Gio trnh Th nghim Ha Phn Tch

NI QUY MN HC TH NGHIM HA PHN TCH

1. Trc buoi thc tap (chuan b nha): xem ky noi dung bai thc tap e nam vng
nguyen tac, cach tnh toan va cach thc hien moi th nghiem trong bai.
2. en phong th nghiem ung gi quy nh, nop ay u bai tng trnh cho giao vien
hng dan ngay sau buoi th nghiem.
3. Nghe va thc hien ung cac ch dan cu the cua giao vien ve bai thc hanh trc
khi tien hanh th nghiem
4. ng ung cho th nghiem quy nh. Kiem tra ngay cac dung cu, neu thieu hoac
hong th bao cao ngay cho giao vien.
5. Co thai o nghiem tuc khoa hoc trong buoi th nghiem: ghi chep ket qua o ro rang,
ay u, trung thc. Gi sach se, gon gang cho th nghiem. Khong t y di chuyen
cac hoa chat ch thdung chung cho ca phong th nghiem.
6. Chu y ren luyen ky nang thc hanh phan tch nh lng: o chnh xac khoi lng
va the tch, cach nhan ung iem cuoi chuan o, cach bao quan dung dch chuan,
ky thuat loc ra, say nung ket tua
7. Trc khi ra ve ra ngay cac dung cu thuy tinh va trang nc cat can than, sap xep
lai gon gang va bao cao vi giao vien.
8. Theo quy nh hien hanh, sinh vien khong c phep d thi hoc phan THC
HANH PHAN TCH NH LNG neu vang qua hai buoi thc tap.

Gio trnh Th nghim Ha Phn Tch

BI 1:

CH DAN CHUNG VE THC HANH HOA PHAN TCH

1.1. i tng, nhim v ca phn tch nh lng

Chn mu i din (chn mt phn nh mu i din cho ton b i tng cn phn
tch), cng vic ny cn phi c quy hoch trc.
Chuyn cht phn tch v dng dung dch: ha tan hon ton mu trong dung mi thch
hp, tin hnh phn tch theo phng php chn. Nu phn tch bng mt s phng
php vt l th c th khng cn ha tan mu nhng cn phi x l ha hc trc.
Tin hnh phn tch theo phng php chn.
Tnh kt qu (nh gi kt qu v chnh xc phn tch).
1.2. Cc phng php phn tch
Phng php phn tch khi lng: Da vo vic cn sn phm to thnh sau qu trnh
thc hin phn ng to kt ta t xc nh hm lng cu t cn phn tch.
Phng php phn tch th tch: Da vo vic o chnh xc th tch dung dch thuc
th c nng chnh xc tnh hm lng cu t cn phn tch.
Cc phng php vt l: Da trn vic o mt tnh cht vt l no ( hp th nh
sng, dn in, in th, cng dng, cng bc x in t,...) m tnh cht ny l
hm lng ca khi lng hoc ca nng ca cu t cn phn tch.
1.3. Biu din kt qu trong phn tch nh lng
1.3.1. Biu din ha hc
Biu din cu t phn tch theo dng tn ti ca n trong cht phn tch. V d: Cr3+,
Cr2O7, CrO4
Biu din cu t phn tch di dng nguyn t hoc di dng oxit thng p dng
i vi cc hp cht cha bit chnh xc thnh phn hoc khi khng cn xc nh trc tip
thnh phn. V d: i vi mu v c phc tp cha oxi ngi ta thng biu din cc
nguyn t di dng oxit: Fe Fe3O4, Si SiO2,
1.3.2. Biu din nng phn trm khi lng (%)
Hm lng cu t c trong mu phn tch thng c biu din theo phn trm khi
lng cu t trong mu:

q%

khoiluongcautucanphantich
.100%
khoiluongmau
2

Gio trnh Th nghim Ha Phn Tch

T l phn trm v khi lng thng c dng biu din nng . N c xc
nh nh sau:

Khi lng ca dung dch (trong trng hp n gin ch c mt dung mi v mt

cht tan) s l:

mdung dch = mcht tan + mdung mi

Do vy chng ta c th vit li cng thc ca nng phn trm khi lng nh sau:

C% w / w

mchat tan
.100%
mdungmoi mchat tan

1.3.3. Nng phn trm khi lng th tch

V d: mt dung dch cha 5g cht tan trong 100ml dung dch th dung dch ny c nng
l 5%w/v.
1.3.4. Nng phn trm v th tch

