dung dch khng mu th
thm 5 ml dung dch NaOH 0,50 mol. L
-1
ri lp li cc bc 3 v 4.
5. Ghi li tng khi lng dung dch NaOH 0,50 mol.L
-1
c thm vo.
6. Chun baz tha trong dung dch bng dung dch HCl 0,30 mol.L
-1
cho n khi mu hng
bin mt v dung dch tr nn c. Ghi li nng mol ca axit v cht chun thu c. Lp li s
xc nh cho n khi no kt qu gn nh khng i (sai s 0,1 ml). Tnh gi tr trung bnh.
7. Ghi li khi lng dung dch HCl 0,30 mol.L
-1
c thm vo.
8. Lp li cc bc ca s chun hai ln na bng cch s dng hai mu mi.
III. Mt s lu th nghim thc hin thnh cng

Trnh un si, bi v cc mu c th b phn hy;

Lm ngui hn hp phn ng bng cch gi bnh di vi nc ang chy;
IV. Phn tch kt qu th nghim v Bo co
1. Tnh lng axit axetylsalixylic c trong mu asppirin
Ln V
NaOH
0,5M

n
NaOH
V
HCl 0,3M
n
HCl
n
ax.axetylsalicilic
thc t

1
2
3
Trung
bnh


V d: S mol (axit axetylsalixylic) theo l thuyt=
, g
, g/ mol
1 00
180 0
= 5.55 mmol
40 ml NaOH 0,5 M cha 20 mmol
Chun 1,00 g mu vi HCl 0.30 M, thc nghim dng trung bnh 27.0 ml
27 ml HCl 0,3M cha 8,10 mmol
n(NaOH dng phn ng vi axit axetylsalixylic) = 20.0 8.10 = 11.9 mmol

1,0 mol axit axetylsalixylic phn ng vi 2,0 mol NaOH nn
S mol (axit axetylsalixylic) =
, 11 9
2
= 5.95 mmol
Bi 3. PHN TCH NH LNG AXIT ASCORBIC
TRONG VIN THUC VITAMIN C
I. C s l thuyt
Axit ascorbic va l mt axit, va l mt cht kh, do , c chun axit-baz v chun oxi ha
kh u c th s dng xc nh lng axit ascorbic trong nhng vin vitamin C thng mi.
Nguyn tc phng php
1. Phng php axit baz
Trong dung mi nc, axit ascorbic l axit phn ly hai nc vi cc gi tr pK
a
ln lt bng 4,2 v
11,6 tng ng vi s phn ly H
+
ca nhm OH nh vo C
3
v C
2
.
Axit ascorbic d dng phn ng vi cc dung dch kim to mui.
+ NaOH
HOH
2
C (CHOH)
3
C
O
COONa + H
2
O
O
HO OH
O
CH
2
OH
H
H OH

nh lng axit ascorbic c th dng phn ng chun nc 1 vi NaOH, ch th phenolphatalein.
2. Phng php oxi ha kh:
Axit L- ascorbic b oxi ha thnh axit L- dehydroascorbic theo bn phn ng oxi ha sau y ( E
0
=
0,127V pH=5)
+ 2H
+
+ 2e
-
O
HO OH
O
CH
2
OH
H
H OH
O
O
O
O
CH
2
OH
H
H OH
Axit ascorbic Axit dehidroascorbic

Axit ascorbic c xc nh da trn phn ng oxi ha n bng iot (trong KI d) theo phng php
chun trc tip vi cht ch th h tinh bt.
Bc 1: iu ch dung dch iot 5I
-
+ IO
3
-
+ 6H
+
3I
2
+ 3H
2
O
Bc 2: I
2
oxi ha axit ascorbic to axit dehidroascorbic
C
6
H
8
O
6
+ I
2
C
6
H
6
O
6
+ 2I
-
+ 2H
+

Ti im tng ng, khi ton b axit ascorbic b oxi ha, I
2
s hin din trong dung dch, phn
ng vi h tinh bt lm xut hin mu xanh. y l im dng ca chun .
II. Cc bc tin hnh th nghim
Th nghim ny gm hai phn, phn u dng chun axit-baz xc nh lng axit ascorbic
trong mt vin vitamin C. Phn th hai dng chun oxi ha kh thc hin xc nh tng t.
Chun b cc dung dch:
1. Chun b cc dung dch
a. Dung dch vitamin C cn xc nh hm lng axit ascorbic
Cn chnh xc vin vitamin C (c v), ha tan vin vitamin C trong nc, lc nu cn thit. Th
tch cui cng ca dung dch nn l 100 mL. Cn li phn b ri tr i v ghi li khi lng axit
ascorbic em TN.
b. Dung dch it:
Ha tan 5 g KI v 0,268 g KIO
3
trong 200 ml nc ct, thm 30 ml axit sunfuric 3M v chuyn vo
bnh nh mc 500 ml, nh mc n vch mc, ta c dung dch KI
3

2. Chun axit-baz
- Ht chnh xc 10ml dung dch vitamin C cn xc nh nng (dung dch a) vo bnh Erlenmeyer,
thm 2-3 git phenolphthalein.
- T buret, nh dung dch NaOH 0,1M v lc u bnh cho ti khi dung dch c mu hng bn
trong khong 30 giy th dng chun .
- Ghi s ml dung dch NaOH chun ( V
0
ml)
- Lm 3 ln ri ly kt qu trung bnh (V ml)
3. Chun oxi ha kh
3.1. S dng dung dch thiosunfat chun xc nh nng dung dch iod cho.
- Dung pipet lay chnh xac 10 ml Na
2
S
2
O
3
0,05N + 5ml em Acetat
- Chuan o dung dch thu c bang dung dch I
2
en khi xuat hien mau vang rm.
- Gn cui chun mi thm 5 git ch th h tinh bt, tip tc chun n khi dung dch xut
hin mu xanh bn trong 30 giy.
- Lp li 3 ln, ly kt qu trung bnh, t tnh nong o dung dch I
2
.
* Lu i vi chun iot bng natri thiosunfat:

1. Vai tr ca m axetat:
to mi trng c pH n nh 4-5. V
- Khng c tin hnh chun I
2
trong mi trng kim v
I
2
+ NaOH = NaIO + NaI + H
2
O
Do phn ng ph ny, kt qu phn tch s khng chnh xc.
- Cng khng tin hnh chun trong mi trng axit mnh v axit lm tng cng phn ng
oxi ha gia O
2
khng kh v I

4I

+ O
2
+ 4H
+
= 2I
2
+ 2H
2
O
2. Ch nh h tinh bt vo cui chun , khi iot ch cn li rt t v:
Nu cho ngay t u, tinh bt hp th iot rt mnh, dn n sai s. Mt khc, tinh bt c th kh
c mt vi cht c tnh oxi ha mnh.

