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TRNG AI HOC A LAT

F7G

Hng dan thc hanh

PHAN TCH NH LNG


BANG CAC PHNG PHAP
HOA HOC

NGUYEN TH NH MAI - ANG TH VNH HOA


2002

HDTH Phan tch nh lng bang cac phng phap hoa hoc

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LI NOI AU
Giao trnh hng dan thc hanh PHAN TCH NH LNG bang cac
phng phap hoa hoc c soan ra nham muc ch giup cac ban sinh vien
hieu va nam chac cac kien thc ly thuyet va ky nang thc hanh cua mon
hoa phan tch 2.
Hoa hoc von c xem la khoa hoc thc nghiem; muon nam vng va
phat trien cac kien thc hoa hoc can phai tien hanh th nghiem; muon
hoan thanh tot cac th nghiem hoa hoc can nam vng cac ky nang thc
hanh, nhng ky nang nay c ren luyen tng bc va ni ren luyen cac
ky nang o chu yeu la phong th nghiem. Do o giao trnh nay c bien
soan vi 8 bai thc hanh va cac c s ly thuyet c ban ve cac phng
phap hoa hoc cua phan tch nh lng, giup sinh vien cung co phan ly
thuyet c ban cua moi bai thc tap ket hp vi viec van dung quy tac
ng lng trong tnh toan ket qua. Cac bai th nghiem a c la chon
va sap xep nham giup sinh vien ren luyen cac thao tac va ky nang th
nghiem vi mc o phc tap tang dan, nh vay sinh vien se co ieu kien
at c yeu cau mon hoc thc hanh nay.
Xin cam n cac ong nghiep va ban oc a khuyen khch ong vien
chung toi bien soan giao trnh. Chan thanh mong ban oc gop y kien xay
dng cho giao trnh hoan thien hn.
Cac tac gia

Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

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NOI QUY PHONG TH NGHIEM


e am bao an toan va ket qua lam viec trong phong th nghiem moi sinh vien
can phai thc hien nghiem tuc noi quy phong th nghiem.
1. Sinh vien co nhiem vu lam ay u cac bai th nghiem theo chng trnh cua bo
mon. Trc khi vao lam th nghiem phai chuan b ay u e cng bai th
nghiem theo yeu cau cua giao vien.
2. Phai en phong th nghiem ung gi quy nh. Trong gi lam th nghiem, sinh
vien muon ra ngoai phong th nghiem phai xin phep giao vien. ng ung cho
th nghiem quy nh. Kiem tra ngay cac dung cu, neu thieu hoac hong th bao
ngay cho giao vien.
3. Trong khi lam th nghiem phai gi yen lang, trat t.
4. Phai gi sach se trong phong th nghiem. Ban lam viec, dung cu, hoa chat dung
cho th nghiem phai sach se va sap xep mot cach hp ly cho cong viec.
5. Nghe va thc hien ung cac ch dan cu the cua giao vien ve bai thc hanh
6. 6 . Can tiet kiem hoa chat th nghiem, lu y tranh gay o v dung cu hoa chat.
Khi o v dung cu, phai bao ngay cho giao vien hng dan.
7. Khong c di chuyen hoa chat dung chung t cho nay sang cho khac. Khong
c mang hoa chat dung cu ra khoi phong th nghiem. Khong lam cac th
nghiem ngoai bai th nghiem.
8. Phai can than khi lam th nghiem. Trung thc va khach quan khi theo doi ket
qua va khi lam bao cao th nghiem.
9. Chu y ren luyen ky nang thc hanh phan tch nh lng: o chnh xac khoi
lng va the tch, cach nhan biet ung iem cuoi chuan o, cach bao quan dung
dch chuan, ky thuat loc ra, say nung ket tua..., ren luyen ky nang tnh toan
trong phan tch nh lng.
10. Sau moi buoi th nghiem phai ra sach dung cu, lau ban, don dep ngan nap
cho lam viec va ban giao ay u lai cho nhan vien phu trach phong th nghiem.

Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

-4-

Phan th 1. GII THIEU VE PHAN TCH NH LNG


Phan tch nh lng tc la xac nh ham lng cua cac chat can phan tch. e
lam c viec o co the co nhieu phng phap khac nhau, tuy theo yeu cau can
phan tch (o nhay, o chnh xac) va trang thiet b hien co ma ngi lam phan
tch co the la chon cac phng phap khac nhau e tien hanh phan tch. Ngay nay
ket qua thu c ch co gia tr khi a c x ly bang phng phap thong ke. V
the sau khi thu c ket qua phan tch, ngi phan tch can phai biet x ly cac so
lieu thu c e a ra ket qua phan tch chnh xac.
I. PHAN LOAI CAC PHNG PHAP PHAN TCH NH LNG:

e phan tch nh lng co nhieu phng phap thng c s dung, o la:


1. Phng phap hoa hoc:
La dung 1 phan ng hoa hoc (tc la s dung 1 thuoc th R nao o cho phan ng
vi chat can xac nh X) e chuyen cau t can xac nh thanh 1 hp chat mi, roi
da vao the tch va nong o cua thuoc th R, hoac khoi lng cua hp chat mi
tao thanh ta tnh c ham lng cua chat X.
a. Phng phap phan tch khoi lng:
Lam ket tua chat can xac nh di dang 1 hp chat xac nh, lam sach ket
tua va em nung en khoi lng khong oi roi can. Da vao lng can e tnh
ham lng chat can xac nh.
b. Phng phap the tch:
Da vao the tch va nong o cua dung dch thuoc th R a phan ng vi 1
the tch xac nh chat can xac nh e tnh ham lng chat can xac nh.
Thuoc ve phng phap the tch co 4 phng phap chuan o chnh:
- Phng phap trung hoa
- Phng phap chuan o phc chat
- Phng phap oxi hoa kh
- Phng phap tao tua.
Phng phap hoa hoc ch ap dung e phan tch nhng mau co nong o ln
(10-3 - 10-1 M). Phng phap nay khong oi hoi nhng may moc hien ai nen de
ap dung.
2. Phng phap vat ly:
Dung cach khao sat tnh chat ly hoc ac trng nao o e xac nh ham lng
cua chat can xac nh. V du: o khoi lng rieng, chiet suat hoac da vao s
tng tac cua vat chat vi bc xa ien t

Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

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3. Phng phap hoa ly:


Da vao tnh chat vat ly (mau sac, o dan ien) cua hp chat hay dung dch
tao ra sau khi co phan ng hoa hoc gia chat can xac nh X va thuoc th R e
xac nh ham lng cua chat can xac nh.
Trong pham vi tai lieu hng dan thc hanh nay, ch gii thieu cac phng
phap phan tch hoa hoc.
II. CACH TNH KET QUA TRONG PHAN TCH THE TCH:

Viec tnh ket qua phu thuoc vao cach bieu dien nong o va cach phan tch.
Cach tnh n gian nhat la da vao nh ngha nong o va qui luat ng lng e
lap cong thc tnh.
Qui luat ng lng: trong mot phan ng hoa hoc so ng lng hoac so
mili ng lng cua cac chat tham gia phan ng phai bang nhau.
So ng lng = CN.V(lt) = so gam/
So mili ng lng = CN.V(ml) = so mg/
1. Trng hp chuan o trc tiep:
Gia s e chuan V0ml dung dch chat X phai dung het VRml dung dch thuoc
th R co nong o ng lng CN,R. Th nong o ng lng cua chat X c tnh
da vao quy luat ng lng: V0CN,X = VRCN,R
T ay suy ra:

C N ,X =

VR C N ,R
V0

Con so gam cua chat X trong V0ml dung dch se la:

m =
X

VR .C N ,R . X
1000

Trong o X la ng lng gam cua chat X


Neu lay a gam mau chat X hoa tan thanh Vml dung dch, sau o lay V0ml dung
dch nay em chuan o chat X th het VR ml dung dch thuoc th R co nong o
ng lng CN,R . Th so gam cua chat X trong Vml dung dch cung chnh la so
gam cua chat X trong a gam mau la:

mX =

VR .C N ,R . V
.
1000
V0

Vay ham lng phan tram cua chat X trong mau:

Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

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Lu y: neu nong o bieu dien theo nong o phan t th phai chuyen sang nong
o ng lng roi tnh.
2. Trng hp chuan o ngc:
Them mot the tch chnh xac va d VRml dung dch thuoc th R co nong o CN,R
vao V0ml dung dch chat can xac nh X. Sau khi X tac dung het vi thuoc th R,

X% =

VR .C N ,R . V 100
. .
1000
V0 a

chuan lng R d bang mot thuoc th R thch hp co nong o CN,R th ton VRml.
Th nong o ng lng cua chat X c tnh t bieu thc cua nh luat ng
lng:
CN,RVR = CN,X V0 + CN,R' VR
T bieu thc nay suy ra CN,X va t o tnh so gam cua X trong V0 dung dch la:

m =
X

C N ,R VR C N ,R ' VR '
1000

Neu lay a gam mau em hoa tan thanh Vml dung dch roi lay V0ml dung dch
tien hanh chuan o ngc nh tren th ham lng % cua chat X trong a gam mau
la:

X% =

C N ,R VR C N ,R ' VR '
1000

X .

V 100
.
V0 a

Neu trng hp chuan o theo kieu khac hai kieu a neu tren th tuy theo ieu
kien cu the e tnh toan.
III. CACH IEU CHE DUNG DCH CHUAN

1. ieu che dung dch chuan t chat goc:


Dung dch chuan la dung dch co nong o chnh xac xac nh. Cach thong
thng e ieu che cac dung dch chuan la dung cac chat goc va cac ong chuan
Chat goc la chat dung e ieu che cac dung dch chuan. Mot chat c goi la
chat goc phai thoa man cac yeu cau di ay:
- Chat phai tinh khiet phan tch hoac tinh khiet hoa hoc.
- Thanh phan hoa hoc phai ng vi 1 cong thc xac nh ke ca nc ket tinh.
- Chat goc va dung dch chuan phai ben.
- Khoi lng phan t (nguyen t) cang ln cang tot
Khi dung chat goc e ieu che dung dch chuan: th can tnh lng can chat goc
can phai can e khi pha thanh Vml dung dch ta c dung dch co nong o CN.
Lng can (a gam) nay c tnh t bieu thc:

C =
N

a
.V

neu V tnh bang ml th : C =

Nguyen Th Nh Mai ang Th Vnh Hoa

a.1000
.V

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

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2. Neu khong co chat goc th trc het can phai chuan b dung dch co nong o
gan ung, sau o dung chat goc hoac dung dch thch hp e xac nh lai nong
o.
3. Mot so cac dung dch chuan chang han cac loai acid c chuan b t cac ong
chuan.

Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

-8-

Phan th 2. GII THIEU CAC BAI THC TAP


Bai 1. CACH S DUNG CAC DUNG CU O KHOI LNG VA THE TCH
Trong phan tch nh lng hoa hoc du thc hien theo phng phap nao cung
phai tien hanh cac phep o c ban la o khoi lng va o the tch.
I. o khoi lng:

1. Cac loai can chnh xac


Can la dung cu c ban e o khoi lng.
Can c vao cau truc cua can ngi ta phan loai thanh can hai a va can mot
a.
Can c lng can toi a cho phep ngi ta phan loai thanh can ky thuat va can
phan tch. Ca hai loai nay eu c xep vao loai can chnh xac v khi lng can
khong qua nho th co the o khoi lng vi 4 ch so co ngha.
Bang di ay so sanh tnh nang cua mot so loai can chnh thng dung trong
phong phan tch nh lng:
Tnh nang ky thuat
Lng can toi a

Can ky thuat

Can phan tch

< 1000g

Lng can toi thieu e co 4


ch so co ngha

> 10g

Gia tr mot vach chia tren


thang trac v

0,1g/vach

o lech chuan ( )

+0,02g

macro

micro

< 200g

<20g

> 0,1g

1mg/vach
+0,2g

> 0,1g
0.01mg/vac
h
+0,02mg

Cac tnh nang ky thuat co the thay oi va bo sung them tuy theo cac hang san
xuat can. Cac can chnh xac nhat la can phan tch a qua nhieu giai oan cai tien
va nay a hoan thien: can nhanh chong, tien li vi o chnh xac ngay cang
cao.Ve c ban, hoat ong cua can da tren nguyen tac cua canh tay on loai mot,
ngha la iem ta nam gia cac iem tac dung cua lc va khoang cach t iem ta
en cac iem tac dung cua lc la bang nhau.
Gia thiet muon xac nh khoi lng M1 cua vat can ta at no len a trai va at
qua can len a phai cho ti khi kim P v tr thang bang (kim tr ve trang thai ban
au). Khoi lng qua can la M2. Theo quy tac momen lc ta co:
F1.l1 = F2.l2
M1.g1.l1 = M2. g2.l2
ay, F1, F2 la cac lc tac dung len vat can va qua can;
g1, g2 la cac gia toc trong lc tng ng.
Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

-9-

Tai mot a iem xac nh th g1 = g2 = g va neu cac na canh tay on cua can
bang nhau l1 = l2 th M1 = M2. Nh vay, khi can ta a o khoi lng la ai lng
thuoc tnh cua vat the, khong phu thuoc a iem khi can.
l1

M1

l2

F1

M2
F2

S o tac dung cua lc len can


2. Cac quy tac s dung can chnh xac (theo hng dan cua can bo phong th
nghiem).
Mot so quy tac can chu y khi s dung can phan tch:
a. Phai at can trong phong rieng, cach ly hi hoa chat an mon cac bo phan cua
can. Khong at can gan cac loai nguon nhiet (tu say, lo nung...) va tranh
khong cho tia mat tri roi thang vao can. Ban ke can phai chac chan.
b. Trc khi can phai kiem tra o thang bang cua mat can theo giot nc cua
chiec ni-vo gan tren san can
c. Khi xem can thay co nhng sai lech g hoac trong khi lam viec thay co
nhng sai lech g phai bao cao vi hng dan vien, tuyet oi khong c t
y sa can.
d. Khong at hoa chat trc tiep len a can ma phai ng trong chen can hoac
mat knh ong ho. Hoa chat long de bay hi hoac hoa chat ran de thang hoa
(v du I2) th phai ay chen can.
e. Vat can phai cung nhiet o vi can e tranh s dan n khong eu cua on
can.
f. Khong can vat co khoi lng vt lng can toi a
g. Luon gi sach se, kho, nhat la a can va san can. c phep dung choi long
mem e quet a can.
II. o the tch

Phep o chnh xac the tch cua cac dung dch c thc hien nh cac loai bnh
o trong suot bang thuy tinh va co o khac.

Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 10 -

1. Phan loai cac bnh o the tch


e o the tch gan ung (vi hai ch so co ngha) ngi ta dung ong ong ( xi
lanh) vi cac c khac nhau: 2, 5, 10, 25, 50, 100, 250, 500, 1000, 2000 ml.
e o the tch chnh xac (vi 3 hay 4 ch so co ngha) ngi ta dung buret,
pipet, bnh nh mc. Cac bnh o nay khi xuat xng eu co ghi the tch chnh xac
200C kem theo o lech chuan ( ) cho phep.
Bnh nh mc: dung e pha loang chat tan en mot the tch chnh xac.
Pipet: dung e lay ra mot the tch chnh xac cua dung dch. Chia lam hai loai:
khong co va co thang chia o.
- Loai pipet khong co thang chia o, co mot hoac hai vach mc tuy loai, co
bau phnh ra oan gia nen con goi la pipet bau. Loai nay dung e lay ra mot
c the tch chnh xac (v du 10 ml, 2 ml), thng dung cac pipet bau sau
ay:100, 50, 25, 10, 2 ml.
* Neu pipet ch co mot vach mc tren cung th ta tha cho chat long chay
t do, cuoi cung cham au mut vao thanh bnh thi gian khoang 4-5 giay,
khong thoi giot chat long con sot lai gan au mut.
* Neu pipet co hai vach mc tren va di th ta cho cham au mut vao
thanh bnh va ch lay the tch gia hai vach mc nay.
Can dung qua bop cao su khi lay dung dch vao pipet e tranh oc hai.
-Loai pipet co thang chia o, hnh tru, dung e lay ra the tch chnh xac trong
pham vi mot c the tch, co thang chia o giong nh buret.
Buret: Dung e o the tch dung dch tieu hao trong qua trnh chuan o. Buret
la ong thuy tinh hnh tru, ay thot lai au mut giong nh pipet, co thang chia
o nhng co khoa au mut nay.
Phep o the tch tren buret (hoac buret co thang chia o): neu the tch u
ln, co the cho so o vi bon ch so co ngha. V du: 18.25 ml (ch so 5 c
lng bang mat). Neu the tch s dung nho hn th ch cho c ba hoac hai ch
so co ngha. V du 3,16 ml; 0,38 ml, v vay e o the tch co o chnh xac cao ta
thng pha loang dung dch chuan R the nao e noi chung the tch s dung vt
qua mc na the tch cua c buret hoac t ra cung ln hn 1/3 c nay. Thng
dung cac buret sau ay:
-Loai 50 ml moi vach chia ng vi 0,1 ml va ch cho phep c lng bang
mat cac gia tr the tch chenh lech nhau 0,03 ml. o lech chuan cho phep la
0,050 ml.
-Loai 25 ml, moi vach chia ng vi 0,1 ml nhng khoang cach gia cac vach
chia u ln e c lng bang mat va cac gia tr chenh lech nhau 0,02 ml. o
lech chuan cho phep la 0,030 ml.
-Loai 10 ml, moi vach chia ng vi 0,02 ml va co the c lng bang mat
cac gia tr chenh lech nhau 0,006 ml. o lech chuan cho phep la 0,010 ml.
Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 11 -

Khi oc the tch tren buret can chu y:


-e tam mat ngang hang vi mat phang tiep xuc ay vien lom cua chat long
neu la chat long khong mau, con neu la chat long co mau th e tam mat ngang
vi mat phang i qua vien ranh gii gia chat long va thanh bnh (theo hng
dan cua can bo phong th nghiem ).
-Nen co phng tien phu tr e oc buret (theo hng dan cua can bo phong
th nghiem ).
-Can i 30 giay sau khi ket thuc chuan o mi oc ket qua chuan o e
chat long bam thanh kp chay ti mat chat long.
2. Kiem tra the tch cua pipet, buret, bnh nh mc
Cac dung cu o the tch dung dch thng lam bang thuy tinh, nen the tch ghi
tren cac dung cu ch ung nhiet o a ghi tren dung cu. Neu o nhiet o khac
nhiet o ghi tren dung cu th the tch dung dch o c se sai khac mot t. Khi o
ta phai tien hanh hieu chnh lai the tch cua dung cu o trong ieu kien th nghiem.
Cach kiem tra va hieu chnh cac dung cu o the tch:
- e kiem tra the tch cua buret, ta ra sach buret, o vao o nc cat hai lan
en vach khong. Chuan b mot coc can sach, kho, co nap ay va can trc khoi
lng tren can phan tch co o chnh xac 0,0001 gam. Lay t buret vao coc can
5 ml nc cat. ay nap coc can va can. Khoi lng cua 5 ml nc cat la hieu so
khoi lng cua hai lan can (khong co nc va co nc). Ghi khoi lng cua 5
ml au. Sau o lai lam ay nc trong buret en vach 0, lai lay vao coc can 10
ml nc t buret va xac nh khoi lng nh lan trc. Bang cach tng t tiep
tuc can 15, 20, 25 v.v... en 50 ml nc chay ra t buret. o nhiet o cua nc.
Dung bang tra khoi lng rieng cua nc nhiet o o, t cac so lieu o ta se
tnh c the tch chnh xac bang cach lay khoi lng nc a can chia cho khoi
lng rieng cua no. V du vi 5ml au 150C can c 5,052g, nhiet o o
khoi lng rieng cua nc la 0,9979 th so hieu chnh la:
Vhc =

Vthat - Vghi = (5,052 : 0,9979) - 5,00 = +0,063 ml

Bang cach tnh toan tng t ta xac nh c Vhc oi vi cac khoang the
tch cua buret. Ve ng bieu dien s phu thuoc cua Vhc (ghi tren truc tung) vao
the tch dung dch tren buret (ghi tren truc hoanh). ng bieu dien o c goi
la ng hieu chnh. Dung ng hieu chnh o co the xac nh c he so
hieu chnh oi vi nhng the tch bat ky nhan c khi dung buret o e chuan
o.
- Dung tch cua pipet cung c kiem tra tng t nh khi kiem tra buret: lay
nc vao pipet en vach mc. o nhiet o cua nc. Sau o o nc trong
pipet vao coc can a say kho va biet chnh xac trong lng, ay nap coc can
va em can tren can phan tch. Hieu so gia trong lng cua coc can co nc
va trong lng cua coc can la trong lng cua nc trong pipet nhiet o a

Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 12 -

o. Da theo bang ty trong cua nc nhiet o o ta suy ra c the tch cua


nc tc la the tch that cua pipet nhiet o ang dung .
- Dung tch cua bnh nh mc cung c hieu chnh tng t nh cach hieu
chnh pipet.
3. Ra va trang bnh o
Cac bnh o can c ra sach cac vet chat beo. Sau khi ra bang nc may ta
ra bang nc xa bong hoac xo a (Na2CO3 ky thuat), trang lai bang nc cat.
Bang cach o, trong ai a so trng hp, bnh o a coi la ra sach. Neu thay
van con co chat beo th co the x ly tiep bang mot trong cac dung dch sau:
- Dung dch manganat mau xanh (5g KMnO4 hoa tan trong 100ml NaOH
10% un nong).
- Dung dch sulfo chromic (15g K2Cr2O7 ky thuat hoa tan trong 100 ml nc
nong ng trong coc chu nhiet. e nguoi roi them t t 100 ml H2SO4 ac _
Dung dch co mau nau tham).
Lu y: cac dung dch nay co the dung lai nhieu lan, co tac dung tay ra manh
va e lau se an mon thuy tinh. V vay ch can o vao dung dch nay, roi trang ra
ngay bang nc cat.
Dau hieu bnh o sach: khi o nc cat vao, thay mc nc dang len eu an,
con khi thao nc ra th tren thanh bnh khong con sot lai mot giot chat long nao
bam l lng ngay thanh bnh.
Lu y:
- Bnh nh mc trc khi dung ch c trang bang nc cat khong c
trang bang dung dch se nap vao.
- Ngc lai buret, pipet phai c trang bang chnh dung dch se nap vao.
III. Thc hanh:

- Sinh vien nghe hng dan cua can bo phong th nghiem, thc hanh phep can
tren can ky thuat va can phan tch cua phong th nghiem va cach s dung, oc the
tch dung dch tren buret, pipet.
- Bang thc nghiem, moi sinh vien tnh the tch cua mot giot dung dch chay ra
khoi buret theo hng dan cua can bo phong th nghiem.

Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 13 -

Bai 2. PHNG PHAP TRUNG HOA


(PHNG PHAP CHUAN O ACID BAZ)
I. Tom tat ly thuyet:

Nguyen tac cua phng phap la da vao cac phan ng trung hoa e xac nh
nong o cua acid, cua baz hay cua cac muoi co tnh acid hoac baz ro ret. Cac phan
ng dung trong phng phap nay eu thoa man cac yeu cau oi vi cac phan ng
dung trong phan tch the tch nhng can lu y cac dung dch chuan phai la nhng
acid hay baz manh e phan ng trung hoa co tnh nh lng cao va cac acid hay
baz can c chuan o khong c qua yeu.
Do acid va baz eu la nhng dung dch khong mau nen e xac nh iem ket
thuc qua trnh chuan o ta phai dung nhng chat co mau thay oi tai iem hoac
gan sat iem tng ng Nhng chat nay goi la chat ch th acid-baz (hoac chat
ch th pH)
Chat ch th acid-baz:
Chat ch th acid-baz thng la nhng acid (HInd ) hoac baz (IndOH) hu c,
thuoc loai pham nhuom. Mau sac cua chat ch th thay oi tuy thuoc vao pH cua
dung dch. Cac chat ch th oi mau trong nhng khoang pH khac nhau, t gia tr
thap en cao, do o ta co the chon cho tng trng hp chat ch th nao co vung
oi mau gan iem tng ng nhat.
Viec chon ung chat ch th e xac nh iem tng ng la ieu kien quan
trong nhat quyet nh o chnh xac cua phep chuan o. e xac nh iem tng
ng vi sai so nho hn 0,1% ta co the dung tat ca cac ch th co khoang pH oi
mau trong bc nhay va co pT cang gan iem tng ng cang chnh xac.
* Ch th n:
Di ay la mot so loai chat ch th acid-baz n thong dung:
Chat ch th

Khoang pH
oi mau

pT

Mau
Acid

Baz

Metyl da cam 0,1% trong nc

3,1 - 4,4

4,0

Vang

Metyl o 0.2% trong ru

4,4 - 6,2

5.5

Vang

Phenolphtalein 0.1% trong ru

8,0 - 9,9

9,0

Khong mau

Tm hong

pT cua chat ch th la ga tr pH ma o chat ch th oi mau ro nhat trong vung


pH chuyen mau.
* Ch th hon hp
Thng gom 2 ch th pH tron lan vi nhau hoac 1 chat la ch th pH con chat
kia la chat mau tr (co mau nhat nh khong thay oi theo pH )
Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 14 -

Ch th hon hp co khoang pH oi mau rat nho va mau dang acid va mau dang
baz rat tng phan. V vay khi chuan o dung ch th hon hp thng cho ket qua
chnh xac hn.
Di ay la mot so loai chat ch th hon hp thong dung:
STT

Thanh phan ch th

Khoang pH oi
mau

pT

B. Indigo carmin 0,25% trong nc

3,9 - 4,3

4,1

Ty le the tch A : B = 1: 1

Tm - luc

A. Metyl da cam 0,1% trong nc


1

A. Metyl da cam 0,2% trong nc


2

B. Brom cresol cham 0,1% trong nc co them 2,9ml


4,1 - 4,5
NaOH 0,05N cho moi 0,1g
Vang - luc cham
Ty le the tch A : B = 1: 1

4,3

A. Metyl o 0,2% trong ru


3

B. Brom cresol cham 0,1% trong ru


Ty le the tch A : B = 1: 3

4,9 - 5,3

5,1

o nho - luc

A. Metyl o 0,2% trong ru


4

B. Metylen cham 0,1% trong ru


Ty le the tch A : B = 1: 1

5,2 - 5,6

5,4

o nho - luc

A. Brom cresol cham 0,1% trong nc co them 2,9ml


NaOH 0,05N cho moi 0,1g
5

B. Clorophenol o 0,1% trong nc co them 4,7ml


NaOH 0,05N cho moi 0,1g
Ty le the tch A : B = 1: 1

5,9 - 6,3

6,1

Luc vang - tm
cham

A. Brom cresol o ta 0,1% trong nc co them 3,7ml


NaOH 0,05N cho moi 0,1g
6

B. Bromthymol cham 0,1% trong nc co them 3,2ml


6,5 - 6,9
6,7
NaOH 0,05N cho moi 0,1g
Vang - Tm cham
Ty le the tch A : B = 1: 1
A. o trung tnh 0,1% trong ru