V d: Ru vang c nng l 12% v/v etanol, iu ny c ngha l trong mi 100ml ru

vang s c 12 ml etanol.
1.3.5. Nng Phn t gam
Nng phn t gam hay nng mol th tch (nng mol) thng c biu th
bng M, c xc nh nh sau:

CM

n chat tan
V dungdich

1.3.6. Nng chun

Nng chun (hay nng ng lng ) cng tng t nh nng mol nhng
dng ng lng thay cho mol cht tan trong dung dch. N biu th s ng lng trong

Gio trnh Th nghim Ha Phn Tch

mt lt. Do vy vi cng mt dung dch c th c nhiu nng ng lng cho cc loi
phn ng khc nhau.
V d: Dung dch axt sulfuric 1M s c nng ng lng 2N cho phn ng
axt/baz nhng ch l 1N trong phn ng to ta BaSO4 . tnh ton nng ng
lng ca mt dung dch no bn cn bit chnh xc nng mol ca n cng nh h s
t lng ca cc cht phn ng c dng.
chuyn i nng ng lng sang cc dng nng khc th trc ht bn
phi tm c nng mol ca n. Nng chun c n v l [ng lng/L].
1.3.7. Nng mol khi lng
Nng mol khi lng c xc nh nh sau:

Cm

n chat tan
m dungmoi

1.3.8. Phn mol

Phn mol c nh ngha l t s ca s mol mt cht trn tng s mol ca tt c cc
cht.
V d: Mt dung dch cha 10 mol etanol trn mi 1000g nc. M 1000g nc c
55.51 mol nc do vy phn mol ca etanol l: 10/(55.51+10) = 0.1527. Phn mol khng
ph thuc vo nhit.
Phn mol c th dng cho hn hp ca bt k cc cht, phn mol c gi tr cc i
lun l 1 v tng tt c phn mol ca cc cht trong hn hp bng 1.
chuyn phn mol sang cc dng nng khc, cn bit khi lng ca dung mi
v cht tan, phn mol khng c n v.

Gio trnh Th nghim Ha Phn Tch

CHUAN O ACID- BAZ

BAI 2:

2.1. Chun NaOH bng HCl 0,050N

2.1.1. Nguyn tc
2.1.1.1. Phn ng chun
H+ + OH- H2O
pH tng ng 7
2.1.1.2. nh im cui
- Dung chat ch th pH
Tuy nong o dung dch, tuy o chnh xac, chon ch th thch hp, thng dung
phenolphtalein, pH chuyen mau 8,2 10 (khong mau hong)
- Dng my o pH
2.1.2. Thc nghim
2.1.2.1. Ha cht
- Dung dch acid chuan C = 0,050N
- Dung dch ch th phenolphtalein 0,1% / Etanol 60%
2.1.2.2. Dng cht ch th
- Buret: Dung dch acid chuan
- Erlen: Hut V ml baz + t nc cat trang thanh bnh + vai giot phenolphtalein.
- Mau dung dch iem cuoi: o hong khong mau.
2.1.3. Ket qua: Tnh nong o ng lng, nong o mol hay nong o khoi lng cua
dung dch khao sat.
2.2. Chuan o dung dch Na2CO3 bang dung dch HCl hay H2SO4
2.2.1. Nguyn tc
2.2.1.1. Phn ng chun
H+ + CO32- HCO3-

Ka1 = 10-6,35

H+ + HCO3-

Ka2 = 10-10,32

2.2.1.2. nh im cui
- Dung chat ch th:
5

Gio trnh Th nghim Ha Phn Tch

+ iem tng ng (1) pH = (p Ka1 + p Ka2) = 8,21
+ iem tng ng (2) pH khong 4 ty thuc nng H2CO3 trong dung
dch
Do o co the nh iem cuoi bang hai ch th:
* Phenol phtalein.
* Metyl da cam chuyn mau 3,1 4,4 ( cam)
Dng my o pH: V ng biu din pH.
2.2.2. Thc nghim
2.2.2.1. Ha cht
- Dung dch chuan HCl
- Dung dch ch th Metyl da cam 0,1%/ nc
- Phenol phtalein 0,1%/ Etanol 60%
2.2.2.2. Cch tin hnh
* Dung chat ch th:
- Buret: dung dch chuan HCl hoc H2SO4
- Erlen: hut V ml dung dch mau Na2CO3 + t nc cat trang thanh bnh + vai giot
ch th Phenol phtalein
- Mau dung dch iem cuoi 1: hng khng mu
Them tiep vai giot ch th nh im cui 2; chuan o tiep n i mu ch th
* Dung my o pH:
- Buret: Dung dch chun HCl
- Becher 250ml: Ht V ml dung dch mu Na2CO3 + t nc cat n khong 100ml.
Ghi pH trong qu trnh chun
2.2.3. Kt qu
Tnh nng khi lng ca Na2CO3 trong mu. Nu mu c cha thm hoc NaOH
hoc NaHCO3, tnh nng khi lng ca tng hp cht trong mu.