3.2. Xc nh lng axit ascorbic.
- Dng Pipet 10 mL a dung dch a vo bnh Erlenmeyer. Thm vo vi git tinh bt lm cht ch
th v chun vi dung dch iod.
- Ghi s ml dung dch iot chun ( V
0
ml)
- Lm 3 ln ri ly kt qu trung bnh (V ml)

III. Phn tch kt qu th nghim v Bo co
S nh gi c da trn s chnh xc ca mi php chun . Tnh 30% cho chun axit-baz,
tnh 60% cho chun oxi ha kh v 10% cho s so snh hai phng php.
1 Chun axit - baz
Chun ln 1 Dung dch Vitamin C mL; Dung dch NaOH dng mL
Chun ln 2 Dung dch Vitamin C mL; Dung dch NaOH dng mL
Chun ln 3 Dung dch Vitamin C mL; Dung dch NaOH dng mL
2 Chun oxi ha kh
2-1 Xc nh nng iot
Chun ln 1 Dung dch Iod mL; Dung dch Na
2
S
2
O
3
dng mL
Chun ln 2 Dung dch Iod mL; Dung dch Na
2
S
2
O
3
dng mL
Chun ln 3 Dung dch Iod mL; Dung dch Na
2
S
2
O
3
dng mL
2-2 Xc nh axit ascorbic
Chun ln 1 Dung dch Vitamin C mL; Dung dch Iod dng mL.
Chun ln 2 Dung dch Vitamin C mL; Dung dch Iod dng mL.
Chun ln 3 Dung dch Vitamin C mL; Dung dch Iod dng mL.
IV. Cu hi kim tra v m rng
1) Gi s axit ascorbic l mt n axit, dng d liu t chun axit-baz tnh lng axit
ascorbic trong c vin vitamin C.
2) Phn ng ca I
2
vi Na
2
S
2
O
3
nh sau:
2 S
2
O
3
2-
+ I
2
S
4
O
6
2-
+ 2I
-

Tnh nng dung dch iod.
3) Phn ng ca axit ascorbic vi I
2
l:
H
2
C
6
H
6
O
6
+ I
2
C
6
H
6
O
6
+ 2 I
-
+ 2H
+

Tnh lng axit ascorbic trong c vin vitamin C
4) So snh u im v khuyt im ca hai phng php chun .
Hng dn Gii:
1.S lg axit = S lg NaOH
C
N

A
.V
A
= C
N

NaOH
. V
NaOH

= C
N

NaOH
. V
NaOH (1)


Xem axit ascorbic l n axit nn n =1
A
= M
A
= 176
Thay cc gi tr
A
, C
N

NaOH
, V
NaOH
vo (1) m
A


m
A

A

2. S lg S
2
O
3
2-
= S lg Iot
C
N Na2S2O3
.V
Na2S2O3
= C
N iot
.V
iot

3. S lg axit = S lg iot
C
N

A
.V
A
= C
N

iot
. V
iot

= C
N

iot
. V
iot (2)


Trong phn ng oxi ha-kh, axit ascorbic nhng 2e n=2
A
= 88
Thay cc gi tr
A
, C
N

iot
, V
iot
vo (2) m
A

4. a) Phng php axit baz
- u im
n gin, d tin hnh, khng yu cu nhng iu kin chun nht nh.
- Khuyt im
B qua s phn ly nc 2 ca axit ascorbic.
b) Phng php oxi ha-kh
- u im
Chun hon ton lng axit ascorbic.
- Khuyt im
Cn m bo nhiu iu kin khi tin hnh chun : nhit , nh sng, pH mi trng, ch th...

Bi 4: CHUN COMPLEXON
A-Gii thiu phng php chun complexon
-Trong chun complexon, cht to phc c s dng l axit etylendiamin tetraaxetic (cn gi l
complexon II hay EDTA), l axit 4 nc. Cng thc



K hiu thng dng l H
4
Y. Tuy nhin, EDTA t tan trong nc, do thng dng mui natri ca
n, k hiu l Na
2
H
2
Y, y l complexon III hay Trilon B (vn quen gi l EDTA).
m
A

A

I. S to phc ca complexon III vi cc ion kim loi
Phn ng to phc M
n+
+ Y
4-
MY
(n-4)+
vi hs to phc |
Phn ng to phc gia EDTA vi ion kim loi ph thuc nhiu yu t trong quan trng nht l
pH. Nguyn nhn l do pH nh hng n s to phc hiroxo ca ion kim loi v s phn li ca
thuc th. Ty theo bn ca phc cht m mi phn ng to phc xy ra mt khu vc pH ti u.
V d, Phn ng gia Fe
3+
v EDTA c th xy ra trong mi trng axit v phc FeY

rt bn, cn
phn ng gia Mg
2+
, Ca
2+
vi EDTA phi c thc hin trong mi trng baz. Mt khc, ngn
nga s to hiroxit kim loi ngi ta thng iu chnh pH hoc thm cc cht to phc ph, v
d chun ion Mg
2+
bng EDTA phi thc hin trong mi trng m (NH
3
+ NH
+
4
) khng
to kt ta Mg(OH)
2
.
II.Ch th trong chun complexon
Phc ca ch th v ion kim loi phi c bn tng i cao, nhng km bn hn phc gia ion
kim loi v thuc th EDTA.
C ch i mu ca ch th:
- Phn ng to phc mu ca ch th In v ion kim loi M + In MIn |
MIn

- Hai dng In v MIn c mu khc nhau. Khi chun bng EDTA, u tin ion kim loi M t do to
phc vi EDTA, khi n im tng ng, EDTA s tc dng vi phc MIn gia ion kim loi v
ch th, to phc MY v gii phng ch th dng In.
MIn + H
2
Y
2-
MY
4-
+ In +2H
+