B.Bromthymolcham 0,1% trong ru


Ty le the tch A : B = 1: 1

7,0 - 7,4

7,2

Hong - luc

A. Bromthymol cham 0,1% trong nc co them 3,2ml


NaOH 0,05N cho moi 0,1g
8

B. Phenol o 0,1% trong nc co them 5,7ml NaOH


0,05N cho moi 0,1g
Ty le the tch A : B = 1: 1

Nguyen Th Nh Mai ang Th Vnh Hoa

7,3 - 7,7
Vang - Tm

Khoa Hoa hoc

7,5

HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 15 -

A. Cresol o 0,1% trong nc co them 5,3ml NaOH


0,05N cho moi 0,1g
9

B. Thymol cham 0,1% trong nc co them 4,3ml NaOH


0,05N cho moi 0,1g
Ty le the tch A : B = 1: 1

8,1 - 8,5

8,3

Vang - Tm

A. Phenolphtalein 0,1% trong ru


10 B.Thymolphtalein 0,1% trong ru
Ty le the tch A : B = 1: 1
A. Thymolphtalein 0,1% trong ru
11 B. Alizarin vang 0,1% trong ru

9,4 - 9,8

9,6

khong mau - tm
10,0 - 10,4
Vang - Tm

10,2

Ty le the tch A : B = 2: 1
II. Thc hanh:

1. Xac nh nong o NaOH :


a. Nguyen tac :
Da tren c s cua phan ng :
H2C2O4 + 2NaOH = Na2C2O4 + 2H2O
Dung phenolphtalein lam ch th .
b. Cach tien hanh :
Dung pipet lay 10 ml dung dch H2C2O4 0,1N vao bnh non 250 ml. Them 2 giot
chat ch th phenolphtalein 0,1%. T buret nho tng giot dung dch NaOH can xac
nh, lac eu cho ti khi dung dch xuat hien mau hong ben khoang 5 giay. Ghi so
ml dung dch NaOH tieu ton (lam 3 lan, lay ket qua trung bnh).
2. Xac nh nong o HCl :
a. Nguyen tac :
Da tren c s phan ng :
HCl + NaOH = NaCl + H2O
Dung phenolphtalein hoac metyl da cam lam ch th.
b. Cach tien hanh :
Dung pipet lay 10 ml dung dch HCl can xac nh vao bnh non 250 ml. Them
2 - 3 giot chat ch th phenolphtalein 0,1%, t buret nho tng giot dung dch NaOH
xuong , lac eu ti khi dung dch co mau hong ben khoang 5 giay. Ghi so ml dung
dch NaOH tieu ton (lam 3 lan, lay ket qua trung bnh).
Cung tien hanh nh th nghiem tren nhng thay ch th phenolphtalein 0,1%
bang ch th metyl da cam 0,1%, va so sanh cac ket qua phan tch (khi dung metyl
da cam lam ch th dung dch chuyen t mau o sang mau da cam).

Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 16 -

3. Xac nh nong o CH3COOH :


a. Nguyen tac :
Da tren c s cua phan ng:
CH3COOH + NaOH = CH3COONa + H2O
Dung phenolphtalein lam chat ch th.
b. Cach tien hanh :
Dung pipet lay 10 ml dung dch CH3COOH can xac nh vao bnh non 250 ml,
them 2 giot chat ch th phenolphtalein 0,1%. T buret nho tng giot dung dch
NaOH xuong ti khi dung dch co mau hong ben khoang 5 giay. Ghi so ml dung
dch NaOH tieu ton (lam 3 lan, lay ket qua trung bnh).
4. Xac nh nong o H3PO4 :
a. Nguyen tac:
Da tren c s cua phan ng:
Nac I

H3PO4 + NaOH = NaH2PO4 + H2O

Nac II
phenolphtalein

NaH2PO4

NaOH

Na2HPO4

ch th metyl da cam
+

H2O

ch th

b. Cach tien hanh:


Dung pipet lay 10ml dung dch H3PO4 can xac nh vao bnh non 250 ml, them
2 giot chat ch th metyl da cam 0,1%. T buret nho tng giot dung dch NaOH
xuong ti khi dung dch chuyen mau o sang vang cam. Ghi so ml dung dch
NaOH a dung. Them 2 - 3 giot chat ch th phenolphtalein 0,1% va tiep tuc nho
dung dch NaOH xuong ti khi dung dch chuyen t mau vang sang da cam. Ghi so
ml dung dch NaOH a dung (lam 3 lan, lay ket qua trung bnh).
Ngoai ra con co the xac nh nong o H3PO4 bang dung dch NaOH dung ch
th hon hp nh sau:
i .Nguyen tac:
Chuan mot the tch chnh xac dung dch H3PO4 en nac I (tao thanh
NaH2PO4) hay chuan o lien en nac II (tao thanh Na2HPO4).
Phan ng chuan o:
en nac I

H3PO4 +

NaOH

NaH2PO4

H2O

Luon en nac II

H3PO4 + 2 NaOH =

Na2HPO4

2H2O

ii . Cach tien hanh:


- Dung pipet lay 10 ml dung dch H3PO4 cho vao bnh tam giac 250 ml , them
1 giot ch th hon hp co pT = 5,1. T buret cho dung dch NaOH xuong t t
cho en khi dung dch chuyen mau t o sang xanh luc (lam 3 lan, lay ket qua
trung bnh)
Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 17 -

- Dung pipet lay 10 ml dung dch H3PO4 cho vao bnh non 250 ml, them 2
giot ch th co pT = 10,2. T buret cho dung dch NaOH xuong ti khi dung dch
chuyen t vang sang tm. ( lam 3 lan , lay ket qua trung bnh)
5. Xac nh nong o NH4OH :
a. Nguyen tac :
Da tren c s cua phan ng :
NH4OH + HCl = NH4Cl + H2O
Dung metyl da cam; metyl o lam ch th .
b. Cach tien hanh :
Dung pipet lay 10 ml dung dch NH4OH loang can xac nh vao bnh non 250
ml, them 2 giot metyl da cam 0,1%. T buret nho tng giot dung dch HCl a biet
nong o xuong ti khi dung dch chuyen t mau vang sang da cam. Ghi so ml
dung dch HCl a dung (lam 3 lan, lay ket qua trung bnh).
Lam th nghiem tng t vi ch th metyl o 0,1%.
So sanh, nhan xet ket qua phan tch.
6. Phan tch mau: Xac nh so gam CH3COOH trong mot lt giam (theo hng
dan cua phong th nghiem).
III. Cau hoi:

1. Phan biet iem cuoi, iem tng ng.


2. Trnh bay cach pha 1l dung dch H2C2O4 t tinh the H2C2O4.2H2O.
3. Tai sao khi ieu che va bao quan dung dch NaOH lai phai tranh s hap phu kh
CO2 t khong kh ?
4. Ve dang ng chuan o dung dch HCl 0,1N bang dung dch NaOH 0,1N va
ng chuan o dung dch NaOH 0,1N bang dung dch HCl 0,1N. T ng
chuan o hay chon cac chat ch th thch hp e sai so cua phep chuan o di
0,1%.
5. Hay tnh bc nhay pH va iem tng ng tren ng cong chuan o dung
dch NH4OH 0,1N bang dung dch HCl 0,1N. Nhng chat ch th nao trong so cac
chat thng dung thch hp cho phep chuan o nay ?
Biet pK NH4OH = 4,75
6. Tnh nong o ng lng cua cac dung dch a chuan o trong bai thc tap.
7. Hay tnh bc nhay pH va iem tng ng tren ng cong chuan o dung
dch CH3COOH 0,1N bang dung dch NaOH 0,1N. Nhng chat ch th nao trong so
cac chat thng dung thch hp cho phep chuan o nay ?
Biet pKCH3COOH = 4,76
8. Xac nh so gam CH3COOH trong mot lt giam cua phong th nghiem.

Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 18 -

Bai 3. PHNG PHAP TRUNG HOA


I. Thc hanh

1. Xac nh chnh xac nong o dung dch HCl 0,1N theo chat goc :
a. Nguyen tac :
Pha dung dch Na2B4O7 t tinh the borax Na2B4O7.10H2O (chat goc) co nong o
chnh xac 0,1N. Hut ra 1 the tch xac nh cho vao bnh tam giac roi chuan o bang
dung dch HCl.
B

Phan ng chuan o :
B4O72- + 5H2O = 2H2BO3- + 2H3BO3
2H2BO3- + 2H+ = 2H3BO3
B4O72- + 5H2O + 2H+ = 4H3BO3
b. Cach tien hanh :
Dung pipet lay 10ml dung dch borat cho vao bnh non 250 ml, them 2 giot ch
th metyl o 0,1%. T buret nho tng giot dung dch HCl en khi dung dch chuyen
t mau vang sang hong da cam. Ghi so ml dung dch HCl a dung (lam 3 lan, lay
ket qua trung bnh).
2. Xac nh nong o Na2CO3 trong dung dch NaOH :
Xut ky thuat luon luon cha mot lng Na2CO3 do NaOH hap thu kh CO2 trong
khong kh.
a. Nguyen tac :
Dung HCl a biet nong o, xac nh Na2CO3 vi 2 chat ch th : phenolphtalein
va metyl da cam .
* Khi phenolphtalein oi mau :
NaOH + HCl = NaCl + H2O
Na2CO3 + HCl = NaHCO3 + NaCl
* Khi metyl da cam oi mau :
NaHCO3 + HCl = NaCl + CO2 + H2O
b. Cach tien hanh :
Dung pipet lay 10 ml dung dch hon hp Na2CO3 - NaOH vao bnh non 250 ml,
them 2 giot chat ch th phenolphtalein 0,1%, dung dch co mau hong. T buret nho
tng giot dung dch HCl lac eu ti khi dung dch mat mau. Ghi so ml dung dch
HCl tieu ton, them 2 giot chat ch th metyl da cam 0,1% dung dch co mau vang.
Tiep tuc nho dung dch HCl xuong en khi dung dch chuyen t mau vang sang da
cam . Ghi so ml dung dch HCl a dung (lam 3 lan, lay ket qua trung bnh).

Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 19 -

Ngoai ra con co the xac nh nong o Na2CO3 trong dung dch NaOH dung ch
th hon hp nh sau:
*) Nguyen tac :
Chuan o mot the tch chnh xac cua dung dch hon hp nay bang dung dch
chuan vi ch th co pT = 8,3 va pT = 4.
Khi dung ch th co pT = 8,3 xay ra phan ng chuan o sau:
NaOH

Na2CO3 +

HCl
HCl

NaCl

NaHCO3 +

H2O
NaCl

Khi dung ch th co pT = 4 (metyl da cam) xay ra phan ng chuan o sau:


NaOH

Na2CO3 +

HCl
HCl

NaCl

H2O

NaCl

+ CO2

H2O

*) Cach tien hanh:


Dung pipet lay 10 ml dung dch can xac nh vao bnh non 250 ml, them mot
giot ch th hon hp co pT = 8,3. Chuan o bang dung dch HCl en khi dung dch
chuyen mau t tm sang vang. (Lam 3 lan, lay ket qua trung bnh).
Dung pipet lay 10 ml dung dch can xac nh vao bnh non 250 ml, them1 giot
ch th metyl da cam. Chuan o bang dung dch HCl en khi dung dch chuyen
mau t vang sang da cam. (Lam 3 lan, lay ket qua trung bnh).
3. Xac nh nong o dung dch NaHCO3 , dung dch Na2CO3 trong hon hp:
a. Nguyen tac :
Tng t nh phan nh lng NaOH lan Na2CO3, trng hp nay khi ch th
phenolphtalein chuyen mau, ta nh lng c mot na Na2CO3:
Na2CO3 + HCl

NaHCO3 + NaCl

sau o, vi ch th metyl da cam, ta nh lng c na phan Na2CO3 con lai


va tat ca phan NaHCO3 co luc au:
NaHCO3 + HCl =

NaCl

H2O

CO2

b. Cach tien hanh:


Giong nh nh lng NaOH co lan Na2CO3.
Ngoai ra con co the xac nh nong o cua NaHCO3, cua Na2CO3 trong hon
hp dung ch th hon hp tng t bai th nghiem 1.2 tren.
4. Xac nh nong o dung dch HCl va H3PO4 trong hon hp :
a. Nguyen tac :
Dung NaOH a biet nong o xac nh HCl va H3PO4 vi 2 chat ch th metyl da
cam va phenolphtalein .
Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 20 -

* Khi metyl da cam oi mau :


HCl + NaOH = NaCl + H2O
H3PO4 + NaOH = NaH2PO4 + H2O
* Khi phenolphtalein oi mau :
NaH2PO4 + NaOH =
b. Cach tien hanh :

Na2HPO4 + H2O

Dung pipet lay 10 ml hon hp HCl + H3PO4 can xac nh vao bnh non 250 ml,
them 2 giot chat ch th metyl da cam 0,1%, dung dch co mau o. T buret, nho
tng giot dung dch NaOH, lac eu ti khi dung dch chuyen t mau o sang mau
vang cam. Ghi so ml dung dch NaOH a dung, them 2 giot chat ch th
phenolphtalein 0,1% va tiep tuc nho NaOH xuong ti khi dung dch chuyen mau t
vang sang da cam. Ghi so ml dung dch NaOH a dung (lam 3 lan roi lay ket qua
trung bnh).
Co the xac nh nong o dung dch HCl va H3PO4 trong hon hp dung ch
th hon hp tng t bai th nghiem xac nh nong o dung dch H3PO4 dung ch
th hon hp.
5. Xac nh nong o H2SO4 va H3PO4 trong hon hp
a. Nguyen tac:
Chuan o mot the tch chnh xac cua hon hp acid bang dung dch NaOH vi
ch th co pT = 5,1 va pT = 10,2.
* Khi dung ch th pT = 5,1 xay ra phan ng chuan o sau:
H2SO4 + 2OH- = SO42- + 2H2O tieu hao Va(ml) dung dch NaOH
H3PO4 + OH- = H2PO4- +