Gio trnh Th nghim Ha Phn Tch

NH LNG ION Cl- TRONG DUNG DCH

BAI 3:

3.1. Chuan o dung dch Cl- theo phng phap Morh (chuan o trc tiep)
3.1.1. Nguyn tc
3.1.1.1. Phn ng chun
Dung dung dch chuan AgNO3:
Ag+ + Cl- AgCl

T AgCl = 10-9,75

ac iem:
- Tua AgCl mau trang, ben trong moi trng acid, tan trong moi trng NH4OH do
can bang tao phc tao Ag(NH3)2+
- Moi trng can co pH < 10 e tranh can bang phu:
2 Ag+ + 2 OH- 2AgOH Ag2O + H2O

T AgOH = 10-7,8

- Neu trong dung dch co NH4+, can chuan o pH < 8 e tranh can bang tao phc
lam tan tua AgCl.
- Co s hap phu cua tua AgCl len cac ion Ag+ va Cl- de gay sai so.
- Can loai nhng ion khac co kha nang tao tua ben vng vi Ag+ nh I-, Br-, SCN-.
- Phep chuan o thch hp vi nong o Cl- trong khoang 10-3 10-2M (sai so < 1%)
3.1.1.2. nh im cui
Dung chat ch th tao tua K2CrO4:
2Ag+ + CrO42- Ag2CrO4
ac iem:
- Tua Ag2CrO4 mau o nau, tan nhiet o cao.
- Moi trng can co pH > 6 e tranh can bang phu:
Ag2CrO4 2 Ag+ + CrO42+
H+

HCrO47

T Ag2CrO4 = 10-11,95

Gio trnh Th nghim Ha Phn Tch

Do o, neu dung dch co NH4+, tot nhat nen chuan o moi trng pH = 7 8. Co
the tao ieu kien nay bang cach them vao dung dch lng NaHCO3 hay Na2B4O7
- Lng ch th can dung thch hp e iem cuoi gan vi iem tng ng. Trong
thc nghiem, e de quan sat iem cuoi, tai thi iem nay, nong o cau t can co tr so:
+ Nong o CrO42- trong tua Ag2CrO4 khoang 10-5M
+ Nong o CrO42- con dang t do 10-4 5. 10-3M
- Can loai nhng ion co kha nang tao tua vi CrO42- nh Ba2+, Pb2+
3.1.2. Thc nghim
3.1.2.1. Ha cht
- Dung dch AgNO3

C = 0,040N

- NaHCO3 hay Na2B4O7 ran

- Dung dch ch th K2CrO4 10% / nc
- Buret: dung dch chuan AgNO3
3.1.2.2. Cch tin hnh
- Erlen: hut V ml dung dch mau Cl- + t nc cat trang thanh bnh, kiem pH dung
dch bang giay pH. Neu can, dung NaHCO3 hay Na2B4O7 ieu chnh en pH thch hp +
V ml dung dch ch th K2CrO4 10% tng ng vi khoang nong o tren.
- Dung dch iem cuoi: vang xuat hien tua o nau lam toan khoi dung dch co
mau vang anh hong.
3.1.3. Kt qu
- Neu mau long, nh nong o ng lng, nong o mol, nong o khoi lng cua
Cl- Neu mau ran, nh nong o phan tram cua NaCl trong mau.
3.2. Chuan o dung dch Cl- theo phng phap Charpentier Volhard (chuan o
ngc)
3.2.1. Nguyn tc
3.2.1.1. Phn ng chun
Them lng tha xac nh dung dch AgNO3 e tao tua AgCl.
Ag+ + Cl-

T AgCl = 10-9,75

AgCl
8

Gio trnh Th nghim Ha Phn Tch

nh lng Ag+ tha bang dung dch chuan KSCN (hay NH4SCN)
SCN- + Ag+ AgSCN

T AgSCN = 10-11,97

(mau trang)
3.2.1.2. nh im cui
Dung ch th tao phc phen sat ba; phan ng ch th trong moi trng pH < 2 vi
lng nho SCN- :

