BI 8: XC NH CH TIU COD

I: Phng php 1: Phng Kalipemanganat ( TCVN 4565 - 88 )

1: Phm vi p dng
- i vi nc ngm hay nc sch, hm lng Cl-< 300
(mg/l)
2: Nguyn tc
Da trn vic oxi ho cc cht hu c c mt trong nc
bng dung dch Kalipemanganat 0,1N trong mi trng axit
nhit si. Lng d Kalipemanganat c chun bng
axit ascorbic 0,1N.
MnO4- + (C,H) +H+ t
Mn2+ + CO2 + H2O
MnO4-d + H2C2O4 + H+
Mn2+ +CO2
+ H2O
3: Yu t cn tr
- Clorua: Nng ln hn 300 ng/l loi b bng cch thm
vo 0,4 mg thu ngn snat.
- Amoni c nng cao cng gy cn tr. Loi b bng cch
un si nc cho cn n 2/3 th tch c.
4: Ho cht, dng c
Ha cht
- 250 ml dung dch KMnO4 0,1N -> m =

0,1.0.25.158
5

= 0,79

(g)
- 250 ml dung dch H2C2O4.2H2O 0.1N
m=

0,1.0,25.126
2

= 1,575 (g)

- Axit H2SO4 m c
Dng c
- Bnh tam gic, bnh nh mc, pipet, bnh tia, qu bp.
5: Tin hnh
- Ht 100 ml mu cho vo bnh tam gic dung tch 250 ml,
cho thm 3 vin bi thu tinh. Sau thm 1 ml H2SO4 c,
10 ml KMnO4 0,1N.Sau em un si dung dch trn bp
in v si 10 pht.
- Ly bnh ra khi bp in, nhanh chng thm vo chnh
xc 10 ml axit H2C2O4 0,1N. Lc u, chun ngc
lng axit d bng KMnO4 n khi dung dch xut hin
mu hng nht ( bn 10s ) th dng chun .
+ Ghi V1KMnO4 dng
- Tin hnh lm tng t vi 1 mu trng. Thay mu mi
trng bng nc ct.

+ Ghi V2KMnO4 dng

KMnO4 0,1N
-Vmu = 100 ml
- 2 ml H2SO4 c
- 10 ml KMnO4 0,1N
- 3 vin bi thu tinh
- 10 ml H2C2O4

un si v
si
10 pht

Khng mu -> hng nht

6: TNh kt qu
- Hm lng COD tnh theo cng thc
COD =

(V 1 V 2).C N KMnO 4.1000.8

vmu

(mgO2/l)

- Vi mu nc ngm sau khi chun :

+ V1KMnO4 chun mu mi trng = 0,5 ml
+ V2 KMnO4 chun mu trng = 0,3 ml
-> Hm lng COD trong mu nc ngm:
(0,5 0,3).0,1.1000.8
100
COD =
= 1,6 (mgO2/l)
- Vi mu nc h sau khi chun
+ V1 KMnO4 = 1,7 ml
+ V2KMnO4 = 0,3 ml
Hm lng COD trong mu nc h:
COD =

(1,7 0,3).0,1.1000.8
100

= 11,2 (mgO2/l).

7: Nhn xt kt qu
- Theo QCVN 09:2008/BTNMT - Quy chun k thut quc
gia v cht lng nc ngm.Hm lng COD trong nc
ngm l 1,6 (mgO2/l) nm trong gii hn ca vng nui
trng thu sn bo tn thu sinh.
- Theo QCVN 08: 2008/BTNMT - Quy chun k thut quc
gia v cht lng nc h. Hm lng COD trong mu
nc h l 11,2(mgO2/l) nm trong gi tr gii hn ca
loi nc A2 nn c th s dng cho mc dch ti tiu,

nui trng thu sn v cc mc ch khc c yu cu cht

lng thp hn.
II: Phng php 2: Phng php Kalidicromat (TCVN 6491 1999 )
1: Phm vi p dng
i vi nc c hm lng COD cao t 30 - 700 mg/l, nu
gi tr COD vt qu 700 mg/l mu nc cn pha long. Gi
tr COD nm trong khong 300 - 600 mg/l t c
chnh xc cao nht, hm lng Cl- < 1000 mg/l.
2: Nguyn tc
- Trong mi trng axitsunfuric c, Vi s c mt ca xc tc
Ag2SO4 th khi un nng K2Cr2O7 oxi ho cc hp cht hu
c. Chun lng d K2Cr2O7 bng dung dch mui Morh
vi ch th feroin, ti im cui chun , mu ca dung dch
chuyn t mu xanh lc sang mu nu .
- Loi b nh hng ca ion Cl- bng HgSO4.
CxHyOz + Cr2O72- + H+ Ag2SO4/HgSO4 CO2 + H2O +
Cr3+
Cr2O72- d + Fe2+ + H+
Cr3+ + Fe3+ + H2O
3: Ho cht , dng c
Ho cht
- 250 ml mui Morh [ (NH4)2.6H2O ] 0,12N
-> mmui = 0,06.0,25.392 = 5,88 (g)
- Dung dch K2Cr2O7 0,04 M. Pha 1l ( cha mui thu ngn )
-> mK2Cr2O7 = 0,04.1.294 = 11,76 (g)
Ho tan 80 (g) HgSO4 trong 800 ml nc ct. Thm vo
mt cch cn thn 100 ml H2SO4 c. ngui v ho tan
11,76 (g) K2Cr2O7 sy kh 105c ( trong 2h ) vo dung
dch. Chuyn ton b vo bnh nh mc v nh mc bng
nc ct n 1000ml.
( Dung dch bn t nht 1 thng ).
- Dung dch Ag2SO4 - H2SO4: cho 10 (g) Ag2SO4 vo 35 ml
nc. Cho t t 965 ml axit H2SO4c. 1 hoc 2 ngy
cho tan ht. Khuy dung dch tng nhanh s ho tan.
- Ch thi feroin: Ho tan 0,7 (g) FeSO 4.7H2O hoc 1 (g)
(NH4)2(FeSO4)2.6H2O trong mt t nc ct. Thm 1,5 (g) 110 phenaltrolin ngm 1 phn t nc C12H8N2.H2O v lc
cho n khi tan ht. nh mc bng nc ct n 100 ml.
Dung dch ny bn trong vi thng nu c bo qun ti.