Phn ng ny xy ra ti im tng ng, do MIn v In c mu khc nhau nn c th dng chun
.
B-p dng phng php complexon xc nh nng Ni
2+
trong dung dch
I. Nguyn tc:
Da trn phn ng to phc bn ca Ni
2+
vi EDTA:
Ni
2+
+ H
2
Y
2-
NiY
2-
+ 2H
+

Phn ng c tin hnh pH=8, cht ch th l murexit .
NiIn
2+
+ H
2
Y
2-
NiY
2-
+ 2H
+
+ In
(vng nht) (tm)
II.Tin hnh
- Cn chnh xc 300 mg niken sunfat v ha tan vo nc. Dng cc ong 100 mL.
- iu ch dung dch m bng cch ha tan 2,7 g ammoni clorua v 17,5 mL ammoniac m c
trong 50 mL nc.
- y dung dch EDTA tiu chun 0,01 M vo mt buret.
- Dng pipet ly 10,00 mL dung dch niken sunfat cho vo cc hnh nn 200 mL v pha long vi
khong 90 mL nc. Va thm va khuy u 10 mL dung dch m vo cc hnh nn. Thm mt t
cht ch th murexide rn v m bo tan ht. (nu cho nhiu, mu ca murexit s cn tr vic
quan st qu trnh chuyn mu ca dung dch).
- Chun vi dung dch EDTA n khi i mu t vng sang tm. Khi mu i chm, thm mt t
ammoniac m c lc cui chun . Th nghim ny cn c thc hin hai ln.
III. Phn tch kt qu th nghim v Bo co
Ghi li cc s liu sau:
1. Lng dung dch EDTA theo mL. Cng ghi li chnh xc chun ca dung dch.
2. Tnh nng Ni
2+
trong dung dch.
3. Tnh s mol nc kt tinh trong mt mol niken sunfat (trnh by cch tnh).
Hng dn gii
Cn c vo lng EDTA dng c th tnh nng ion kim loi:
C
Ni
+ 2
=
EDTA EDTA
Ni
V C (mol / l )
V
+

2

T , tnh khi lng NiSO
4
nguyn cht nc kt tinh trong tinh th.
IV. Cu hi kim tra v m rng
1) Cht ch th Eriocrom en T, phm nhum azo c tnh axit yu:
H
2
In

+ H
2
O

H
3
O
+
+ HIn
2
; K
a2
= 10
6,3

xanh
HIn
2
+ H
2
O

H
3
O
+
+ In
3
; K
a2
= 10
11,6

xanh vng da cam
Ha tan 1,25 gam mt mu NiSO
4
.nH
2
O v pha long chnh xc thnh 500 ml. Ly 50,00 ml
dung dch thu c, thm 25,00 ml Na
2
HY 0,0216 M v chun hn hp bng dung dch ZnSO
4

dng eriocrom en T lm ch th pH = 10 (m NH
3
+ NH
+
4
) ht 11,00 ml dung dch ZnSO
4
0,012
M. Tnh hm lng Ni trong mu. (P S: 19,16%)
2) Chun 50,00 ml dung dch Na
2
H
2
Y pH = 10,00 (m NH
3
+ NH
+
4
) dng Eriocrom en T lm
ch th ht 32,05 ml dung dch MgSO
4
0,045 M.
Chun 100,00 ml nc sui pH = 10,00 ht 8,40 ml EDTA lm i mu ch th Eriocrom en
T.
Mt khc, sau khi thm NaOH d vo 50,00 ml nc sui lm kt ta ion Mg
2+
di dng
Mg(OH)
2
. em lc tch kt ta v chun Ca
2+
bng EDTA dng murexit lm ch th th phi dng
ht 3,35 ml EDTA.
Tnh s mg CaO v MgO c trong 1,00 lt nc sui.
(P S: 19,75 mg MgO v 108,40 mg CaO)

BI 5. NHN BIT V TCH CC ION TRONG DUNG DCH
5.1. NHN BIT MT S ION THNG DNG C TRONG DUNG DCH HN HP BNG
MT PHN NG
I. C s l thuyt
1. Nhn bit HCO

3


Thuc th c trng cho ion HCO

3
l dung dch axit mnh (H
+
). Nu dung dch c cha HCO

3
th
khi thm axit vo s thy dung dch si bt kh.
HCO

3
+ H
+
H
2
O + CO
2
|
2. Nhn bit SO
2
4


Thuc th c trng cho anion ny l dung dch BaCl
2
trong mi trng axit long.
Ba
2+
+ SO
4
2-
BaSO
4
+
Mi trng axit d l cn thit v mt lot cc anion nh CO
3
2-
, PO
4
3-
, SO
3
2-
, HPO
4
2-
cng cho
kt ta trng vi ion Ba
2+
.
3. Nhn bit Cl


Thuc th c trng ca anion ny l dung dch bc nitrat AgNO
3
trong mi trng HNO
3
long:
Ag
+
+ Cl
-
AgCl+
4. Nhn bit Fe
2+

* Cho dung dch NaOH hoc NH
3
vo dung dch Fe
2+
th kt ta Fe(OH)
2
mu trng hi xanh s c
to thnh. Ngay sau , trong dung dch kt ta ny tip xc vi oxi khng kh v b oxi ha thnh
Fe(OH)
3
c mu nu .
4 Fe(OH)
2
+ O
2
+ 2 H
2
O 4 Fe(OH)
3

* xc nh Fe
2+
khi c mt Fe
3+
ngi ta c th s dng thuc th o-phenantrolin, phn ng to
phc mu .
Fe
2+
+ 3 o-Phen [Fe(o-Phen)
3
]
2+

Cu to ca o Phenantrolin:
N N

* xc nh Fe
2+
cng c th dng Kali ferixianua K
3
[Fe(CN)
6
],
Fe(CN)
3
6
+ Fe
2+
Fe
3
[Fe(CN)
6
]
2
+ xanh tuc bun
Thuc th khng to kt ta vi ion Fe
3+

5. Nhn bit Fe
3+

Thuc th c trng ca ion Fe
3+
l dung dch ion thioxianat SCN
-
, n to vi ion Fe
3+
ion phc
c mu mu:
Fe
3+
+ SCN
-
Fe(SCN)
2+

II. Cc bc tin hnh th nghim
Xc nh s c mt ca cc ion HCO

3
, SO
2
4
, Cl

, Fe
3+
, Fe
2+
c mt trong cng mt dung dch. Cn
chia dung dch hn hp lm 5 mu.
1. Xc nh HCO