SCN- + Fe3+ FeSCN2+

SCN
FeSCN

ac iem:
- Tao moi trng acid e tranh viec tao tua Fe(OH)3, thng dung HNO3 vi {H+}
0,3M
- Do T AgCl < T AgSCN nen gan iem tng ng co the co can bang phu:
AgCl

Ag+ + Cl-

+
SCN-

FeSCN2+

AgSCN

AgSCN + Fe3+

Loai can bang phu nay bang cach loai hay co lap tua AgCl, co the dung bien phap:
+ Loc bo tua AgCl khoi dung dch trc khi chuan o.
+ un soi dung dch vai phut trc khi chuan o.
+ Them dung moi hu c khong tron lan vi nc nh nitrobenzen e bao tua lai
bang cach lac that manh dung dch trc khi chuan o.
- Phc FeSCN2+ co mau o. ieu kien e mau xuat hien ro la{FeSCN2+} 7.10-6M
va {SCN-} > 3. 10-6M. Thc nghiem cho thay, e co s tao phc gan iem tng ng,
co the dung lng ch th vi nong o au trong dung dch chuan o = 0,2M (sai so
khoang 0,1%)
3.2.2. Thc nghim

Gio trnh Th nghim Ha Phn Tch

3.2.2.1. Ha cht
- Dung dch chuan AgNO3
- Dung dch chuan NH4SCN hay KSCN
- Dung dch HNO3 (11)
- Dung dch ch th phen sat ba bao hoa Fe(NH4)(SO4)2.12H2O ng vi nong o
1mol/l.
- Buret: dung dch chuan NH4SCN hay KSCN
3.2.2.2. Cch tin hnh
- Erlen: Hut V ml dung dch mau Cl- + t nc cat trang thanh bnh + 1 ml HNO3
(11) + lng tha xac nh dung dch chuan AgNO3 (tha khoang 50% so vi lng
can dung e tao tua AgCl). Loai anh hng can bang phu do AgCl bang cach:
+ Them 0,5 ml nitro benzen va lac manh dung dch.
+ Hoac un soi dung dch trong vai phut. Them lng thch hp ch th phen sat ba.
- Dung dch iem cuoi: khong mau co tua trang AgCl dung dch mau cam nhat
3.2.3. Kt qu
- Neu mau long, nh nong o ng lng, nong o mol, nong o khoi lng cua
Cl- Neu mau ran, nh nong o phan tram cua NaCl trong mau.

10

Gio trnh Th nghim Ha Phn Tch

BAI 4:

NH LNG DUNG DCH KMnO4 va Na2S2O3

4.1. Chuan o dung dch KMnO4 bang dung dch acid oxalic (H2C2O4)
4.1.1. Nguyn tc
4.1.1.1. Phn ng chun
- Trong moi trng acid:
2MnO4- + 5C2O42- + 16H+ 2Mn2+ + 10CO2 + 8H2O
EoMnO-4/Mn2+ = 1,51 V
Eo 2CO2 / C2O42- = -0,49 V
ac iem:
- Phan ng can thc hien trong moi trng acid, nhng do tnh kh manh cua
C2O42- nen ch tao moi trng bang H2SO4 trong dung dch loang.
- Phan ng ban au cham, nhng khi co Mn2+, ong vai tro xuc tac, phan ng xay
ra nhanh hn.
- Phan ng nhanh nhiet o khoang 60oC, nen can un dung dch trc khi chuan
o, nhng nhiet o cao hn, acid oxalic co the b phan huy cho ra CO2.
- Van toc phan ng cham, can pha loang dung dch chuan o va lac manh bnh khi
chuan o.
4.1.1.2. nh im cui
Chat ch th la chnh ngay dung dch KMnO4 vi lng tha ngay sau iem tng
ng tao dung dch co mau hong nhat ben 2 phut.
4.1.2. Thc nghim
4.1.2.1. Ha cht
- Dung dch chuan acid oxalic 0,050N
- Dung dch H2SO4 (1 : 5)
- Buret: dung dch mau KMnO4
4.1.2.2. Cch tin hnh