H2O tieu hao Vb (ml) dung dch NaOH


VI = Va + Vb

* Khi dung ch th pT = 10,2 xay ra phan ng chuan o sau:


H2SO4 + 2OH- = SO42- + 2H2O tieu hao Va (ml) dung dch NaOH
H3PO4 + 2OH- = HPO42- + 2H2O tieu hao 2Vb (ml) dung dch NaOH
VII =
Vay VII - VI =

Vb

2VI - VII =

Va

+ 2Vb

Va

T ay ta tnh c nong o ng lng cua H2SO4 va nong o ng lng


cua H3PO4 trong dung dch.
b. Cach tien hanh:
- Dung pipet lay 10 ml dung dch hon hp acid can xac nh nong o vao bnh
tam giac 250 ml, them 1 giot ch th co pT = 5,1 roi chuan o bang dung dch
NaOH en khi dung dch chuyen mau t o nho sang xanh luc. Ghi the tch VI
(lam 3 lan, lay ket qua trung bnh).
Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 21 -

- Dung pipet lay 10 ml dung dch hon hp acid can xac nh nong o vao bnh
tam giac 250 ml, them 2 giot ch th co pT = 10,2 . T buret cho xuong luon VI ml
dung dch NaOH, sau o nho t t tng giot dung dch NaOH en khi dung dch
chuyen mau t vang sang tm. Ghi the tch VII (lam 3 lan, lay ket qua trung bnh).
6. Phan tch mau : Xac nh ham lng phan tram cua Na2CO3 trong mau phong
th nghiem ( theo hng dan cua phong th nghiem )
II. Cau hoi:

1. Trnh bay cach pha 1lt dung dch Na2B4O7 0,1N t tinh the borat
(Na2B4O7.10H2O).
B

2. Giai thch c s chon cac chat ch th trong cac bai th nghiem.


3. Tnh nong o ng lng cua cac dung dch trong cac bai th nghiem.
4. Xac nh ham lng phan tram cua Na2CO3 trong mau phong th nghiem

Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 22 -

Bai 4. PHNG PHAP OXY HOA KH PHEP O PERMANGANAT


I. Tom tat ly thuyet:

Phng phap chuan o oxy hoa - kh la phng phap chuan o da tren phan
ng trao oi electron e xac nh cac chat dang oxy hoa hoac dang kh. e xac
nh mot chat oxy hoa ngi ta dung dung dch chuan la dung dch chat kh co
nong o chnh xac va ngc lai e xac nh mot chat kh ngi ta dung dung dch
chuan la dung dch chat oxy hoa.
- Dung dch chuan oxy hoa: KMnO4, K2Cr2O7 , I2-Na2S2O3, KBrO3, KIO3
- Dung dch chuan kh : TiCl3, Muoi Mohr
e xac nh mot chat nao o, ngi ta thng a chung ve dang oxy hoa hay
kh thch hp.
1. Chat ch th oxy hoa - kh:
Trong phng phap oxy hoa - kh co trng hp khong can s dung chat ch th
ma van nhan ra iem cuoi. V du khi chuan cac chat kh bang dung dch KMnO4,
mot giot dung dch KMnO4 d se lam cho dung dch co mau hong o la dau hieu
e ket thuc chuan o.
Con trong a so trng hp phai dung chat ch th.
Chat ch th oxy hoa -kh la nhng chat ma dang oxy hoa va dang kh co mau
khac nhau. Mau sac cua chat ch th bien oi phu thuoc vao the oxy hoa cua dung
dch.
Mot so chat ch th quan trong :
a. Diphenylamin:

NH

La mot baz hu c khong tan trong nc , tan trong acid H2SO4 am ac .


Trong dung dch, di tac dung cua chat oxy hoa manh (nh K2Cr2O7)
Diphenylamin b oxy hoa bat thuan nghch thanh Diphenylbenzidin .

Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

NH

NH

NH

(Dang kh ) khong mau

-2e-

- 23 -

2H

Eo = 0,76V

(Dang oxy hoa ) mau tm

Khoang the chuyen mau : 0,76 0,059/2


Khi E < 0,73 th dung dch khong mau
Khi E > 0,79 th dung dch co mau tm .
b. Diphenylamin Sulfonat:

NH

SO3Na

De hoa tan trong nc .C che oi mau nh Diphenylamin E0 = 0,85 V. Dang


kh khong mau, dang oxy hoa co mau tm hong co the dung lam ch th e chuan
o cac chat oxy hoa bang FeSO4
c. Acid N-PhenylAnthranilic:
NH

Eo = 1,08 V pH = 0

COOH

C che oi mau giong cac ch th tren, dang kh khong mau, dang oxy hoa co
mau hong tm.
2. Mot so phng phap chuan o oxy hoa kh hay s dung:
a. Phng phap Permanganat:
Da tren phan ng oxy hoa bang dung dch KMnO4. Phan ng nay co the thc
hien trong moi trng acid , kiem hoac trung tnh. Nhng trong thc te khi tien
hanh chuan o bang phng phap permanganat ngi ta thng tien hanh trong
moi trng acid v :
* Trong moi trng acid, ion Mn2+ khong co mau nen de nhan ra iem tng
ng.

Nguyen Th Nh Mai ang Th Vnh Hoa

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HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 24 -

* Kha nang oxy hoa cua KMnO4 trong moi trng acid manh hn nhieu so vi
trong moi trng kiem
Muon xac nh cac chat kh bang dung dch KMnO4 th phai biet chnh xac
nong o cua KMnO4, nhng KMnO4 khong phai la chat goc (v no cha nhieu tap
chat, dung dch lai de b phan huy) nen khong the chuan b dung dch KMnO4
chuan theo lng can. Ma sau khi pha xong phai dung mot dung dch chuan khac
e chuan lai. Ngi ta hay dung dung dch acid Oxalic (H2C2O4) co nong o xac
nh e chuan lai dung dch KMnO4 (trong moi trng acid)
MnO4- + 8H+ + 5eC2O42-

Mn2+ + 4H2O

-2e

2CO2

2MnO4- + 5C2O42- + 16H+

2Mn2+ + 10CO2 + 8H2O

5H2C2O4 + 2KMnO4 + 3H2SO4

2MnSO4 + 10 CO2 + 8H2O + K2SO4

Luc nay H2C2O4 = 1/2M H2C2O4 ; KMnO4 = 1/5 M KMnO4


V KMnO4 thng co lan MnO2 v vay e dung dch KMnO4 c ben, sau khi
pha xong can phai loai bo MnO2 bang cach loc, phai loc bang pheu loc thuy tinh
khong dung giay loc v KMnO4 co the oxy hoa c giay. Sau o bao quan dung
dch KMnO4 trong nhng lo thuy tinh mau toi va cat gi nhng cho toi v anh
sang se lam qua trnh phan huy KMnO4 xay ra mau:
4KMnO4 + H2O

4MnO2 + 4KOH

+ 3O2

Phng phap nay c s dung rong rai trong thc te v KMnO4 la chat oxy
hoa manh nen co the giup xac nh c nhieu chat kh, va lai qua trnh chuan o
khong can ch th e xac nh iem cuoi v ban than KMnO4 co mau ch can 1 giot
d la u lam cho dung dch co mau hong giup nhan iem tng ng.
Moi trng acid c tao ra bang H2SO4, khong dung HCl v ion Cl- se gay ra
phan ng cam ng
10Cl- + MnO4- + 8H+

5Cl2 + Mn2+ + 4H2O

(EoCl2 / 2Cl- = 1.36V)

Bang thc nghiem ngi ta thay rang, neu them vao dung dch chuan o mot
lng Mn2+ th phan ng cam ng se khong xay ra nen ngi ta hay dung hon hp
bao ve Zymmerman (hon hp gom: MnSO4 - H3PO4 - H2SO4)
b. Phng phap Iod:
C s cua phng phap phan tch the tch bang phng phap Iot la qua trnh
oxy hoa - kh, bien I2 thanh I- va ngc lai bien I- thanh I2:
I2 + 2e

2I- (Eo = 0,5345V)

* Mot so chat kh co Eo < 0,5345 V th co the b oxy hoa bi I2


* Mot so chat oxy hoa co Eo > 0,5345 V th co the b kh bi INgi ta dung ca hai tnh chat oxy hoa va kh cua cap I2 / 2I- trong phan tch
the tch

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HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 25 -

i- nh lng chat kh :
V du :

I2 + Na2S2O3
2S2O32- -

2e

Na2S2O6 + 2NaI

(Eo = 0,08 V)

S4O62-

Khi chuan dung dch Na2S2O3 bang I2 mau nau sam cua dung dch I2 se
bien mat ngay khi toan bo Na2S2O3 a c oxy hoa het va mot giot d I2 lam
dung dch co mau vang, cho nen co the chuan o ma khong can dung ch th.
Nhng v mau vang nhat cua I2 rat kho nhan biet iem cuoi nen ngi ta hay dung
ho tinh bot lam ch th. Ho tinh bot co the tao vi I2 mot chat hap phu I2 thanh mau
xanh am khi d I2 hoac bien mat mau khi het lng I2 t do, ieu nay giup nhan
ra iem tng ng de va chnh xac hn. Ch lu y la khong nen cho ch th ho
tinh bot khi trong dung dch con nhieu I2. Ngoai ta con co the dung phng phap
iod e xac nh mot so chat kh khac nh :
SO32-

SO42- + 2I- + 2H+ (Eo SO42- / SO32- = 0,17 V)

+ I2 + H2O

S + 2I- + 2H+ (Eo S / S2- = 0,14 V)

H2S + I2
Sn2+ + I2

Sn4+ + 2I- (Eo Sn2+ / Sn4+ = 0,15 V)

ii- nh lng chat oxy hoa :


Ngi ta phai dung phng phap gian tiep nh sau :
Cho mot the tch chnh xac dung dch chat oxy hoa can xac nh nh K2Cr2O7
vao hon hp dung dch KI d trong moi trng acid. e yen 5 phut cho phan ng
tren xay ra hoan toan, roi dung dung dch Na2S2O3 a biet nong o chnh xac e
chuan lng I2 c giai phong ra
2Na2S2O3 +

I2

Na2S4O6 +

2NaI

Phai dung KI d e phan ng xay ra hoan toan va I2 sinh ra se tao vi I- d mot


phc tan I3-.
Tng t ngi ta co the xac nh :
Br2 + 2I2MnO4- + 10I- + 16H+
ClO3- + 6I- + 6H+

2Br- + I2
2Mn2+ + 5I2 + 8H2O
Cl- +

3I2 + 3H2O

Lu y :
- EoI2/2I- khong u ln nen nhng phan ng trong phep chuan o kho co the
xay ra hoan toan, muon no xay ra hoan toan ta phai tao nhng ieu kien thch hp
- I2 la chat de bay hi nen phai chuan o nguoi va khi nhiet o tang th o
nhay cua ho tinh bot se giam i.
- Khong tien hanh trong moi trng kiem v I2 ket hp vi kiem
- I2 t tan trong nc nen phai dung KI d e tao I3-, nen thc chat chuan I2
bang Na2S2O3 chnh la chuan I3- bang Na2S2O3
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HDTH Phan tch nh lng bang cac phng phap hoa hoc

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- Phai e yen mot thi gian e cho phan ng xay ra hoan toan
- Phai e yen trong bong toi v anh sang se lam cho phan ng phu sau ay xay
2I2 + 2H2O
ra nhanh hn :
4I- + 2H+ + O2
Dung dch chuan Na2S2O3 cung khong the chuan b t lng can c v
Na2S2O3 khong phai la chat goc.
c. Phng phap Dicromate :
K2Cr2O7 co tnh tnh oxy hoa trong moi trng acid
Cr2O72- + 14H+

2Cr3+

+ 6e

+ 7H2O

: Eo = 1,36 V

Dung dch chuan K2Cr2O7 chuan rat on nh . Hau het cac phep chuan o bang
KMnO4 co the thay bang K2Cr2O7 nhng phai dung chat ch th e xac nh iem
cuoi nh Diphenylamin, Diphenylbenzidine. u iem la co the s dung moi trng
HCl ma khong can hon hp bao ve Zymerman .
II. Thc hanh:

1. Xac nh nong o KMnO4 :


a. Nguyen tac :
Ngi ta thng xac nh nong o cua KMnO4 trong moi trng axit qua cac
chat goc sau :
- H2C2O4 .2H2O
- Na2C2O4 hoac (NH4)2C2O4 . H2O
- K4 [ Fe(CN)6 ] ...
Trong bai nay, ta xac nh nong o KMnO4 bang chat goc H2C2O4. H2O
MnO4- + 5e + 8H +
C2O42- - 2e
5H2C2O4+2KMnO4+3H2SO4
b. Cach tien hanh :

Mn 2 + + 4H2O
2CO2
2MnSO4 +10CO2+8H2O+K2SO4

Dung pipet lay 10 ml dung dch H2C2O4 0,05N va pha vao bnh non 250 ml,
them 2 ml H2SO4 3N un nong (khong c un soi). T buret nho tng giot
KMnO4 can xac nh, lac eu ti khi dung dch co mau hong ben khoang 50 giay
(lam 3 lan, lay ket qua trung bnh).
2. Xac nh nong o Fe3+ :
a. Nguyen tac :
- Kh Fe3+
Fe2+ bang Zn0 hoac bang SnCl2 trong moi trng acid (
ay dung SnCl2) va loai SnCl2 d bang HgCl2
2FeCl3 + SnCl2

