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31 PT Dinhluongbang HH
31 PT Dinhluongbang HH
F7G
HDTH Phan tch nh lng bang cac phng phap hoa hoc
-2-
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
HDTH Phan tch nh lng bang cac phng phap hoa hoc
-3-
HDTH Phan tch nh lng bang cac phng phap hoa hoc
-4-
HDTH Phan tch nh lng bang cac phng phap hoa hoc
-5-
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
m =
X
VR .C N ,R . X
1000
mX =
VR .C N ,R . V
.
1000
V0
HDTH Phan tch nh lng bang cac phng phap hoa hoc
-6-
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
C =
N
a
.V
a.1000
.V
HDTH Phan tch nh lng bang cac phng phap hoa hoc
-7-
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.
HDTH Phan tch nh lng bang cac phng phap hoa hoc
-8-
Can ky thuat
< 1000g
> 10g
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
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
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.
HDTH Phan tch nh lng bang cac phng phap hoa hoc
- 10 -
HDTH Phan tch nh lng bang cac phng phap hoa hoc
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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
HDTH Phan tch nh lng bang cac phng phap hoa hoc
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- 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.
HDTH Phan tch nh lng bang cac phng phap hoa hoc
- 13 -
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
3,1 - 4,4
4,0
Vang
4,4 - 6,2
5.5
Vang
8,0 - 9,9
9,0
Khong mau
Tm hong
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
3,9 - 4,3
4,1
Ty le the tch A : B = 1: 1
Tm - luc
4,3
4,9 - 5,3
5,1
o nho - luc
5,2 - 5,6
5,4
o nho - luc
5,9 - 6,3
6,1
Luc vang - tm
cham
7,0 - 7,4
7,2
Hong - luc
7,3 - 7,7
Vang - Tm
7,5
HDTH Phan tch nh lng bang cac phng phap hoa hoc
- 15 -
8,1 - 8,5
8,3
Vang - Tm
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:
HDTH Phan tch nh lng bang cac phng phap hoa hoc
- 16 -
Nac II
phenolphtalein
NaH2PO4
NaOH
Na2HPO4
ch th metyl da cam
+
H2O
ch th
H3PO4 +
NaOH
NaH2PO4
H2O
Luon en nac II
H3PO4 + 2 NaOH =
Na2HPO4
2H2O
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:
HDTH Phan tch nh lng bang cac phng phap hoa hoc
- 18 -
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).
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
Na2CO3 +
HCl
HCl
NaCl
H2O
NaCl
+ CO2
H2O
NaHCO3 + NaCl
NaCl
H2O
CO2
HDTH Phan tch nh lng bang cac phng phap hoa hoc
- 20 -
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- +
Vb
2VI - VII =
Va
+ 2Vb
Va
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
HDTH Phan tch nh lng bang cac phng phap hoa hoc
- 22 -
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
HDTH Phan tch nh lng bang cac phng phap hoa hoc
NH
NH
NH
-2e-
- 23 -
2H
Eo = 0,76V
NH
SO3Na
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.
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
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+
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
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-
+ I2 + H2O
H2S + I2
Sn2+ + I2
I2
Na2S4O6 +
2NaI
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
Nguyen Th Nh Mai ang Th Vnh Hoa
HDTH Phan tch nh lng bang cac phng phap hoa hoc
- 26 -
- 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:
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
HDTH Phan tch nh lng bang cac phng phap hoa hoc
- 27 -
Mn2+ + 4H2O
Fe3+
5Fe2+ + MnO4- + 8H +
* 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
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.
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.
HDTH Phan tch nh lng bang cac phng phap hoa hoc
- 29 -
I. Thc hanh:
2Cr3+ + 7H2O
Fe2+ - e
Cr2O72- + 6Fe2+ + 14H+
Fe3+
2Cr3+ + 6Fe3+ + 7H2O
HDTH Phan tch nh lng bang cac phng phap hoa hoc
- 30 -
Cr2O72- + 9 I- + 14H+
Phan ng chuan o:
I3- + 2S2O32-
3 I- + S4O62-
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-
HDTH Phan tch nh lng bang cac phng phap hoa hoc
- 31 -
3I3- + 3H2O
Phan ng chuan o:
I3- + 2 S2O32-
3 I- + S4O62-
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
HDTH Phan tch nh lng bang cac phng phap hoa hoc
- 33 -
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)
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
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-
AgOH
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:
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
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+ .
HDTH Phan tch nh lng bang cac phng phap hoa hoc
- 36 -
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+
HDTH Phan tch nh lng bang cac phng phap hoa hoc
- 37 -
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]
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
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.
HDTH Phan tch nh lng bang cac phng phap hoa hoc
- 39 -
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
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
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
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+
- 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.
HDTH Phan tch nh lng bang cac phng phap hoa hoc
- 42 -
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+
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
HDTH Phan tch nh lng bang cac phng phap hoa hoc
- 44 -
H5Ind-
H4Ind2-
Cam
Vang
Vang
H3Ind3-
H2Ind4-
Vang
HInd5-
o tm
Ind6-
Tm
Cham
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
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
H2Ind4-
PbH2Ind4- + H2Y2-
PbH2Ind2PbY2-
o tm
H3Ind3-
H+
vang chanh
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
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-
6H+
+
HInd5- + H+
co mau hong
H4Ind-
CuH2Ind- +
H2Y2-
CuH2Ind- +
CuY2-
cam
2H+
H4Indtm hong
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
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
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.
HDTH Phan tch nh lng bang cac phng phap hoa hoc
- 50 -
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