3
(mu th nht): S dng axit HNO
3
(trnh cc ion SO
2
4
,Cl

)
Ly 2 ml dung dch phn tch cho vo ng nghim, thm vi git dung dch HNO
3
.
2. Xc nh SO
2
4
(mu th hai)
Ly 2 ml dung dch phn tch cho vo ng nghim, thm vi git dung dch Ba(NO
3
)
2
.
3. Xc nh Cl

(mu th ba)
Ly 2 ml dung dch phn tch cho vo ng nghim, thm vi git dung dch AgNO
3
.
4. Xc nh Fe
3+
(mu th t)
Ly 2 ml dung dch phn tch cho vo ng nghim, thm vi git dung dch NH
4
SCN.
5. Xc nh Fe
2+
(mu th nm)
Ly 2 ml dung dch phn tch cho vo ng nghim, thm vi git dung dch o-phenantrolin. Hoc ly
2 ml dung dch phn tch cho vo ng nghim, thm vi git dung dch Kali ferixianua K
3
[Fe(CN)
6
].
III. Mt s lu th nghim thc hin thnh cng
1. V cc ion u c mt trong cng mt dung dch nn thuc th c trng ch phn ng vi ion cn
nhn bit m khng tc dng vi cc ion cn li trong dung dch. C th s dng th t nhn bit cc
ion hoc chia dung dch thnh nhiu mu, trnh a thm ion cn nhn vo dung dch;
2. S dng cng t ht ly dung dch, khi nh git khng cc git dung dch ri trn thnh
ng nghim;
3. Nu hin tng xy ra chm, c th lc nh ng nghim;
4. d quan st nn t ng nghim trn nn giy trng
5. Khi nhn ion Fe
2+
, phi tin hnh phn ng pH < 7, phi trnh s c mt cc cht oxi ha
c th oxi ha Fe
2+
thnh Fe
3+
v cc cht kh Fe(CN)
3
6
thnh Fe(CN)
4
6
.
5.2. TCH V NHN BIT MT S ION THNG DNG THUC CC NHM PHN
TCH KHC NHAU C TRONG DUNG DCH HN HP
I. C s l thuyt
1. Nhn bit Pb
2+

Thuc th c trng cho ion Pb
2+
l dung dch KI. Khi thm KI vo dung dch c cha Pb
2+
s thy
xut hin kt ta mu vng.
Pb
2+
+ 2 I
-
PbI
2
+
Kt ta ny tan ra khi un nng ng nghim, kt ta xut hin tr li thnh tinh th ng nh vng khi
ngui.
2. Nhn bit Cu
2+

* Thuc th c trng cho ion ny l dung dch amoniac hoc kh H
2
S.
Cu
2+
+ 4 NH
3
[Cu(NH
3
)
4
]
2+
xanh thm
Cu
2+
+ H
2
S CuS+ en
3. Nhn bit Ag
+

Thuc th c trng ca ion ny l dung dch axit clohidric.
Ag
+
+ Cl
-
AgCl+
4. Nhn bit Al
3+

Cho dung dch NaOH vo dung dch Al
3+
th kt ta Al(OH)
3
mu trng s c to thnh. Khi thm
lng d NaOH kt ta s tan dn cho n khi thu c dung dch trong sut.
Al
3+
+ 3 OH
-
Al(OH)
3
+
Al(OH)
3
+ OH
-
[Al(OH)
4
-
]
II. Cc bc tin hnh th nghim
Xc nh s c mt ca cc ion Pb
2+
, Ag
+
, Cu
2+
, Al
3+
c mt trong cng mt dung dch.
Ly 5 ml dung dch phn tch cho vo ng nghim, thm vi git dung dch HCl kt ta hon ton.
Cho ng nghim vo my ly tm tch ring kt ta (A) v phn dung dch (B).
1. Xc nh Ag
+
v Pb
2+

Ly phn kt ta (A) cho vo ng nghim cha 5 ml nc ct ri un nng, chuyn phn dung dch
trong sang mt ng nghim khc cha 2 ml dung dch KI. Phn cht rn khng tan c cho vo ng
nghim c cha 2 ml dung dch NH
3
c ri khuy u bng a thy tinh. Quan st hin tng v
rt ra kt lun.
2. Xc nh Cu
2+
v Al
3+

Sc kh H
2
S ti d vo phn dung dch B. Thm tip dung dch NaOH ti d. Quan st hin tng v
a ra kt lun.
BI 6. PHN NG OXI HA KH
Th nghim 1: iu ch oxi trong phng th nghim
I. Cc bc tin hnh ca th nghim thc hnh
I.1 iu ch oxi t hn hp KClO
3
v MnO
2

Trn 5,0g KClO
3
nghin nh vi khong 1,25g MnO
2
(t l 4:1) ri cho hn hp vo mt ng
nghim kh.
Lp ng nghim cha ho cht ln gi st nh hnh v. Lp nt c cm ng dn kh vo ng
nghim ng ha cht. Th kn ca thit b bng cch ly mt t nc cho vo ng dn kh. Sau
khi nt vo ng nghim nu mc nc trong ng dn kh thp hn ming ng dn kh th thit b
kn, sau a ng dn kh vo bnh thu kh.






Hnh 5. iu ch t KClO
3
v thu oxi bng cch y nc
Chun b l thy tinh, chu nc thu kh oxi bng phng php y nc hoc y khng kh.
Chm n cn, h nng u ho cht trong ng nghim sau un tp trung ti ch c cha nhiu
ho cht.
Thu y l kh O
2
, y kn l. Tip tc thu l kh O
2
khc.
KClO
3

+MnO
2
O
2
I.2 iu ch t KMnO
4

Ly khong 2,0 g KMnO
4
vo mt ng nghim kh. Lp ng nghim ln gi st, sao cho ming
ng nghim hi thp hn y ng nghim. Thm mt lp bng vo bn trong ming ng nghim,
ri lp nt c cm ng dn kh. Th kn ca thit b bng cch p dng nguyn l bnh thng
nhau nh trn.
Chm n cn, h nng u ho cht trong ng nghim sau un tp trung ti ch c cha nhiu
ho cht.
Sau khi nung mt thi gian, c bt kh sinh ra. Nhng bt kh u tin c ln kh nit nn khng
thu ngay.
Thu y l kh O
2
, y kn l. Tip tc thu l kh O
2
khc.