2FeCl2 + SnCl4

SnCl2 + 2HgCl2

Hg2Cl2 + SnCl4

Nguyen Th Nh Mai ang Th Vnh Hoa

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HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 27 -

- Chuan Fe2+ va c chuan bang KMnO4


MnO4- + 5e + 8H+
Fe2+ - e

Mn2+ + 4H2O
Fe3+

5Fe2+ + MnO4- + 8H +

5Fe3+ + Mn2+ + 4H2O

* Chu y :
Ion Cl- lam tr ngai phan ng. e tranh anh hng cua ion Cl- ngi ta them
hon hp bao ve (gom 67g MnSO4. 4H2O + 138 ml H3PO4 d = 1,7 + 130 ml H2SO4
d = 1,81 pha trong 1 lt ).
b. Cach tien hanh :
Dung pipet lay 10 ml dung dch Fe3+ can xac nh vao bnh non 250 ml, them 2
- 3 ml HCl 1:2, un nong ti 60 - 700C roi lay ra, cho tng giot dung dch SnCl2
5% vao va lac eu ti khi dung dch mat mau vang them 1 giot dung dch SnCl2 roi
pha loang ti gan 100 ml bang nc cat. Them tng giot dung dch HgCl2 5% lac
eu, neu co ket tua trang la c. Con neu co ket tua xam en th phai lam lai.
Them 10 ml hon hp bao ve (MnSO4 + H3PO4 + H2SO4). T buret nho tng giot
dung dch KMnO4 co nong o xac nh, lac eu ti khi dung dch co mau hong ben
khoang 50 giay. Ghi so ml dung dch KMnO4 a dung (lam 3 lan, lay ket qua trung
bnh).
3. Xac nh nong o H2O2 :
a. Nguyen tac :
5 H2O2 + 2 MnO4- + 6 H+

2 Mn2+ + 5 O2 + 8 H2O

b. Cach tien hanh :


Lay 10ml dung dch can phan tch them 3 ml H2SO4 3N roi chuan o bang dung
dch KMnO4 en xuat hien mau hong ben khoang 50 giay, ghi so ml dung dch
KMnO4 a dung (lam 3 lan, lay ket qua trung bnh).
4. Phan tch mau: Xac nh so gam H2O2 trong 1lt dung dch phong th nghiem
(theo hng dan cua phong th nghiem )
III. Cau hoi:

1. V sao khong the ieu che dung dch chuan KMnO4 bang cach tnh theo lng
can chnh xac ?
2. Co the chuan o dung dch KMnO4 bang dung dch H2C2O4 theo th t ngc
lai ngha la cho acid H2C2O4 tren buret c khong ?
3. Tai sao khi xac nh nong o dung dch KMnO4 phai un nong (khong c un
soi) dung dch at di ?
4. Hay neu tac dung cua tng thanh phan trong hon hp bao ve Zymmerman khi
chuan o Fe2+ bang phng phap permanganat.

Nguyen Th Nh Mai ang Th Vnh Hoa

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HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 28 -

5. Ban chat cua phep xac nh Fe3+ bang phng phap permanganat la g. Tai sao
khi dung chat kh la SnCl2 lai phai loai lng SnCl2 d. Lam the nao ?
6. Trnh bay nguyen tac xac nh nong o dung dch H2O2 bang phng phap
permanganat. Xac nh so gam H2O2 trong mot lt dung dch mau phong th
nghiem.

Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 29 -

Bai 5. PHNG PHAP OXY HOA KH PHEP O DICROMAT VA IOD

I. Thc hanh:

1. Xac nh nong o Fe2+ :


a. Nguyen tac :
Dung K2Cr2O7 biet nong o, xac nh Fe2+ trong moi trng axit
Cr2O72- + 14H+ + 6e

2Cr3+ + 7H2O

Fe2+ - e
Cr2O72- + 6Fe2+ + 14H+

Fe3+
2Cr3+ + 6Fe3+ + 7H2O

Dung chat ch th diphenylamin co Eo= 0,76V hoac diphenylamin sulfonat co Eo


= 0,84V hay acid phenylanthranilic co Eo = 1,08V .
b. Cach tien hanh :
-Vi ch th diphenylamin: dung pipet lay 10 ml dung dch Fe2+ can xac nh
vao bnh non 250 ml. Them 1ml H3PO4 4N + 5ml HCl 1:2 + 2-3 giot chat ch th
diphenylamin. T buret nho tng giot K2Cr2O7 nong o xac nh, lac ti khi dung
dch co mau xanh tm. Ghi so ml K2Cr2O7 a dung (lam 3 lan, lay ket qua trung
bnh).
-Vi ch th diphenylamin sulfonat: tien hanh tng t nh tren
-Vi ch th acid phenylanthranilic: tien hanh tng t nh tren nhng khong
them acid H3PO4.
-Nhan xet cac ket qua phan tch khi s dung cac ch th tren.
2. Xac nh SO32- trong Na2SO3 :
a. Nguyen tac :
Chuan o trc tiep SO32- bang dung dch K2Cr2O7 trong moi trng H2SO4 hoac
HCl ti khi oi mau cua diphenylamin. Phan ng chuan o:
3SO32- + Cr2O72- + 8H+

3SO42- + 2Cr3+ + 4H2O

b. Cach tien hanh :


Lay 10 ml dung dch can xac nh cho vao bnh non 250 ml, them 10 ml HCl 1:2
va 3 - 4 giot ch th diphenylamin. Pha loang thanh 30 ml. Chuan o bang dung
dch K2Cr2O7 en khi xuat hien mau xanh tm. Ghi the tch dung dch K2Cr2O7 a
dung (lam 3 lan, lay ket qua trung bnh).

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HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 30 -

3. Xac nh nong o Na2S2O3 :


a. Nguyen tac :
Lay mot the tch chnh xac dung dch chuan K2Cr2O7 cho phan ng vi lng
d KI trong moi trng acid e tao ra lng tng ng I3-.Chuan o I3- trc tiep
bang Na2S2O3 vi ch th ho tinh bot.
Cr2O72- + 6I- + 14H+
3I2 +3I-

2Cr3+ +3I2 + 7H2O


3 I3 -

Cr2O72- + 9 I- + 14H+

2Cr3+ + 3 I3- + 7H2O

Phan ng chuan o:
I3- + 2S2O32-

3 I- + S4O62-

b. Cach tien hanh :


Dung pipet lay 10 ml dung dch K2Cr2O7 co nong o xac nh vao bnh non 100
ml, them 5 ml H2SO4 4N + 10 ml KI 5%, lac nhe ay bnh non bang knh ong ho ,
e yen cho toi 10 phut. T buret nho tng giot dung dch Na2S2O3 ti khi dung
dch co mau vang luc + 1 ml ho tinh bot 1%. Tiep tuc nho tng giot dung dch
Na2S2O3 ti khi mat mau xanh tm. Ghi so ml dung dch Na2S2O3 a dung (lam 3
lan, lay ket qua trung bnh).
4. Xac nh nong o Cu2+ :
a. Nguyen tac :
Trong moi trng acid (pH = 1 2 ) Cu 2+ oxy hoa I- e tao thanh ket tua CuI va
mot lng tng ng I3-.Chuan o lng I3- bang dung dch Na2S2O3 vi ch th
ho tinh bot.
Cu2+ + I- + 1e
3I- - 2e
2Cu2+ +5I-

CuI
I32CuI

I3-

Ngoai ra thng them NH4SCN vao, van am bao lam tang the cua Cu2+ / Cu+
lam giam s hap phu I2 ( di dang I3- ) tren be mat cua ket tua CuI, v luc nay a
c thay bang CuSCN
CuI + SCN-

CuSCN + I-

Phan ng chuan o:
I3- + S2O3 2-

3I- + S4O62-

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- 31 -

b. Cach tien hanh :


Dung pipet lay 10 ml dung dch Cu2+ can xac nh vao bnh non 250 ml. Them
2,5 ml dung dch CH3COOH 4N va 2,5 ml dung dch KI 5% lac nhe. ay bnh non
bang knh ong ho va e yen cho toi khoang 10 phut. T buret nho tng giot
dung dch Na2S2O3 , lac eu ti khi dung dch co mau vang rm + 0,5 ml ho tinh
bot va tiep tuc nho tng giot dung dch Na2S2O3 xuong ti mat mau xanh tm, them
2,5 ml dung dch KSCN 10% lac ky, chuan o en hoan toan mat mau xanh. Ghi
so ml dung dch Na2S2O3 a dung (lam 3 lan, lay ket qua trung bnh).
5. Xac nh nong o acid :
a. Nguyen tac :
Trong moi trng trung tnh, KIO3 khong oxy hoa c KI e giai phong I2.Tuy
nhien khi co mat acid,can bang cua phan ng dch chuyen ro ret, giai phong ra
mot lng I2 ( di dang I3- ) tng ng vi lng acid manh co mat. Ta chuan
o lng I3- giai phong ra bang dung dch chuan Na2S2O3 roi tnh ra nong o acid
manh.
IO3- + 8 I- + 6H+

3I3- + 3H2O

Phan ng chuan o:
I3- + 2 S2O32-

3 I- + S4O62-

Dung ho tinh bot lam ch th .


b. Cach tien hanh :
Lay 10 ml dung dch H+ can xac nh nong o cho vao bnh 250 ml a cha san
2 ml KIO3 1,5% va 2 ml KI 10% . Lac eu hon hp 1 - 2 phut. Chuan lng I2
thoat ra bang dung dch chuan Na2S2O3 en khi dung dch co mau vang rm, th
them t t ho tinh bot e c mau xanh cham ro ret. Tiep tuc chuan o en mat
mau xanh cham (lam 3 lan, lay ket qua trung bnh).
6. Phan tch mau: Xac nh so gam Fe2+ trong 1 lt dung dch phong th nghiem.
II. Cau hoi:

1. So sanh phng phap permanganat va phng phap bicromat.


2. Vai tro cua H3PO4 trong phep xac nh Fe2+ vi ch th diphenylamin. Tai sao
khi dung ch th acid phenylanthranylic thay cho ch th diphenylamin e chuan
o Fe2+bang phng phap bicromat th lai khong can ti H3PO4 ?
3. Nhng chat oxy hoa nao, chat kh nao co the xac nh bang phng phap
iod. Neu nguyen tac chung e xac nh bang phng phap nay.
4. Hay mo ta ac iem cua cap I2 / 2I- ve mat v tr trong bang the oxy hoa va
ve kha nang ap dung no trong phan tch.
5. Hay neu nhng ieu kien can tuan theo khi tien hanh nh lng bang
phng phap iod.
6. Xac nh nong o ng lng cua cac chat trong bai thc tap.
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HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 32 -

7. Tnh so gam Fe2+ trong mot lt dung dch mau phong th nghiem.
8. Tnh lng can e pha mot lt dung dch K2Cr2O7 0,1N

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HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 33 -

Bai 6. PHNG PHAP CHUAN O KET TUA


I. Tom tat ly thuyet:

1. Nguyen tac:
Phng phap chuan o ket tua da tren cac phan ng tao thanh hp chat t tan.
Cac phan ng nay phai thoa man cac ieu kien sau:
- Phan ng phai xay ra hoan toan, hp chat tao thanh phai co cong thc xac
nh.
- Toc o phan ng phai kha ln.
- Phan ng phai chon loc.
- Phai co chat ch th thch hp cho phep xac nh c iem tng ng cua
phep chuan o.
Co nhieu phng phap chuan o ket tua nhng phng phap bac la phng
phap hay dung nhat hien nay, thuoc th c s dung la dung dch AgNO3 dung
e chuan cac halogenua Cl-, Br-, I-, va SCN-.
2. Cac phng phap xac nh iem cuoi trong phng phap o Bac:
a. Phng phap Mohr: Dung K2Cr2O4 lam ch th, tai iem cuoi chuan o se
xuat hien ket tua Ag2CrO4 mau o gach, dung e xac nh Cl-, Br-.
Nguyen tac them vao dung dch can xac nh (dung dch muoi cua Cl-, Br-) ch
th CrO42-. Sau o chuan o bang dung dch AgNO3, khi o se xay ra cac phan
ng:
Ag+

+ X- (Cl- , Br-)

Ag+d

CrO42-

Ta co T AgBr = 10-12.28

AgX

(1)

Ag2CrO4 o gach

(2)

, T AgCl = 10-9.75 , T Ag2CrO4 = 10-11.95

Ket thuc qua trnh chuan o khi dung dch chuyen t mau trang uc cua AgCl
hoac vang nhat cua AgBr sang o gach cua Ag2CrO4.
Van e quan trong ay la phai tnh nong o CrO42- nh the nao e cho phan
ng th (2) xay ra ngay ung tai iem tng ng. Khi cho AgNO3 vao dung dch
gom Cl- (hoac Br-),CrO42- th AgCl (hoac AgBr) se ket tua trc tuy nhien do tch
so tan cua chung khong khac nhau mc o cho phep e cho chat nay ket tua
hoan toan roi mi xuat hien ket tua kia. V vay ay can phai xac nh [CrO42-]
can thiet e cho Cl- (hoac Br-) c ket tua hoan toan va ket tua cua CrO42- vi
Ag+ phai xuat hien tai iem tng ng. Ta a tnh c [CrO42-] = 10-2,2M =
6.31.10-3 M trong thc te ngi ta hay dung nong o 5.10-3 M.
Phng phap Mohr c dung e nh lng Cl-, Br- nhng khong c dung
e xac nh I- va SCN- v tua AgI va AgSCN hap phu manh CrO42- qua ro ret lam
cho s chuyen mau xay ra trc iem tng ng va iem tng ng khong