11

Gio trnh Th nghim Ha Phn Tch

Erlen: hut V ml dung dch chuan acid oxalic + khoang 50 ml nc + 5 ml dung dch
H2SO4. un nhe dung dch khoang 60oC.
- Mau dung dch iem cuoi: khong mau hong nhat ben 2 phut.
4.1.3. Kt qu
Tnh nong o ng lng, nong o mol cua dung dch KMnO4.
4.2. Chuan o dung dch Na2S2O3 bang dung dch K2Cr2O7 (chuan o gian tiep)
4.2.1. Nguyn tc
4.2.1.1. Phn ng chun
Trong moi trng acid, vi lng tha I- va lng xac nh dung dch Cr2O72chuan:
Cr2O72- + 9 I- + 14H+ 2Cr3+ + 3I-3 + 7H2O
EoCr2O72- /2Cr3+ = 1,33V
Eo I3-/3I- = 0,545 V
Lng I3- tao thanh c chuan o bang dung dch khao sat S2O32ac iem:
- Nong o H+ tang lam tang tnh nh lng cua can bang nhng cung lam I- de b
oxy hoa bi O2 trong khong kh. Moi trng thch hp vi {H+} = 0,2 0,4M. Co the
dung HCl, H2SO4.
- e phan ng hoan toan, can ieu kien {I-} 2% va e yen hon hp phan ng
ni toi 10 phut
4.2.1.2. nh im cui
Dung ch th ho tinh bot.
4.2.2. Thc nghim
4.2.2.1. Ha cht
- Dung dch chuan K2Cr2O7 0,050N
- Dung dch KI 10%/ nc
- Dung dch H2SO4 (1 : 5)
- Dung dch ch th ho tinh bot.
+ Buret: dung dch mau Na2S2O3.
12

Gio trnh Th nghim Ha Phn Tch

4.2.2.2. Cch tin hnh
+ Erlen: hut V ml dung dch chuan K2Cr2O7 + khoang 30 ml nc + 5 ml dung dch
H2SO4 + 5 ml KI.
Chuan o en dung dch co mau vang nhat, them vai giot ch th, dung dch co mau
xanh, chuan o en mat mau xanh cua ch th, dung dch co mau xanh xam nhat cua ion
Cr3+
Lu y: Phan thc nghiem rat de gap sai so do tnh de bay hi cua I2.
4.2.3. Kt qu
nh nong o ng lng cua dung dch Na2S2O3
Ghi chu: co the nh nong o I2 bang dung dch chuan K2Cr2O7 qua dung dch trung
gian Na2S2O3 vi 2 phep chuan o tren.

13

Gio trnh Th nghim Ha Phn Tch

BAI 5:

NH LNG ONG, SAT

5.1. Chuan o dung dch Cu2+ bang dung dch Na2S2O3 (chuan o gian tiep)
5.1.1. Nguyn tc
5.1.1.1. Phn ng chun
Trong moi trng hi acid vi lng tha I- :
2Cu2+ + 5I- 2CuI + I3--

TCuI = 10-11,96

EoCu2+/CuI = 0,86 V ; Eo I3-/3I- = 0,545V

Lng I3- tao thanh c chuan o bang dung dch Na2S2O3
ac iem:
- Can loai nhng ion co kha nang oxy hoa. Co the loai Fe3+ bang dang phc ben
FeF63- gan iem cuoi, e tranh hien tng I3- b hap phu tren be mat tua CuI, them
lng NH4 SCN e chuyen sang dang tua CuSCN, T CuSCN = 10 -14,32
5.1.1.2. nh im cui
Dung ch th ho tinh bot
5.1.2. Thc nghim
5.1.2.1. Ha cht
- Dung dch chuan Na2S2O3 0,050N
- Dung dch NH4SCN 10%/ nc
- Dung dch KI 10%/ nc.
- Dung dch NH4F 2%/ nc
- Dung dch ho tinh bt
5.1.2.2. Cch tin hnh
+ Buret: Dung dch chuan Na2S2O3.
+ Erlen: Hut V ml dung dch mau + khoang 30 ml nc (dung dch co pH6) + 2 ml
dung dch NH4F + 5 ml KI. Chuan o en dung dch co mau vang nhat + vai giot ch th,

14

Gio trnh Th nghim Ha Phn Tch

dung dch co mau xanh, chuan o en mau xanh ch th that nhat, them 2 ml dung dch
NH 4SCN, chuan o tiep en mat mau xanh.
5.1.3. Kt qu
Tnh nong o ng lng, nong o mol cua dung dch Cu2+ trong dung dch mau.
Tnh nong o khoi lng cua Cu trong dung dch mau dang CuSO4.5H2O.
5.2. Chuan o dung dch Fe2+ bang dung dch KMnO4
5.2.1. Nguyn tc
5.2.1.1. Phn ng chun : trong moi trng acid manh
MnO4- + 5 Fe2+ + 8H+ 2Mn2+ + 5Fe3+ + 4 H2O
EoMnO4-/Mn2+ = 1,51 V
EoFe3+/Fe2+