Hnh 6. iu ch t KMnO
4
v thu oxi bng cch y nc
I.3. iu ch t H
2
O
2
Lp dng c nh hnh di y.






Hnh 7. iu ch t H
2
O
2
v thu oxi bng cch y nc
Cho mt lng H
2
O
2
vo phu brom, cho 0,5 gam MnO
2
vo bnh thy tinh c
nt cao su. M t t kho phu brom cho dd H
2
O
2
chy xung, tip xc vi cht xc tc MnO
2
;
kh O
2
c thu vo l thu kh bng phng php y nc.
MnO2
H2O2
KMnO
4
O
2
Lp bng

Mi hc sinh chun b t nht 4 l c nt nhm thu kh oxi chun b cho cc th nghim v tnh
cht ca oxi.
II. Mt s lu th nghim thc hin thnh cng
Khi lp ng nghim cha ho cht ln gi st cn ch : ming ng nghim hi chc xung
phng hn hp cht rn m, khi un hi nc bay ln s khng chy ngc li lm v ng nghim.
Lu KClO
3
l mt cht gy n nn khng nghin nhiu mt lc, khng nghin ln vi bt k
mt cht no khc. L ng KClO
3
khng c h nt nht l khi cnh cc cht P, C, S.
trnh hin tng cc ht tinh th KMnO
4
b kh O
2
y vo ng dn nn mt lp bng
ming ng nghim, gn ng dn kh.
Khi ngng thu kh phi tho ri ng dn kh ra trc khi tt n cn.
Khng thu kh t nhng bt kh u tin, v cn ln nit trong khng kh.
Khi thu kh oxi, gi li mt lp nc mng trong l kh oxi.
Th nghim 2. Oxi tc dng vi kim loi v phi kim
I. Cc bc tin hnh th nghim
I.1. Oxi tc dng vi st
Thu kh oxi vo l thu tinh (ly t th nghim 1), y
l c mt lp nc mng hoc mt lp ct mng.
Ly si dy Fe (thp) nh, tt nht l dy phanh xe p
di 30cm cun trn thnh l xo. Cm mt u cun
dy vo thanh g nh, u kia cun dy kp cht khong
1/3 que dim . t chy phn que dim ri t t a vo
l cha oxi.
Quan st hin tng (nh sng, mu sc, u dy Fe,
thnh l thy tinh); nhn xt.




I.2. Oxi tc dng vi Natri
Thu kh oxi vo l thu tinh (ly t th nghim 1)
Ct 1 mu Na bng ht ng nh, ct b ht lp
oxit quanh, dng giy lc thm kh du.
Cho mu Na vo mung t ha cht xuyn qua
ming ba cc tng. Sau un nng trn n cn
cho n khi Na nng chy hon ton c mu sng





Hnh 9. Oxi tc dng vi Na


Hnh 8. Oxi tc dng vi Fe
H
2
O
mu dim
O
2

dy st


Ct
Na
O2

Ba cc tng
Hnh 5. Oxi tc dng vi Na
ng nh ri a vo l cha oxi. Quan st.
I.3. Oxi tc dng vi Lu hunh
t nng mt u a thu tinh ri cho chm vo
mt lng nh bt S, bt S nng chy bm ngay vo
u a thy tinh.
a a thu tinh dnh S vo ngn la, S chy
ngay u a thu tinh. Quan st hin tng S







Hnh 10. Oxi tc dng vi lu
hunh

chy trong khng kh, sau a nhanh u a ang chy vo l cha oxi. Quan st hin tng lu
hunh chy trong kh oxi.
II. Mt s lu th nghim thc hin thnh cng
1. Tt nht l nn dng 01 si dy thp tch t dy phanh xe p. Trong l thy tinh cha oxi c mt
lp nc mng hoc mt lp ct mng.
Phn ng chy ca Fe xy ra nhit cao, do phi gn mt mu dim u l xo cung
cp nhit lc u cho phn ng.
Nu dy thp g phi nh sch trc khi t.
2. Nn cho vo l cha O
2
mt lp ct mng.
a mung t xung su 2/3 l; khng chm vo thnh l; khi rt mung t ra y ngay
l bng nt.
Na d cn c x l bng cch ngm trong etanol hoc trc khi ra mung t ly mt t giy
cun thnh hnh phu, t mung t vo gia phu nhng vo chu nc Na cn d s phn ng
ht.
3. Khng nn a thy tinh nng chm vo thnh l thy tinh.
C th thay l cha oxi bng ng nghim cha oxi.
Tuyt i khng dng a thu tinh ang nng chm vo c chu bt lu hunh.
Trong l nn cho trc mt lp nc mng th sn phm.
Bi 7. TC PHN NG CN BNG HO HC


S

O2
Hnh 6. Oxi tc dng vi Lu hunh
Th nghim 1. Cc yu t nh hng n tc phn ng
I. Cc bc tin hnh th nghim
I.1. nh hng ca nng n tc phn ng
Chun b 2 cc: Cc 1 ng 25ml dung dch Na
2
S
2
O
3
0,1M, cc 2 ng 10ml dung dch Na
2
S
2
O
3

0,1M.
Lm th nghim theo trnh t sau:
Thm 15ml nc ct vo cc 2 pha long dung dch.
25ml dung dch H
2
SO
4
0,1M vo cc 1, lc nh. Dng ng h bm giy xc nh thi gian
t lc dung dch H
2
SO
4
vo n lc kt ta xut hin.
25ml dung dch H
2
SO
4
0,1M vo cc 2, lc nh. Dng ng h xc nh thi gian xut hin
kt ta.
So snh thi gian xut hin kt ta 2 cc.
I.2. nh hng ca nhit n tc phn ng
25ml dung dch H
2
SO
4
0,1M vo cc 1 ng 25ml dung dch Na
2
S
2
O
3
0,1M nhit thng.
Dng ng h xc nh thi gian t lc 2 dung dch vo nhau n lc bt u c kt ta xut
hin.
Cng ly 2 dung dch nh trn vo cc 2 nhng em un nng c 2 dung dch n khong 50
60
0
C ri mi vo nhau. Dng ng h xc nh thi gian xut hin kt ta. So snh vi thi gian
trng hp khng un nng.
I.3. nh hng ca b mt cht rn n tc phn ng
Cn 2 mu vi (CaCO
3
) c khi lng bng nhau: mt mu c kch thc ht ln hn v mt
mu c kch thc ht nh.
Dng pipet ht 2 th tch bng nhau ca dung dch HCl 4M vo 2 ng nghim.
Cho 2 mu vi chun b vo 2 ng nghim trn. Cho mu ht vo ng 1, cho mu bt vo ng
2. Quan st hin tng.
Dng ng h xc nh thi gian v so snh thi gian CaCO
3
ca hai mu phn ng ht.
II. Mt s lu th nghim thc hin thnh cng
Ly dung dch ng th tch, cn thn khi s dng pipet
Cn in t khng di qut gi
Bm ng h kp thi, ng thi im
Khi un nng dung dch, cn quan st nhit k
Ghi chp thi gian kp thi.
Th nghim 2. nh hng ca nhit n cn bng ho hc
I. Cc bc tin hnh th nghim
Lp mt dng c gm hai ng nghim c
nhnh (a) v (b), c ni vi nhau bng
mt ng nha mm, c kho K m (hnh
11).
Np y kh NO
2
vo c hai ng (a) v (b)
nhit thng. Nt kn c hai ng, mu
ca hn hp kh trong cn bng c hai ng
(a) v (b) l nh nhau.