Nguyen Th Nh Mai ang Th Vnh Hoa

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HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 34 -

ro rang gay ra sai so ln. S chuan o theo phng phap Mohr can phai c tien
hanh trong moi trng trung tnh hoac baz yeu, thng th pH = 6,5 10,3 o la v:
- moi trng acid (pH thap), o nhay cua ch th giam do o tan Ag2CrO4
tang.
Ag2CrO4
CrO42- + H+

2Ag+

CrO42-

HCrO4-

ieu nay gay ra sai so dng, mat khac


2CrO42- + 2H+

Cr2O72- + H2O lam giam nong o CrO42-

- Trong moi trng kiem (pH qua cao) th:


Ag+ + OH-

AgOH

Ag2O + H2O cung gay ra sai so

Thng ngi ta hay dung dung dch NaHCO3 e tao moi trng
Lu y :
- Neu trong dung dch chuan o co NH4+ th phai chuan o trong moi trng pH
= 6,5 7,2 v neu pH > 7,2 th se co s tao thanh NH3 va NH3 se tao phc ben vi
ion Ag+ gay sai so
- Dung dch chuan o khong c cha cac ion can nh : nhng ion co the phan
ng c vi CrO42- nh Ba2+, Pb2+ , va khong co nhng anion co the tao ket
tua vi Ag+ nh CO32-, C2O42-, PO43- neu co , chung ta phai tm cach che.
b. Phng phap Fajans:
S dung ch th hap phu, thng dung la Fluorescein dung e xac nh Cl-, Br-,
I , va SCN-.
-

Trong qua trnh chuan o cac halogenua X- bang AgNO3, trc iem tng
ng trong dung dch d X- nen AgX se hap phu X- tao thanh nhng hat keo
mang ien tch am {(AgX)nClx-x}. Tai iem tng ng trong dung dch khong d
Ag+ va X- nen cac ket tua khong mang ien tch, chung lang xuong lam cho dung
dch tr nen trong. Ngi ta goi la iem ang ien. Sau iem tng ng dung
dch co d Ag+ nen ket tua AgX hap phu Ag+ hnh thanh hat keo mang ien tch
dng {(AgCl)nAgx+x}
Da vao tnh hap phu cua cac hat keo Fajans a dung mot so pham mau hu c
co kha nang hap phu len be mat cua ket tua tao mau ac trng e nhan ra iem
tng ng ma fluorescein la mot ien hnh. Fluorescein (viet tat la HFl) la mot
acid hu c yeu co kha nang phat huynh quang, dang phan t t do va dang anion
khi b hap phu co mau khac nhau. Trong nc co can bang nh sau:
HFl

H+ + Fl-

Trc iem tng ng cac hat keo mang ien tch am, nen cac anion Fl- cua
fluorescein khong b hap phu. Sau iem tng ng cac hat keo mang ien tch
dng nen cac anion Fl- b hap phu:

Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc
(AgCl)nAgx+x +

xFl-

xanh luc

- 35 -

{(AgCl)nAgxx+}xFlMau hong

Lu y : Khong phai dung dch chuyen t xanh luc sang hong ma sau iem tng
ng do s hap phu tren be mat tua nen tua se co mau hong.
ieu kien cua nhng chat ch th hap phu la :
- Phai va ch hap phu tai iem tng ng
- Moi trng dung dch phai thch hp e dang b hap phu ton tai c
(thng pH <10)
Hien tng t hap phu se tang khi dien tch be mat cua hat keo tang len. Nen
trong thc te ngi ta hay them ho tinh bot hoac dextrin e tang dien tch be mat
va gi tua AgX trang thai keo.
c. Phng phap Volhard:
Nguyen tac: Them mot lng d dung dch AgNO3 a biet nong o chnh xac
vao dung dch X-, roi chuan lng Ag+ d bang dung dch SCN- (NH4SCN hoac
KSCN) vi ch th la Fe3+. Cac phan ng cua qua trnh chuan o:
Ag+
Ag+d

+ X-

AgX

+ SCN-

SCN- d + Fe3+

AgSCN

TAgSCN = 1,1.10-12

Fe(SCN)2+ phc ben co mau o mau

Vay iem tng ng la luc dung dch chuyen sang mau hi hong, v TAgSCN
= 1,1.10-12 < TAgCl =10-9,75 nen co the xay ra phan ng:
AgCl

+ SCN-

AgSCN + Cl-

e ngan nga phan ng nay, ta phai loc tua AgCl trc khi chuan Ag+d bang
SCN-. Ngoai cach loc bo tua AgCl ngi ta co the cho them mot t Nitrobenzen,
chat nay se bao quanh AgCl ngan khong cho AgCl phan ng vi SCN-.
Mat chung ta ch nhan ra mau hong iem tng ng khi [Fe(SCN)2+]
6,4.10-6M.
Nh vay phng phap Volhard co the dung e xac nh trc tiep Ag+ (dung
dung dch chuan KSCN vi chat ch th la Fe3+) ngoai ra no con co the xac nh
Cl-, Br-, I-, theo phng phap chuan o ngc khi o:

CN

=
X

(C N V ) AgNO 3 (C N V ) SCN
V

Khac vi 2 phng phap trc, phng phap nay thc hien trong moi trng acid
(0,1-1 N ) e ngan nga s thuy phan cua muoi Fe3+ .

Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 36 -

II. Thc hanh:

1. Xac nh nong o Cl- theo phng phap Mohr :


a. Nguyen tac :
Phan ng chuan o :
Cl- + Ag+

AgCl trang

Phan ng ch th :
CrO42- + 2Ag+
b. Cach tien hanh :

Ag2CrO4 o gach

Dung pipet lay 10 ml dung dch cho vao bnh tam giac, them 2 ml dung dch
NaHCO3 5%, 0,5 ml K2CrO4 5%. T buret nho t t dung dch AgNO3 0.01M,
lac manh en xuat hien mau o gach (lam 3 lan, lay ket qua trung bnh).
2. Xac nh nong o Cl- theo phng phap Fajans :
a. Nguyen tac :
Chuan o Cl- bang dung dch AgNO3 0.01M trong moi trng em NaHCO3 khi
co mat Fluorescein (HFl) lam ch th.
Phan ng chuan o :
Cl- + Ag+

AgCl trang

Phan ng ch th : Khi cho d 1 giot Ag+, hat keo (AgCl)n tch ien dng se
hap phu anion Fl- va tr thanh mau hong.
(AgCl)n.Agx+x + xFl-

[(AgCl)n.Agxx+]xFl-

xanh luc

mau hong

b. Thc hanh :
Dung pipet lay 10 ml dung dch vao bnh tam giac, them 2 ml NaHCO3 5%, 3
giot ch th Fluorescein 0,5%. T buret nho t t dung dch AgNO3 0.01M lac
manh en khi be mat ket tua chuyen sang mau hong (lam 3 lan, lay ket qua trung
bnh).
3. Xac nh nong o Br- theo phng phap Volhard :
a. Nguyen tac :
Ket tua Br - di dang AgBr bang mot lng d chnh xac AgNO3 0.01M khi
co mat muoi Fe3+ .
Phan ng chuan o :
Br - + Ag+
Ag+d + SCN-

AgBr
AgSCN

Phan ng ch th :
Fe3+ + SCN-

FeSCN2+

Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 37 -

b. Cach tien hanh :


Dung pipet lay 10 ml dung dch cho vao bnh tam giac, them 2 ml HNO3 6N. T
buret them chnh xac 1 lng AgNO3 a biet nong o ti khi khong con ket tua
na, them 5 ml AgNO3 na, 10 giot ch th phen sat III bao hoa. T buret nho tng
giot SCN- co nong o a biet xuong, lac eu ti khi dung dch oi mau. Ghi so ml
SCN- a dung lam 3 lan, lay ket qua trung bnh .
4. Xac nh nong o K4[Fe(CN)6] theo ZnSO4.7H2O:
a. Nguyen tac :
Phan ng chuan o :
3Zn2+ + 2K+ + 2Fe(CN)64-

Zn3K2[Fe(CN)6]2

Phan ng ch th :
Do ket tua Zn3K2[Fe(CN)6]2 rat t tan nen nong o Fe(CN)64- trc T rat
nho, lam cho cap ferri / ferro co the cao vot, vt qua EIno = +0,76 V cua
diphenylamin.
E = Eo ferri/ferro + 0.059 lg

[ferri]
[ferro]

= +0.36 + 0.059 lg

[ferri]
[ferro]

V vay dung dch co mau cham tm cua diphenylamin benzidin.


Sau T, nong o ferro tang ot ngot lam cho the E ferri/ferro giam ot ngot,
thap hn +0,76V. V vay diphenylamin benzidin chuyen ve dang khong mau.
Cach tien hanh :
Dung pipet lay 10 ml dung dch Zn2+ 0,05M vao bnh tam giac. Them 20
giot H2SO4 ac, 3 ml (NH4)2SO4 10% + 2 giot ch th diphenylamin 1% + 1 ml dung
dch K3[Fe(CN)6] 1%, chuan o bang dung dch K4[Fe(CN)6] ti khi dung dch
chuyen t mau cham tm sang mau xanh la cay nhat, va chuan o va lac that
manh dung dch (lam 3 lan, lay ket qua trung bnh).
5. Phan tch mau: Xac nh ham lng phan tram Cl- trong muoi an (theo hng
dan cua phong th nghiem ).
III. Cau hoi:

1. Neu cac ieu kien can thiet e mot phan ng ket tua co the dung c trong
phan tch the tch.
2. Phng phap Mohr, Fajans va Volhard dung e xac nh nhng ion nao. Neu
cac ieu kien e thc hien cac phng phap tren.
3.Vai tro cua NaHCO3 trong phep xac nh Cl- theo phng phap Mohr va
Fajans. Them 2 ml HNO3 6N khi thc hien phng phap Volhard e lam g ?
Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 38 -

4.Giai thch c che oi mau cua chat ch th diphenylamin trong phep inh lng
kem bang phng phap lam ket tua vi K4[Fe(CN)6].
5. Tnh nong o ng lng cua cac chat trong cac bai thc tap.
6. Xac nh ham lng phan tram NaCl trong mau phong th nghiem.

Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 39 -

Bai 7. PHNG PHAP PHAN TCH KHOI LNG


I. Thc hanh:

1. Xac nh SO42- trong MgSO4.7H2O di dang can BaSO4:


a. Nguyen tac:
Hoa tan mau sulfat trong nc cat. Tien hanh ket tua sulfat di dang BaSO4
trong moi trng acid, un nong, them tng giot dung dch BaCl2 loang en ket tua
hoan toan. Phan ng ket tua:
SO4 2- +

Ba 2 +

BaSO4

cho d
BaSO4 la ket tua tinh the trang, c lam muoi e ket tua tr nen tinh khiet va
de loc. Loc gan va ra gan tren giay loc mn (bang xanh). Nung en khoi lng
khong oi 9000C .
Cac sai so he thong can lu y loai bo:
- Can ket tua trong moi trng acid e tranh s ket tua cua muoi t tan khac cua
Ba2+ nh BaCO3, Ba3(PO4)2. Tuy nhien neu qua nhieu acid manh th co the lam tan ro
ret BaSO4 e tao thanh Ba(HSO4)2 tan (sai so am).
- Can lam muoi ket tua e loai tr s cong ket cac sulfat kim loai( Fe3+,
Mg2+...). Chung co phan t lng thap hn BaSO4, lam thap ket qua xac nh. S
cong ket muoi NH4+ cung lam thap ket qua xac nh (sai so am)
- S co mat Cr 3+ lam cho ket tua BaSO4 kem hoan toan v Cr3+ tao c phc
sulfat tan lam giam thap ket qua xac nh (sai so am )
- S cong ket cac anion Cl-, NO3-, ClO3- tren tua BaSO4 co tac dung lam cao ket
qua xac nh (sai so dng).
- Khi nung ket tua BaSO4 qua nhanh (khong d Oxy e ot chay giay loc) co
the xay ra phan ng kh BaSO4 bi cacbon cua giay loc ( sai so am )
BaSO4 +

4C

BaS

4CO

b. Cach tien hanh:


- Can khoang 0,3 0,4 g mau cho vao coc c 250 ml. Hoa tan trong khoang 50
ml nc cat va them 2 ml HCl 2N. Neu thay co can khong tan th em loc tren
giay loc bang o hoac trang. Ra giay loc va thu hoi nc loc lan nc ra, them
nc cat thanh khoang 100 ml. un nong ti 60 700C. T buret nho tng giot
dung dch BaCl2. 2H2O 1% va nho va khuay eu bang ua thuy tinh au bt cao
su. Khi cho tiep ma khong thay ket tua them, th can c vao so mL a dung tren
buret, cho them d khoang 50% na e s ket tua BaSO4 c hoan toan. Khuay
eu dung dch mot lan na va at coc vao bnh cach thuy e lam muoi t 1 en 2
gi (neu co ieu kien th e cach em).

Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 40 -

- Loc gan ket tua tren giay loc mn khong tan (bang xanh) ra gan ket tua 3 lan
bang nc cat un nong va sau cung chuyen nh lng toan bo ket tua trong coc
len giay loc. Lng vet ket tua bam vao thanh coc th lay ra bang cach dung mot
mau giay loc nho khong tan lau mat trong cua thanh coc, mau giay loc nay em
gop vao giay loc tren pheu. Cung co the dung ua thuy tinh au bt cao su e lay
ra vet ket tua bam vao thanh coc, sau o lau sach au ua nay vao giay loc a
dung e ket tua.
- Goi giay loc va co ket tua theo ch dan cua can bo phu trach roi at vao chen
s co anh so va c un nong trc 900C en khoi lng khong oi va a can
chnh xac khoi lng m1 (g). at chen mi au phan ngoai lo nung e tro hoa
hoan toan sau o ay chen nung vao sau trong lo, ong ca lo lai. Nung 9000C
en khoi lng khong oi. Coi la at khi hai lan can lien tiep sai nhau di 0,2 mg.
Can khoi lng m2 tren ung chiec can a dung e can m1. Tnh % SO4 2- trong
mau.
2. Xac nh Fe3+ trong phen sat di dang can Fe2O3:
a. Nguyen tac:
Dung NH3 ac e ket tua nhanh chong Fe3+ di dang hydroxyd trong dung
dch nong:
2Fe 3+ + 6NH3 + (x + 6)H2O

2Fe(OH)3. xH2O + 6NH4+


dang ket tua

Dang ket tua thuoc dang vo nh hnh (sol) nen can nhanh chong em loc va
ra, khong lam muoi. Nung ket tua e chuyen thanh Fe2O3:
2Fe(OH)3.xH2O

Fe2O3

(x +3)H2O

9000C
dang ket tua

dang can

Cac sai so he thong can lu y loai bo:


- Can ket tua t dung dch NH3 ac, dung dch Fe3+ ac va nong e ket tua
vo nh hnh nhanh chong ong tu thanh khoi tach ra khoi tng long, giam cong
ket (sai so dng).
- Loc gan lay ket tua bang giay loc khong tan, mn trung bnh (bang trang
hoac bang o) e chay nhanh, giam cong ket (sai so dng).
- Dung dch ra can phai nong va co them chat ien ly manh de phan huy
nhiet o cao. Chat ien ly co tac dung ngan chan qua trnh pepti hoa ket tua ong
tu (sai so am).
- Can nung ket tua co u oxy, tang nhiet o t t len ti 9000 10000C e
ngan nga s kh mot phan Fe3+
Fe2+ tao ra Fe3O4 (kiem tra bang nam
cham). Neu thay con lan Fe3O4 th tam vai giot HNO3 ac, dung ua thuy tinh
dam nho thanh bot mn, lau ua thuy tinh bang mau giay loc khong tan va tiep tuc
nung en khoi lng khong oi (sai so am).
Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 41 -

Neu dung dch ch co muoi Fe3+ (khong lan Fe2+) th khi cho d NH3 phai thu
c ket tua mau o, neu thay mau en hoac gan nh en th chng to a lan
Fe2+. Tot hn la bo i lam lai, hoac trc khi nung th tam HNO3 ac e oxy hoa
Fe2+

Fe3+ (sai so am).

- Dung dch NH3 ac e lau trong bnh thuy tinh thng co lan mot phan oxid
silicnen trc khi dung phai loc (sai so dng).
- V ket tua Fe(OH)3.xH2O rat t tan nen co the ra bang NH4NO3 nhieu lan
cho en khi het ion Cl- (dung AgNO3 th). Lu y acid hoa nc ra bang vai giot
HNO3 roi mi nho AgNO3 (sai so dng).
b. Cach tien hanh:
- Lay coc c 100 ml cho vao 5 ml HCl ac, 3 ml HNO3 ac. at ua thuy tinh
vao coc, ay bang mat knh ong ho va un nong. Trang ua thuy tinh, knh ong
ho va thanh trong cua coc bang nc cat sao cho the tch dung dch trong coc
khong vt qua 20 30 ml.
- Khuay lien tuc va o nhanh 10 ml NH3 ac (loai 25%) phai thay mui NH3,
tiep tuc khuay va o vao o 50 ml nc cat nong. Tiep tuc un 10 phuc roi bat au
loc gan len giay loc bang trang. Ra bang NH4NO3 2% en khi het ion Cl- (1 giot
AgNO3 1% cho vao 5mL nc ra a acid hoa bang HNO3. Sau cung chuyen nh
lng toan bo ket tua len giay loc, dung ua thuy tinh au bt cao su va mot mau
giay loc khong tan lau sach vet ket tua con bam tren thanh coc. Goi giay loc va
chuyen sang chen s a nung trc 9000C va a can trc khoi lng m1 (g). Nung
t t 9000C cho e khi khoi lng m2 (g) khong oi. Kiem tra s co mat cua oxyd
sat t bang nam cham.
Tnh so gam sat co trong mau.
3. Phan tch mau: Xac nh nong o Fe3+ trong mau phong th nghiem (theo
hng dan cua phong th nghiem).
II. Cau hoi:

1. Neu tac dung cua s lam muoi ket tua BaSO4, neu keo dai co hai khong ?
2. Neu s y e cho mot phan BaSO4 bien thanh BaS th x ly nh the nao ?
3. T cac ieu kien cu the cua viec xac nh Fe3+ hay neu cac quy tac chung
nhat e thu c mot ket tua vo nh hnh tinh khiet va de loc.

Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 42 -

Bai 8. PHNG PHAP COMPLEXON


I. Tom tat ly thuyet:

1. Nguyen tac:
Cac phng phap chuan o phc chat da tren phan ng tao phc cua cac
chat. Co nhieu phng phap chuan o phc chat nhng trong phan tch the tch
ngi ta thng dung nhat la phng phap Complexon.
Nguyen tac cua phng phap nay la da tren kha nang tao phc ben gia ion
kim loai can xac nh vi cac thuoc th hu c complexon. Cac phan ng nay
thoa man cac ieu kien cua phan ng dung trong phan tch the tch. V vay
phng phap nay rat pho bien
Complexon la ten goi chung cua cac dan xuat cua cac acid
aminopolycarbocylic, co nhieu loai complexon nhng trong phan tch thng dung
complexon III (con goi la EDTA) la acid EtylenDiaminTetraAcetic viet tat H4Y
HOOC CH2
HOOC CH2

CH2 COOH
CH2 CH2 N

CH2 COOH

Nhng do H4Y t tan trong nc nen trong thc te ngi ta hay dung muoi
dinatri cua no goi la complexon III (con goi la Trilon B) viet tat Na2H2Y
HOOC CH2
NaOOC CH2

CH2 COONa
N

CH2 CH2 N

CH2 COOH

Trong phng phap nay can phai s dung nhng chat ch th mau kim loai e
nhan ra iem tng ng. Nh vay khi cho ch th vao dung dch can phai phan
tch th ion kim loai can xac nh se phan ng vi ch th tao thanh mot phc co
mau. Khi chuan bang H2Y2- th thuoc th nay se ay ch th ra khoi phc mau va
tao thanh e tao thanh phc MeY2- khong mau ben hn. Nh vay iem cuoi cua
phep chuan o, chat ch th mau kim loai dang t do se c giai phong ra. V
vay khi dung dch chuyen t mau cua phc gia ch th vi kim loai sang han mau
cua ch th t do th o la thi iem ket thuc chuan o. Do o ieu kien can thiet
cho viec chuan complexon trc tiep la hang so ben cua phc gia kim loai vi
H2Y2- phai ln hn o ben cua phc gia kim loai vi ch th.
Du cac ion kim loai co hoa tr khac nhau nhng 1 ion gam kim loai luon luon
tng tac vi 1 ion gam complexon III ong thi giai phong ra 2H+ .
Me2+ +

H2Y2-

MeY2-

+ 2H+

Me3+ +

H2Y2-

MeY-

+ 2H+

Me4+ +

H2Y2-

MeY

+ 2H+

Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 43 -

Cho nen ng lng gam cua kim loai va complexon eu bang phan t lng
cua chung chia cho 2.
2. Cac ch th thng dung trong chuan o complexon:
e nhan ra iem tng ng trong phng phap complexon ngi ta hay
dung nhat la cac ch th mau kim loai, o la nhng chat mau hu c co kha nang
tao vi ion kim loai phc co mau, va trong nhng ieu kien xac nh mau cua
phc o khac vi mau cua chat ch th t do.
Cac chat ch th mau kim loai thng la nhng acid yeu hoac baz yeu, v vay
mau cua ch th cung phu thuoc vao pH cua dung dch. Do o khi chuan mot ion
kim loai nao o bang phng phap complexon can chon pH thch hp e phan ng
tao phc gia ion kim loai va complexon III xay ra hoan toan va mau cua ch th
t do phai tng phan vi mau cua phc gia no vi ion kim loai e de nhan ra
diem tng ng v the can dung nhng dung dch em. Nhng ch th thng
dung gom:
a. Eriocrom T en
(ETOO hoac NET) la mot a acid yeu ky hieu la H3Ind. Trong dung dch nc
no phan ly va co mau thay oi theo pH
H3Ind

H2Indo

HInd2-

Ind3-

Xanh biec

Da cam

Trong khoang pH t 7 11 ch th nay ton tai dang HInd2- co mau xanh con
phc cua cac ion kim loai vi ch th co mau o (s chuyen mau o- xanh hoac
xanh - o la tng phan) v vay khi dung ch th nay ngi ta hay tien hanh moi
trng pH = 10. pH nay ch th (HInd2- ) se tao vi ion kim loai phc co mau o
nho
Me2+

HInd2Xanh

MeInd- + H+
o nho

Khi chuan bang complexon III phc MeInd- b pha v ion kim loai ket hp vi
complexon III tao thanh 1 phc ben hn con HInd2- c giai phong ra va tch luy
lai trong dung dch lam cho dung dch co mau xanh
MeInd- +

H2Y2-

MeY2-

o nho

HInd2- +

H+

Xanh

Vay ket thuc chuan o khi dung dch chuyen t mau o nho sang xanh biec, e
duy tr pH t 8 10 ngi ta thng dung he em NH4OH - NH4Cl
b. Murexit:
Thng viet tat la H4Ind- trong nc no phan ly nh sau:
H4IndTm hong

H3Ind2Tm

H2Ind3Xanh tm

Khi pH < 9: ch th co mau tm


Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 44 -

pH > 9: ch th co mau xanh tm


Tuy theo nhng kim loai khac nhau ma phc tao thanh gia ch th nay vi ion
kim loai se co mau khac nhau, chang han ch th nay se tao vi Ca2+ mot phc co
mau o, vi Co2+, Ni2+, Cu2+ se tao phc co mau vang. V vay e tao s chuyen
mau tng phan th khi chuan Ca2+ bang complexon III vi ch th murexit nen
tien hanh moi trng pH > 9 th se ket thuc chuan o khi dung dch chuyen t o
sang xanh tm, oi khi tien hanh nhng pH = 9 se chuyen t mau o sang tm.
Khi chuan Co2+, Ni2+ , Cu2+ th tien hanh moi trng pH < 9 (cu the t 7 8) th
ket thuc chuan o khi dung dch chuyen t vang sang tm.
c. Xylenol cam :
Viet tat la H6Ind
H6Ind

H5Ind-

H4Ind2-

Cam

Vang

Vang

H3Ind3-

H2Ind4-

Vang

HInd5-

o tm

Ind6-

Tm

Cham

pH t 1 en 6 chat ch th co mau vang. Hau het phc cua kim loai vi ch th


nay co mau o hoac tm. V vay phep chuan o complexon vi ch th nay thng
c tien hanh pH trong khoang t 1 en 6.
d. PAN:
Viet tat la H2Ind+
Trong khoang pH kha rong (t 1 en 6) chat ch th t do co mau vang trong khi
o phc cua kim loai vi ch th co mau o hoac hong. V vay phep chuan o
complexon vi ch th nay thng c tien hanh pH trong khoang t 1 en 6.
e. PAR:
Viet tat la H3Ind+
Trong khoang pH kha rong (t 1 en 11,5) chat ch th t do co mau vang trong
khi o phc cua kim loai vi ch th co mau o hoac o nho.
II. Thc hanh:

1. Xac nh nong o Mg2+ :


a. Nguyen tac :
Dung dung dch complexon III co nong o chnh xac chuan o dung dch Mg2+
pH = 10, dung eriocrom T en lam ch th :
Mg2+ + HInd2MgInd- + H2Y2-

MgInd- + H+
MgY2- + HInd2- + H+

o nho
b. Cach tien hanh :

xanh

Dung pipet lay 10 ml dung dch Mg2+ can xac nh vao bnh non 250 ml. Them
vao o 1,5 ml dung dch em NH4Cl - NH4OH, 1 hat au ch th Eriocrom T en
(theo t le NaCl: Eriocrom T en la 100:1). Lac eu dung dch co mau o nho. T
Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 45 -

buret nho tng giot dung dch Complexon III co nong o a biet en khi dung dch
chuyen sang mau xanh biec. Ghi so ml dung dch complexon III a dung (lam 3
lan, lay ket qua trung bnh).
2. Xac nh Zn2+ :
a. Vi ch th Eriocrom T en: Tng t bai xac nh nong o Mg2+.
b. Vi ch th Xylenol cam
Nguyen tac:
Chuan o trc tiep Zn 2+ bang dung dch ComplexonIII vi ch th Xylenol da
cam tai moi trng em acetat ( pH = 5):
Zn2+

H2Ind4 -

ZnH2Ind2- + H2Y2-

ZnH2Ind2ZnY2-

o tm

H3Ind 3-

H+

vang chanh

Cach tien hanh:


Dung pipet lay 10 mL dung dch Zn2+ vao bnh tam giac 250 ml, them vao 2 ml
em acetat (pH = 5), 2 3 giot ch th Xylenol cam 1%. Chuan o bang dung dch
Complexon III ti khi dung dch chuyen mau t o tm sang vang chanh (lam 3
lan, lay ket qua trung bnh).
3. Xac nh nong o Pb2+ :
a. Vi ch th Xylenol cam:
Nguyen tac:
Chuan o trc tiep Pb2+ bang dung dch ComplexonIII vi ch th Xylenol cam
tai moi trng em acetat (pH = 5):
Pb2+