= 0,771 V

ac iem:
- Tao moi trng acid bang dung dch H2SO4, khong dung HCl
- Phan ng ban au cham, co Mn2+ ong vai tro xuc tac, phan ng nhanh hn.
5.2.1.2. nh im cui
Lng tha cua dung dch KMnO4 ngay sau iem tng ng lam dung dch co
mau hong nhat (ben 2 phut)
5.2.2. Thc nghim
5.2.2.1. Ha cht
- Dung dch chuan KMnO4 0,050 N
- Dung dch H2SO4 (1 : 5)
5.2.2.2. Cch tin hnh
+ Buret: dung dch chuan KMnO4
+ Erlen: hut V ml dung dch mau + khoang 30ml nc + 5 ml H2SO4
+ Mau dung dch iem cuoi : khong mau hong nhat ben 2 phut.
Lu y: co the ap dung phep chuan o nay e nh chuan dung dch KMnO4 bang
dung dch chuan Fe2+ c pha che t muoi Mohr Fe(NH4)2(SO4)2. 6H2O
5.2.3. Kt qu

15

Gio trnh Th nghim Ha Phn Tch

- Tnh nong o mol cua Fe2+ trong dung dch mau. Tnh ham lng % khoi lng
cua Fe dang Fe(NH4)2(SO4)26H2O trong mau ran

16

Gio trnh Th nghim Ha Phn Tch

BAI 6:

NH HAM LNG Fe3+ TRONG DUNG DCH

THEO PHNG PHAP KHOI LNG

6.1. Nguyen tac

Dung chat tao tua la NH4OH. Phan ng tao tua:
Fe3+ + 3OH- Fe(OH)3

T Fe(OH)3 = 10-37,5

Phan ng chuyen dang tua sang dang can khoang 800oC:

2 Fe(OH)3 Fe2O3 + 3H2O
1000oC dang can co the chuyen thanh Fe3O4
ac iem:
- Tua Fe(OH)3 dang vo nh hnh co mau nau r, tao trong moi trng co pH 3.
Neu trong mau co lan Al3+, tao tua pH 11. Do o, can tao tua trong ieu kien thch
hp: dung dch nong, am ac, them nhanh chat tao tua, them ngay dung dch chat ien
ly e giam hap phu. Loc sau khi tao tua 5 -10 phut.
- Tua c loc bang pheu thuy tinh va giay loc nh lng bang o (loai khong tro,
mong). Sau khi ra, tua c nung 800oC e chuyen sang dang can.
- Lng mau cho 1 lan tao tua c dung ng vi lng can khoang 0,1 0,2 gam.
6.2. Thc nghiem
6.2.1. Ha cht
- Dung dch NH4OH
- Dung dch NH4NO3 1%/nc.
- Dung dch AgNO3 1%/nc
6.2.2. Cch tin hnh
+ Becher 100 ml: Hut V ml dung dch mau hay m (g) mau a c hoa tan nh tren.
Neu dung dch mau co lan chat khong tan, phai loc lai. Neu dung dch mau , them
lng nc toi thieu e tang the tch dung dch ng vi lng cua dang tua vo nh hnh
c tao thanh.

17

Gio trnh Th nghim Ha Phn Tch

+ un gan soi dung dch, them tng giot dung dch NH4OH , khuay eu en dung
dch co mui ro, trong dung dch co tua mau nau r (neu dung dch mau co lan Al3+, can
tao tua moi trng co pH 11). Them ngay 50 ml dung dch NH4NO3 nong lam ong
tu tua va lam giam hap phu.
+ Loc tua qua giay loc mong, khong tro (giay bang o). Ra tua bang dung dch
NH4NO3 nong en het ion Cl- (kiem bang dung dch AgNO3, sau khi acid hoa dung dch
qua loc bang vai giot dung dch HNO3)
+ Goi tua, cho vao chen sanh (a nung 800oC va can). ot va nung tua 800oC
en khoi lng khong oi.
6.3. Ket qua
- Tnh nong o mol cua Fe3+ trong dung dch mau.
- Tnh ham lng % khoi lng cua Fe dang Fe2O3 trong mau ran.