ng kho K li ngn khng cho kh hai ng khuch tn vo nhau. Ngm ng (a) vo nc . Mt
lt sau ly ra so snh mu ng (a) vi ng (b).
II. Mt s lu th nghim thc hin thnh cng
Cn thn khi iu ch NO
2
v np vo hai ng nghim (a) v (b). Kh NO
2
c nn cn ch n
cnh bo nguy him v gi an ton khi th nghim.
S dng nt cao su va kht vi ming ng nghim v kim tra nt tht cht sau khi np kh.
Kim tra k kha thy tinh v ng dn cao su sao cho tht kn.
C th thay chu nc bng cch s dng n cn un nh ng (b).
Bi 8. NGHIN CU TNH CHT HA HC CA ANDEHIT-XETON,
AXIT CACBOXYLIC
Th nghim 1: Phn ng oxi ha fomandehit bng thuc th
I. Cc bc tin hnh th nghim
I.1. Vi thuc th Tollens
Ra sch ng nghim bng cch cho vo ng nghim 2ml dung dch NaOH 10% un si, b
dung dch kim v trng ra vi ln bng nc sch.
Cho vo ng nghim sch 1ml dung dch AgNO
3
3%, cho tip 1ml dung dch NaOH 10%, xut hin
kt ta, cho tip dung dch NH
3
5% vo hn hp phn ng cho ti khi kt ta mi to thnh tan
ht. Tip tc cho vo hn hp phn ng mt vi git kim NaOH 10%. Rt khong 1ml dung dch
fomanlin 40% vo hn hp phn ng. Ch rt nh theo thnh ng nghim. un nh hn hp vi

Hnh 11. Th nghim nhn bit s chuyn
dch cn bng ca phn ng
2NO
2
(k) N
2
O
4
(k)


pht trn n cn

(khng cho hn hp phn ng si), duy tr nhit 35
o
C trong thi gian 2,0 -
3,0 pht. Quan st th nghim.
I.2. Vi thuc th Fehling:
Cch pha thuc th Fehling: ha tan 0,4 gam CuSO
4
.5H
2
O trong 10ml nc ct (nu dung dch
c th cn lc) c dung dch A. Ha tan 0,2 gam C
4
H
4
O
6
NaK.4H
2
O v 1,5 gam NaOH trong
10ml nc ct c dung dch B. Thuc th Fehling (ch pha ngay trc khi s dng hn
ch s to thnh kt ta Cu(OH)
2
): trn 1 th tch dung dch A v 1 th tch dung dch B, lc
u, thu c dung dch thuc th Fehling trong, xanh bic.
S dng thuc th Fehling lm th nghim tng t thuc th Tollens.
I.3. Vi thuc th Benedict:
Cch pha thuc th Benedict: ha tan 17,3g natri citrat trong 70ml nc ct un si, thm 10g
Na
2
CO
3
khan, lm lnh, thm t t 10ml dung dch CuSO
4
17,3%, thm nc n 100ml, dung
dch benedict c mu xanh dng.
S dng thuc th benedict lm th nghim tng t thuc th Tollens.
II. Mt s lu th nghim thc hin thnh cng
Nu ng nghim khng c ra tht sch th kt ta Ag sinh ra nhanh, khng to ra gng m
to mt mng en. Khi un nng hn hp phn ng khng nn lc ng nghim m yn cho lp
Ag to ra t t mi thu c gng p.
Th nghim xong, ra ng nghim bng dung dch HNO
3
long, cc cht vo cc thu hi sn
phm.
C th thay vic un nng nh hn hp bng cch t ng nghim vo ni cch thy ang si hoc
ngm ng nghim trong cc nc si.
Cn cho d kim do phn ng oxi ha andehit xy ra trong mi trng kim

Th nghim 2: Tnh cht ha hc c trng ca axeton
I. Cc bc tin hnh th nghim
I.1. Phn ng iodofom ca axeton
Cho vo ng nghim sch 10 ml axeton, th vo ng nghim 2,0 gam Iot, lc u cho
ti khi Iot bt u tan trong axeton. Sau thm t t tng git dung dch 10% NaOH v
tip tc lc ng nghim trn ln cc cht, ri gi ng nghim nhit
phng 20 pht.
Nu vn khng c g xy ra, lm nng ng nghim nh cc th nghim
ng n-c nng, duy tr nhit 35
o
C trong thi gian 5 pht. Quan st
hin tng.
I.2. Phn ng ca axeton vi 2,4- initro phenylhirazine (DNPH)
iu ch thuc th 2,4-initrophenylhyrazin bng cch ho tan 3,0 gam 2,4-initro phenylhyrazin
vo 15 ml axit sunfuric c v thm vo dung dch ny 20 ml nc vi 70 ml etanol 95%, trong iu
kin khuy trn tt hn hp.
Ho tan 100 mg axeton trong 2 ml etanol 95%, ri 2 ml thuc th 2,4-initro phenylhyrazin vo
dung dch ny. Lc mnh hn hp.
II. Mt s lu th nghim thc hin thnh cng
Cn s dng ng th t cc ha cht phn ng
Trong c hai th nghim phi lc u tay v duy tr nhit cn thit