H2Ind4-

PbH2Ind4- + H2Y2-

PbH2Ind2PbY2-

o tm

H3Ind3-

H+

vang chanh

Cach tien hanh:


Dung pipet lay 10 ml dung dch Pb2+ vao bnh tam giac 250 ml, them vao 2ml
em acetat (pH = 5), 2 3 giot ch th Xylenol cam 1%. Chuan o bang dung dch
ComplexonIII ti khi dung dch chuyen mau t o tm sang vang chanh (lam 3 lan,
lay ket qua trung bnh).
b. Vi ch th Eriocrom T en:
Nguyen tac:
Viec chuan o bang complexon III phai tien hanh trong moi trng kiem.
Nhng moi trng kiem ch ket tua, can cho vao muoi cua axit tactric KNaC4H4O6
hoac triethanolamin N(OH2CH2OH)3, nhng trong ieu kien nay s chuyen mau
cua chat ch th Eriocrom T en iem tng ng khong ro.
Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 46 -

Ngi ta thng dung phng phap chuan ngc hoac thay ch bang complexon
Zn hoac Mg nh sau:
Cach tien hanh:
- Chuan o ngc :
Dung pipet lay 10 ml dung dch Pb2+ can xac nh vao bnh non 250 ml.
Them chnh xac 1 lng d complexon III co nong o a biet. Lac eu, them 5 ml
hon hp em NH4Cl - NH4OH, 1 hat au chat ch th Eriocrom T en trong NaCl.
T buret nho tng giot dung dch Zn2+ co nong o a biet ti khi dung dch
chuyen t mau xanh biec en o nho. Ghi so ml dung dch Zn2+ a dung (lam 3 lan
roi lay ket qua trung bnh).
- Chuan o thay the :
Dung pipet lay 10 ml dung dch Zn2+ vao bnh non 250 ml va tien hanh chuan
o nh bai 2 , ta c complexonat Zn. Lay chnh xac bang pipet 10 ml dung dch
Pb2+ can xac nh vao bnh non ng complexonat Zn (ZnY2-) . Lac ky , trong dung
dch se xay ra phan ng :
ZnY2- + Pb2+

PbY2- + Zn2+

T buret nho tng giot dung dch complexon III xuong, lng Zn2+ b ay ra
theo phan ng tren ti khi dung dch oi mau t o nho sanh xanh biec. T o suy
ra lng Pb2+ c xac nh. Ghi so ml dung dch complexon III a dung (lam 3
lan, lay ket qua trung bnh).
4. Xac nh nong o Ca2+ :
a. Vi ch th Murexid:
Nguyen tac :
Chuan o Ca2+ bang EDTA vi ch th Murexid pH = 12.
Ca2+ +H4IndCaH2Ind- + H2Y2-

CaH2Ind- + 2H+
CaY2- + H4Ind-

tm hong

Cach tien hanh :


Dung pipet lay 10 ml dung dch Ca2+ can nh phan vao bnh non 250 ml pha
loang gap oi the tch bang nc cat, them 0,5 ml NaOH 1N va 1 hat au ch th
murexid trong NaCl (1%). Dung dch co mau o. T buret nho tng giot dung dch
Complexon III co nong o xac nh ti khi dung dch chuyen t o sang tm. Ghi
so ml dung dch Complexon III a dung (lam 3 lan, lay ket qua trung bnh).
b. Vi ch th Fluorexon:
Nguyen tac:

Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 47 -

Chuan o mot the tch chnh xac Ca 2+ bang dung dch ComplexonIII trong moi
trng KOH co pH # 12 vi ch th Fluorexon.
Ca 2+

H6Ind

CaInd4- + H2Y2-

CaInd4- +
CaInd2-

phat huynh quang

6H+
+

HInd5- + H+

khong phat huynh quang

mau xanh luc

co mau hong

Cach tien hanh:


Dung pipet lay 10 ml dung dch Ca2+ can xac nh cho vao bnh tam giac 250
ml, them 0,5 ml KOH 1N, lac eu, mot hat au ch th Fluorexon 1%. Chuan o
bang dung dch ComplexonIII cho en khi tat mau huynh quang( lam 3 lan, lay ket
qua trung bnh).
5. Xac nh nong o Cu2+ :
a. Vi ch th Murexid:
Nguyentac:
Chuan o Cu2+ bang dung dch ComplexonIII vi ch th Murexid trong moi
trng em amoniac co pH = 8.
Cu 2+

H4Ind-

CuH2Ind- +

H2Y2-

CuH2Ind- +
CuY2-

cam

2H+
H4Indtm hong

Cach tien hanh :


Dung pipet lay 10 ml dung dch Cu2+ can xac nh vao bnh non 250 ml. Them 1
ml NH4Cl 1M + 1 hat au ch th Murexid. Them t t tng giot dung dch
NH4OH 1M en khi xuat hien mau vang . Sau o chuan o bang dung dch
ComplexonIII en khi dung dch chuyen t mau vang sang tm hong (lam 3 lan,
lay ket qua trung bnh).
b. Vi ch th Xylenol cam: tng t bai xac nh nong o Zn2+ vi ch th Xylenol
cam.
6. Xac nh Ca2+ nong o thap khi co them MgY2-:
Nguyen tac:
Khi nong o ban au C0 cua Ca 2+ tng oi ln ( > 0.001M) ta co the chuan o
Ca 2+ bang dungdch Complexon III hoan toan tng t nh khi chuan o Mg 2+:
dung em amoniac co pH = 10 va ch th Eriocrom T en.
Tuy nhien, khi C0 cang thap (< 0,001M) th s chuyen mau cua ch th Eriocrom
T en cang xay ra sm hn va iem cuoi chuan o cang nam ngoai khoang bc
nhay. o la v khi C0 cang nho th khoang bc nhay pCa cang thu hep va iem
au cua bc nhay pCa cang cao len, trong khi pCacuoi oi vi ch th Eriocrom T
en th hau nh co nh neu phan ng chuan o van gi nguyen ieu kien pH.
Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 48 -

Tnh trang tren co the khac phuc bang cach khi chuan o Ca2+ nong o thap ta
cho them mot lng nhat nh MgY2-, khi o, trc iem tng ng cua phep
chuan o Ca 2+ ta quan sat thay s pha huy CaInd- (mau hong nhat) e tao thanh
phc MgInd- ben hn (mau o nho manh). S tao thanh MgInd- c giai thch
bang s chuyen dch ang ke cua can bang phan ng sau:
CaInd- +
pK

MgY 2-

5,4

MgInd- +

8,7

7,0

CaY 2-

(1)

10,7

lgKcan bang = 17,7 14,1 = 3,6


Sau iem tng ng cua phep chuan o Ca2+, khi Ca2+ a chuan o het, th
vi mot giot ComplexonIII d lap tc xay ra phan ng ch th sau:
MgInd- + H2Y2-

MgY2- + HInd2-

o nho

(2)

xanh cham

Vay lng MgY2- b mat i trong phan ng (1) (trc iem tng ng) lai
c hoan tra lai trong phan ng (2) (sau iem tng mg).
Cach tien hanh:
- ieu che MgY2- ngay trong dung dch chuan o.
Lay 2 ml dung dch Mg2+ (# 0,001M) cho vao bnh tam giac 250 ml, them 10 ml
em amoniac pH = 10, mot hat au ch th Eriocrom T en, lac eu dung dch.
Chuan o bang dung dch ComplexonIII 0,001M en chuyen mau ro ret t o nho
sang xanh cham. Ghi the tch V1. Tuyet oi khong cho d dung dch ComplexonIII
Nap them dung dch ComplexonIII en vach khong cua buret . Them 10 ml
dung dch cha Ca2+( co nong o t 0,0001 en 0,001M) vao bnh tam giac va
ieu che MgY2-.Mau lap tc bien tr lai o nho; chuan o cho ti khi chuyen sang
mau xanh biec, ghi the tch V2 a cho tieu ton cho chuan o Ca2+ (lam 3 lan, lay
ket qua trung bnh cuaV1 va V2 ) .
7. Xac nh nong o Fe3 + vi ch th acid sulfosalicylic:
Nguyen tac:
Dung dung dch ComplexonIII xac nh Fe3+ trong moi trng co pH = 2 vi
acid sulfosalicylic lam ch th.
Fe3+

+ H2Sal

Fe(sal)+ + H2Y2tm o

Fe(sal)+
FeY-

2H+

+
+

H2Sal

vang nhat

Cach tien hanh:


Dung pipet lay 10 mL dung dch Fe3+ can xac nh cho vao bnh non 250 mL,
them 4 giot acid sulfisalicylic 25%. Neu dung dch khong co mau tm th them tng
giot CH3COOH ti xuat hien mau tm o. un nong en 700C, roi t buret nho

Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

- 49 -

tng giot dung dch ComplexonIII, lac eu en mat mau tm o cua dung dch (lam
3 lan, lay ket qua trung bnh).
8. Phan tch mau: Xac nh so gam Ca2+ ; so gam Mg2+ trong mot lt dung dch
mau ban au (theo hng dan cua phong th nghiem).
III. Cau hoi:

1. The nao la phng phap chuan o trc tiep, chuan o ngc, chuan o thay
the. Neu v du minh hoa. Giai thch c che oi mau, lap cong thc tnh nong o
ng lng cua cac dung dch trong cac v du minh hoa.
2. Giai thch c che oi mau khi chuan o ion Mg2+ bang dung dch Complexon
III dung Eriocrom T en lam ch th.
Tai sao phai dung hon hp em amoniac- amoni trong phep chuan o tren ?
3. Tai sao ch th Eriocrom T en ch dung cho phep chuan o Complexon trong
khoang pH t 7 en 11 ?
4. Giai thch c che oi mau cua cac ch th (Murexid, Fluorescein, Xylenol cam)
trong cac bai th nghiem.
5. Tnh nong o ng lng cua cac chat trong bai thc tap.
6. Tnh so gam canxi va so gam magie trong mot lt dung dch mau phong th
nghiem.

Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

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TAI LIEU THAM KHAO


1- PGS Cu Thanh Long, GVC Vu c Vinh. Hng dan thc hanh phan tch nh
lng bang cac phng phap hoa hoc ket hp vi phng phap x ly thong ke hien
ai. Tu sach trng ai hoc khoa hoc t nhien t/p Ho Ch Minh, 1998.
2- Nguyen Thac Cat, T Vong Nghi, ao hu Vinh. C s ly thuyet hoa hoc phan
tch, NXB Gao Duc 1996.
3- Le Xuan Mai, Nguyen Bach Tuyet. Giao trnh phan tch nh lng. Tu sach
trng ai hoc bach khoa t/p Ho Ch Minh, 1996.
4- A.P. Creskov. C s hoa hoc phan tch tap 2. NXBH & THCN Ha noi, 1990.
5- Nguyen Tinh Dung. Hoa hoc phan tch (Phan III). NXB Giao duc, Ha noi,
2000.
6- H. A. Latine. Phan tch hoa hoc tap 2, NXB khoa hoc va ky thuat Ha noi, 1976.
7- Daniel C. Harris- Quantitative chemical analysis. W. H. Freeman and CompanyNewYork- 1995
8- David Harvey - Modern Analytical chemistry, the McGraw- Hill Companies,
Inc- Singapore- 2000.

Nguyen Th Nh Mai ang Th Vnh Hoa

Khoa Hoa hoc

HDTH Phan tch nh lng bang cac phng phap hoa hoc

-1-

MUC LUC
Phan th 1. GII THIEU VE PHAN TCH NH LNG ................................... 4
I. Phan loai cac phng phap phan tch nh lng: ............................................... 4
ii. Cach tnh ket qua trong phan tch the tch: ......................................................... 5
iii. Cach ieu che dung dch chuan .......................................................................... 6
Phan th 2. GII THIEU CAC BAI THC TAP .................................................... 8
Bai 1. CACH S DUNG CAC DUNG CU O KHOI LNG VA THE TCH ........ 8
I. o khoi lng:....................................................................................................... 8
II. o the tch............................................................................................................ 9
III. Thc hanh: ........................................................................................................ 12
Bai 2. PHNG PHAP TRUNG HOA (PHNG PHAP CHUAN O ACID
BAZ).......................................................................................................................... 13
I. Tom tat ly thuyet: ............................................................................................... 13
II. Thc hanh: ......................................................................................................... 15
III. Cau hoi:............................................................................................................. 17
Bai 3. PHNG PHAP TRUNG HOA ..................................................................... 18
I. Thc hanh ............................................................................................................ 18
II. Cau hoi:............................................................................................................. 21
Bai 4. PHNG PHAP OXY HOA KH PHEP O PERMANGANAT ........... 22
I. Tom tat ly thuyet: ............................................................................................... 22
II. Thc hanh: ......................................................................................................... 26
III. Cau hoi:............................................................................................................. 27
Bai 5. PHNG PHAP OXY HOA KH PHEP O DICROMAT VA IOD ............ 29
I. Thc hanh:........................................................................................................... 29
II. Cau hoi:.............................................................................................................. 31
Bai 6. PHNG PHAP CHUAN O KET TUA ...................................................... 33
I. Tom tat ly thuyet: ............................................................................................... 33
II. Thc hanh: ......................................................................................................... 36
III. Cau hoi:............................................................................................................. 37
Bai 7. PHNG PHAP PHAN TCH KHOI LNG ............................................. 39
I. Thc hanh:........................................................................................................... 39
II. Cau hoi:.............................................................................................................. 41
Bai 8. PHNG PHAP COMPLEXON ................................................................... 42
I. Tom tat ly thuyet: ............................................................................................... 42
II. Thc hanh: ......................................................................................................... 44
III. Cau hoi:............................................................................................................. 49

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