18

Gio trnh Th nghim Ha Phn Tch

NH LNG ION Ca2+

Bi 7:

7.1. Nguyn tc
Dng dung dch C2O42- to ta vi dung dch Ca2+ theo phn ng
Ca2+ + C2O42- + H20 CaC2O4.H2O

T CaC2O4 = 10-8,64

c im:
- Ta CaC2O4.H2O c mu trng c, c th c cn dng CaC2O4.H2O sau khi
sy 100 1050C (kt qu thng b sai tha 0,5 1%)
- Dng cn cng c th l CaC2O4 nu nung ta CaC2O4.H2O 475 5250C hoc
CaO nu nung ta 12000C.
- Cc ion kim loi Ba2+, Cd2+, Pb2+,.... gy nh hng n kt qu xc nh Ca2+ do
cng to ta bn vi C2O42- Khng c to ta trong mi trng acid trnh s tan ta CaC2O4 (mi
trng thch hp c pH>=4)
- Thuc th nng, long c thm chm vo mu cha Ca2+ (cng nng. long),
khuy u thu c tinh th to.
- Sau khi to ta, yn dung dch to iu kin cho tinh th ht ta pht trin ln ln.
- Ta c lc v c chuyn sang dng cn vi phng tin v cch thc ph thuc
vo dng s c cn.
7.2. Thc nghim:
7.2.1. Ha cht
- Dung dch (NH4)2C2O4 5%/nc
- Dung dch (NH4)2C2O4 1%/nc
- Dung dch NH4OH (1:1)
- Dung dch ch th metyl 0,1%/etanol 60%
- Dung dch AgNO3 1%/nc
7.2.2. Cch tin hnh
To ta
- Becher 200 ml: Ht V(ml) dung dch mu Ca2+ ( lc b cn khng tan) + nc ct
n khong 70 ml. Thm vi git metyl . un dung dch va si. Thm chm 10-20 ml
dung dch (NH4)2C2O4 5% nng (va thm va khuy u). Trung ha dung dch bng tng
19

Gio trnh Th nghim Ha Phn Tch

git NH4OH (1:1) cho n khi dung dch chuyn t sang vng. yn dung dch (khng
un) t nht 1 gi.
Lc ta v nung ra ta:
Nu ta c cn dng CaC2O4.H2O hoc CaCO3: lc ta qua chung lc Gooch
hoc chung thy tinh c. Ra ta bng dung dch (NH4)2C2O4 1% nng t nht 5 ln cho
n khi dung dch qua lc khng cn Cl- (th bng AgNO3 sau khi acid ha dung dch qua
lc bng HNO3). Sy 100-1050C trong 1-2 gi. ngui trong bnh ht m , cn dng
CaC2O4.H2O.
Hoc chuyn chn cha ta vo l Muffle, nung 5000C trong 2 gi hoc cho n khi
khi lng khng i. ngui trong bnh ht m v cn dng CaCO3 ( phng ta
b chuyn i mt phn thnh CaO, lm m ta bng dung dch (NH4)2CO3 bo ha:
CaO + (NH4)2CO3

CaCO3 +2NH3 + H2O. Sy 1050C v cn)

7.3. Kt qu: Tnh nng khi lng ca Ca2+ trong mu lng hoc phn trm khi
lng dng hp cht trong mu rn.

20

Gio trnh Th nghim Ha Phn Tch

NH LNG ION SO42-

BI 8:

8.1. Nguyn tc
nh lng ion SO42- trong dung dch theo phng php khi lng
Dng cht to ta l dung dch Ba2+ (dng BaCl2). Phn ng to ta:
Ba2+ + SO42- BaSO4

TBaSO4 = 10-9,97

c im
- Ta BaSO4 dng tinh th mn, mu trng, to ta trong mi trng acid trnh phn
ng to ta ph khc. Cn to ta trong mi trng thch hp: dung dch nng, long v
khuy u khi thm chm cht to ta.
- Loi nhng ion c kh nng ng to ta
- Ta c lc bng phu thy tinh v giy lc nh lng (loi khng tro).
- Ta c nung 8000C trong chn snh ( nung v cn). Nung ta trong mi trng
oxy trnh phn ng kh ca C (do giy lc)
BaSO4 + C BaS + 4 CO
- Dng cn l BaSO4
- Lng mu cho mt ln to ta c dng ng vi lng dng cn khong 0,2 0,3g.
8.2. Thc nghim
8.2.1. Ha cht
-

Dung dch BaCl 5%/ nc

Dung dch AgNO3 1%/ nc

Dung dch HCl (1 : 2)