Nu kt ta khng xut hin ngay, th yn dung dch 15 pht

Th nghim 3: Phn ng este ha
I. Cc bc tin hnh th nghim
Rt vo ng nghim 2,5 ml C
2
H
5
OH 96
0
, rt tip vo 2,5ml axit axetic, cho thm vo hn hp phn
ng 1ml H
2
SO
4
m c, lc nh hn hp phn ng cho cc cht trn u vo nhau; thm vo hn
hp phn ng vi vin bt. [y ng nghim bng nt cao su c cm ng dn kh hnh thc th,
a u ng dn kh vo ng nghim c cha sn ng nghim nc lnh, u ng dn kh gn st
ti y ca ng nghim ng nc, ton b ng nghim ny c ngm trong cc ng nc . ]
[ngng t este thnh dng lng]
un nng ton b hn hp phn ng. Ch un ui t y ng nghim ln pha ming ng nghim
este sinh ra bay sang ng nghim thu sn phm c nhng trong cc nc lnh; este thu c c
mi thm c trng.
II. Mt s lu th nghim thc hin thnh cng
Khi ngng th nghim, tho nt ng dn kh, tt n cn, b ng dn kh khi ng thu sn phm.
Th sn phm bng cch: Ly ngn tay ci bt ming ng nghim cha etylaxetat, dc ngc ng,
etylaxetat tip xc vi ngn tay khong pht, h m ngn tay nc phun ra thnh tia.
Bi 9. TNH CHT CA MT S CHT HU C
Th nghim 2: Phn ng ca glucoz vi thuc th Tolen, Felinh, Benedict v nc brom
I. Cc bc tin hnh th nghim
I.1. Nhn bit glucoz bng thuc th Tollens
Ra sch ng nghim bng cch cho vo ng nghim 2ml dung dch NaOH 10% un si, b dung
dch kim v trng ra vi ln bng nc sch.
Cho 1ml dung dch AgNO
3
3% vo ng nghim sch s 1, cho tip 1ml dung dch NaOH 10%, kt
ta xut hin, cho tip dung dch NH
3
5% vo hn hp phn ng cho ti khi kt ta mi to
thnh tan ht. Tip tc cho vo hn hp phn ng mt vi git kim NaOH 10%. Rt thm 2ml
dung dch glucoz 1% vo hn hp phn ng. Ch rt nh theo thnh ng nghim. un nng hn
hp vi pht trong ni nc nng 60
o
C - 70
o
C

(khng cho hn hp phn ng si). Quan st th
nghim.
I.2. Nhn bit glucoz bng thuc th Fehling hoc thuc th Benedict
Pha thuc th Fehling v thuc th Benedict nh hng dn Bi 4 th nghim 1 trang 69.
Cho 2ml dung dch glucoz 1% vo ng nghim, thm tip 1ml thuc th Fehling (hoc thuc th
Benedict). Lc u ng nghim, un n khi bt u si, quan st hin tng.
Ch : Phn ng vi thuc th Benedict rt c trng v nhy vi ng kh hn phn ng
vi thuc th Fehling
I.3. Nhn bit glucoz bng dung dch nc brom
Rt 2ml dung dch brom vo ng nghim sch s 3, thm tip vi git dung dch glucoz 1%, lc
mnh ng nghim. Quan st hin tng.
II. Mt s lu th nghim thc hin thnh cng
Nu ng nghim khng c ra tht sch th kt ta Ag sinh ra nhanh, khng to ra gng m to
mt mng en. Khi un nng hn hp phn ng khng nn lc ng nghim m yn cho lp Ag to
ra t t mi thu c gng p.
Phn ng vi thuc th Benedict rt nhy, ch cn s dng glucose 0,1% l to kt ta
Cu
2
O gch, tuy nhin kt ta ln vi dung dch mu xanh dng nn dung dch chuyn sang
mu xanh m.
+ Nu s dng glucose 1% th lng kt ta sinh ra ln, s nhn thy r kt ta Cu
2
O (ln vi mu
xanh ca dung dch nn khng thy mu gch m chuyn sang nu, gn nh en).
Th nghim xong, ra ng nghim bng dung dch HNO
3
long, cc cht vo cc thu hi sn
phm.
Th nghim 3: S thy phn ca tinh bt
I. Cc bc tin hnh th nghim
Cch pha ch dung dch h tinh bt: Ly 3 gam tinh bt cho vo cc thy tinh 200ml, thm tip
khong 100ml nc si, khuy u, thu c dung dch h tinh bt.
Cho vo ng nghim khong 3ml dung dch h tinh bt, thm tip khong 4ml nc v 1ml dung
dch H
2
SO
4
(1:5). un si hn hp phn ng t 3-5 pht, khi un cn dng a thy tinh khuy u
hn hp phn ng. Sau khi un khong 3 pht, ly khong 0,5ml dung dch phn ng cho vo ng
nghim khc, ngui, nh vi git dung dch I
2
(pha trong cn). Nu dung dch chuyn mu xanh c
ngha l h tinh bt cha thy phn ht. Tip tc un hn hp phn ng cho n khi ly dung dch
trong ng nghim ang thy phn, em th vi dung dch I
2
(pha trong cn) khng c mu xanh.
Tinh bt b thy phn ht.
hn hp phn ng trong ng nghim ngui, trung ha axit d trong dung dch h tinh bt n
mi trng kim d (th bng qu tm). Chia hn hp phn ng thnh 2 phn vo 2 ng nghim
th sn phm.
ng nghim 1 th phn ng vi thuc th Tollens. Quan st hin tng
ng nghim 2 th phn ng vi thuc th Fehling hoc Benedict. Quan st hin tng
II. Mt s lu th nghim thc hin thnh cng
Mun cho th nghim thnh cng cn phi un si k, khuy u hn hp phn ng.
Phi trung ha axit H
2
SO
4
d trong hn hp phn ng n mi trng kim d.
Th nghim 4: Mt s phn ng mu ca amino axit v protein
I. Cc bc tin hnh th nghim
I.1. Cho vo ng nghim s 1 khong 2ml dung dch Glyxin (H
2
NCH
2
COOH), thm vo
khong mt vi git thuc th Ninhyrin. Quan st s xut hin ca mu sc.
I.2. Cho vo ng nghim s 2 khong 2ml dung dch protein (lng trng trng), thm vo khong
1ml dung dch NaOH 30% v thm tip vi git CuSO
4
5% (thuc th biure). Lc u hn hp phn
ng. Quan st mu sc ca dung dch v gii thch.
I.3. Cho vo ng nghim s 3 khong 1ml dung dch protein (lng trng trng), sau thm vo ng
nghim 0,5ml HNO
3
c (d= 1,4g/ml). Lc u hn hp phn ng. Quan st mu sc ca dung dch
v gii thch.
Bi 10. iu ch axit benzoic bng PHN NG OXY HA toluen vi KMnO
4
nng.
I. Nguyn tc
Khi oxy ha toluene bng KMnO
4
trong nc ta thu c axit benzoic dng mui kali benzoat
tan trong nc v mangan dioxit khng tan.
C
6
H
5
-CH
3
+ 2KMnO
4
C
6
H
5
-COOK + 2 MnO
2
+ + KOH + H
2
O
Khi kt thc phn ng, loi KMnO
4
d bng ancol etylic hoc axit oxalic, lc loi b mangan
dioxit. Bc hi dch lc, thm t t axit clohydric c n phn ng axit s thu c axit
benzoic dng kt tinh.
C
6
H
5
-COOK + HCl C
6
H
5
-COOH+ + HCl
Lc, ra ta bng nc lnh. Ly kt ta v sy kh ngoi khng kh. (Axit benzoic c th tinh ch
bng phng php thng hoa).
II. Cc bc tin hnh th nghim
Cho 1,0 gam toluen, 75 ml nc ct v vi vin bt (hoc mnh s) vo bnh cu y trn
dung tch 150 ml. Lp ng sinh hn hi lu v un hn hp cch li aming si nh. Trong khi
lc u, cho t t tng phn ca 3,4 gam KMnO
4
vo bnh (qua ng sinh hn) trong khong 1,0
gi. Sau khi cho ht KMnO
4
, dng vi ml nc rt qua ng sinh hn ha tan ht nhng tinh
th KMnO
4
bm trong rut ng.
Tip tc un nng v lc lin tc khong 4,0 gi na.
Lm lnh hn hp, lc b MnO
2
trn phu thy tinh (c th lc trn phu Buchner loi ht MnO
2
)
ly dung dch trong. Ra kt ta MnO
2
bng 10 ml nc nng (ra nh vy 2 ln)
Gp phn dung dch ra v phn nc lc vo cc thy tinh, un trn bp in (qua li amiang)
hoc trn ni cch ct cho n khi th tch dung dch cn khong 10 15 ml. Lc ln na trn phu
thy tinh loi ht MnO
2
v cng ra kt ta bng 10 ml nc nng. Tip tc c dung dch cho
n khi t th tch 7 10 ml. ngui dch lc ri axit ha bng axit HCl long (1: 1) cho n
phn ng axit theo giy Cngg. Axit benzoic tch ra di dng kt ta trng. Lc ht qua phu
Buchner s thu c axit benzoic, ra kt ta bng mt lng nh nc lnh, lm kh trong khng
kh. Hiu sut : 1 gam (khong 80% so vi l thuyt), nng chy 122
0
C.