8.2.2. Cch tin hnh

- Becher 100ml: Ht V ml dung dch mu lng hay mg mu rn c ha tan. Nu
dung dch c ln cht khng tan th phi lc li. Thm 1ml dung dch HCl, thm nc ct
n 70ml. un dung dch va si, thm chm 10 20 ml dung dch BaCl2 nng, khuy u,
un cch thy 15 30 pht. Nu thun tin th tng thm thi gian cch thy.
- Lc ta bng giy lc khng tro. Ra ta bng nc nng n ht ion Cl- (kim tra li
bng dung dch AgNO3), cho vo chn snh nung 8000C v cn. t ta n thnh

21

Gio trnh Th nghim Ha Phn Tch

than en (ht bc khi). Nung 8000C khong 30 pht, chn ngui v cn. Nung li nu
cn n khi khi lng khng i.
8.3. Kt qu
Tnh nng khi lng SO42- dng hp cht trong mu lng hay phn trm khi
lng trong mu rn

22

Gio trnh Th nghim Ha Phn Tch

NH LNG DUNG DCH H2O2

Bi 9:

9.1.

Chun dung dch H2O2 bng dung dch KMnO4

9.1.1. Nguyn tc
9.1.1.1. Phn ng chun
Trong mi trng acid mnh:
2MnO4- + 5 H2O2 + 16 H+ 2 Mn2+ + 5 O2 + 8 H2O
E0O2/H2O2 = 0,682 V
c im :
- Phn ng chm nn cn pha long dung dch chun v lc mnh erlen khi chun
, c bit giai on u khi dung dch cha c hoc c rt t Mn2+ (Mn2+ c tnh xc tc
dng cho chun ).
- Cn mi trng acid mnh (dng H2SO4 long) v chun tht chm hn ch
vic to thnh MnO2 (l cht xc tc ca qu trnh phn hy H2O2).
- Nn lm lnh dung dch trc khi chun hn ch hin tng H2O2 b phn hy
to O2.
9.1.1.2. nh im cui
Da vo s xut hin ca mu hng (bn 2 pht) do dng tha KMnO4.
9.1.2. Thc nghim
9.1.2.1. Ha cht
- Dung dch chun KMnO4 0,05N
- Dung dch H2SO4 (1:5)
9.1.2.2. Cch tin hnh
- Buret: Dung dch KMnO4
- Erlen: Ht V(ml) dung dch mu H2O2 + khong 50ml nc + 5 ml dung dch
H2SO4, lm lnh nu cn.
- Chun bng dung dch KMnO4, mu ca dung dch ti im cui: khng mu
chuyn hng nht bn 2 pht.
9.1.3. Kt qu
Tnh nng mol, nng th tch v nng khi lng ca dung dch mu H2O2.

23

Gio trnh Th nghim Ha Phn Tch

9.2. Chun dung dch KMnO4 bng dung dch Acid Oxalic
9.2.1. Nguyn tc
9.2.1.1. Phn ng chun
Trong mi trng acid mnh:
2MnO4- + 5 C2O4 2- + 16 H+ 2 Mn2+ + 10 CO2 + 8 H2O
E0MnO4-/Mn2+ = 1,51 V
E02CO2/C2O42- = - 0,49 V
c im :
- Phn ng cn thc hin trong mi trng acid, nhng do tnh kh mnh ca C2O42nn ch to mi trng bng H2SO4 trong dung dch long.
- Phn ng ban u chm, nhng khi c Mn2+ ng vai tr xc tc, phn ng xy ra
nhanh hn.
- Phn ng nhanh nhit 600C nn cn un dung dch trc khi chun , nhng
nhit cao hn, acid Oxalic c th b phn hy cho ra CO2.
- Vn tc phn ng chm, cn pha long dung dch chun v lc mnh khi chun

9.2.1.2. nh im cui
Cht ch th l chnh ngay dung dch KMnO4 vi lng tha ngay sau im tng
ng to dung dch c mu hng nht bn 2 pht.
9.2.2. Thc nghim
9.2.2.1. Ha cht
- Dung dch chun acid Oxalic 0,05N
- Dung dch H2SO4 (1:5)
9.2.2.2. Cch tin hnh
- Buret: Dung dch KMnO4
- Erlen: Ht V ml dung dch chun acid Oxalic + khong 50ml nc + 5 ml dung
dch H2SO4. un nh dung dung dch 600C
- Chun bng dung dch KMnO4, mu ca dung dch ti im cui: khng mu
chuyn hng nht bn 2 pht.
9.2.3. Kt qu
Tnh nng mol, nng ng lng ca dung dch KMnO4
24