Lu :
- Toluen c, tc dng ln h thn kinh nn trong khi un khng toluen bay ra ngoi, hoc rt
vo da.
- Trc khi axit ha dung dch lc, cn m bo khng cn vn c ca MnO
2
(lc b tip) v
mu hng ca KMnO
4
(loi bng ancol etylic hoc axit oxalic).

Giai on 2- iu ch etylbenzoat bng PHN NG ESTE HA
I. Cc bc tin hnh th nghim
Cho 2 ml ancol etylic vo bnh Vuyc dung dch 150ml, nh t t 1,5 ml H
2
SO
4
c vo ancol trong
bnh, ng thi lc u. y bnh bng nt c lp phu nh git. Lp ng sinh hn rut thng vo
nhnh bnh cu, ui ng sinh hn c ng ni cong dn vo bnh hng. Rt vo phu chit hn hp
gm 30 ml ancol etylic v 4,9 gam axit benzoic, lc nh. un bnh phn ng trn bp cch ct n
nhit 140
o
C ri nh t t hn hp ancol v axit benzoic xung bnh vi tc bng tc cht
lng chy sang bnh hng. Trong sut thi gian phn ng lun gi nhit 140
o
C.
Sau khong mt gi ri phn ng kt thc, chuyn cht lng bnh hng vo phu chit, lc cht
lng vi dung dch Na
2
CO
3
cho n khi t mi trng trung tnh hoc kim yu, kim tra bng giy
qu. Tho b lp nc di. Lc lp este ( trn) vi dung dch CaCl
2
bo ha loi ancol d.
Tch ly lp este trn, lm kh bng CaCl
2
khan hoc Na
2
SO
4
khan. Chng ct trong bnh Vuyc
trn ni nc si, thu este etyl benzoat nhit 70
o
C. Nhn bit etylbenzoat bng quan st l cht
lng khng mu, trong sut, c mi thm ca qu chn
Ch : Etyl benzoat c th to hn hp ng ph nh sau:
- Hn hp 91,8% ester vi 8,2% nc si 70,4
0
C.
- Hn hp 69,2% ester vi 30,8% alcol ethylic si 71,8
0
C.
- Hn hp 83,2% ester, 9% alcol ethylic v 7,8% nc si 70,3
0
C.
II. Phn tch kt qu th nghim v Bo co
chuyn dch cn bng theo chiu thun thng dng mt s bin php sau:
+ Dng d mt trong hai cht phn ng, trong th nghim ny ta dng d cht no? V sao? Vit
phng trnh ha hc cho phn ng.
+ Gim nng cht to thnh, este etyl benzoat c nhit si 213
o
C cao hn cc este bo n
chc. Trong th nghim chng ct theo kiu no ly c este?
Mc ch lc cht lng sau phn ng vi dung dch Na
2
CO
3
cho n khi t mi trng trung tnh
hoc kim yu lm g?
Khi lc lp este vi dung dch CaCl
2
bo ha xy ra qu trnh g loi ancol cn d?
III. Cu hi kim tra v m rng
1) Trnh by nguyn tc ca phn ng iu ch etylbenzoat?
2) Hy trnh by cc bin php nng cao hiu sut ca phn ng este ha c ng dng trong qu trnh
iu ch etylbenzoat?
3) Trnh by cch loi sn phm ph, tinh ch etylbenzoat t hn hp phn ng.
4) So snh phn ng este ha to etyl benzoat vi phn ng este ha to etyl axetat?