Dng c: Bnh tam gic, bnh nh mc, pipet,buret, bnh tia,

qu bp,ng nghim.
4: Tin hnh
- Ph mu
+ Ht 2ml mu mi trng cho vo ng nghim, thm 1ml
K2Cr2O7/ HgSO4. y cht np ng nghim, lc u dung
dch, tin hnh ph mu trong l khong 2h v nhit
150c.
+ Tin hnh lm tng t vi mt mu trng. Thay 2ml mu
mi trng bng nc ct.
- Chun
+ Mu sau khi ph ngui v chuyn vo bnh tam gic
100 ml. Trng ng nghim v thm nc ct n khong
30 ml
+ Thm 2 git ch th feroin, lc u,dung dch c mu xanh
lc
+ Tin hnh chun bng dung dch mui Morh n khi
dung dch chuyn sang mu nu th dng chun .
Ghi V1 ml mui Morh tiu tn.
+ Vi mu trng tin hnh lm tng t
Ghi V2 ml mui Morh tiu tn.

Mui Morh 0,12N

- Mu ph v thm
nc ct n 30 ml
- 2 git ch th feroin.

Xanh lc -> nu
5: Tnh kt qu
Hm lng COD tnh theo cng thc

(V 2 V 1).C N mui.1000.8
vmu
COD =
(mgO2/l)
- Vi mu nc h sau khi chun
+ Mu mi trng : V1muiMorh = 2,1 ml
+ Mu trng : V2mui Morh = 1,9 ml
Hm lng COD trong mu nc h
COD =

( 2,1 1,9).0,12.1000.8
2

= 96 (mgO2/l).

II: Xc nh tng N
1: Phm vi ng dng
- Xc nh ion nitrat trong mu nc th v nc sinh hot.
- Gii hn xc nh 30 - 50 (mgN/l)
2: Nguyn tc
- Chuyn ton b cac hp cht ca Nit v dng NO3 - bng
cch x l mu trong l vi sng( III/ Bi 13 - Ph mu tng
Nit ).
- Hp cht Nitrat + Natrisalixylat + NaOH -> Phc mu vng
chanh
o hp thh quang bc sng 415
nm.
3: Cc yu t nh hng
Cc cht l lng, cn, mu sc: X l bng cch lc mu
hoc cho KNO3.
4: Ho cht, dng c
Ho cht
- Dung dch NO3- chun gc 1 (gN/l): Pha 100 ml
-> mNaNO3 =

1.0.1.85
14

= 0,6071 (g)

- Dung dch NO3- chun lm vic 1 (mgN/l): Pha long dung

dch gc 1000 ln.
- Dung dch Natrisalixylat (HO-C6H4-COONa) 10 (g/l)
-> Ho tan 1 (g) Natrisalixylat trong 100 ml nc ct. Bo
qun dung dch trong chai thu tinh hoc chai Polyetylen
- Dung dch NaOH 200 (g/l): Cn 20 (g) NaOH pha trong
100ml nc ct.
- Axit H2SO4 c.

 Dng c: Bt s, bnh nh mc, pipet, qu bp. a thu

tinh, cc cn.
5: Tin hnh
- Xy dng ng chun
Chun b dy chun gm 5 bnh nh mc 25 ml c
nh s t 0 -> 4, 5 bt s dung tch 50 ml. Tin hnh cho
cht chun , thuc th v cc ho cht khc theo th t.
Stt
0
1
2
Dung dch NO3 lm vic
0
1
2
cho vo bt s (ml )
Dung dch Natrisalixylat
1
1
1
(ml)
un trn bp n cn (ch khng chy) sau
Axit H2SO4 c ( ml)
1
1
1
Lc k cho tan ht cn,
yn 10 pht.
Nc ct (ml)
5
5
5
Dung dch NaOH (ml)
10
10
10
nh mc bng nc ct n vch 25 ml.
C (mgN/l)
0
0,04 0,08
Abs
0
0,026 0,06

3
3

4
4

ngui.
1
1

5
10

5
10

0,12 0,16
0,075 0,101

- Mu mi trng:Ht 20 ml mu x l trong l vi sng a cc

hp cht ca Nit v dng NO3- sau khi ly mu ra thm nc
ct nh mc ln 50 ml. Ht 10 ml mu x l cho vo bt
s. Thm cc ho cht v thc hin nh dy chun.
- dy chun v mu mi trng n nh mu trong 10 pht
ri em i o hp th quang ti bc sng 415 nm.
6: Tnh kt qu
Abs = a.Cx + b -> Cx =

Abs b
a

Cx nng NO3- tnh theo ng chun

-> [NO3-]mu mi trng =

Cx.Vdm
Vmu

Y = 0,6275x - 0,0026
R2 = 0,9739

- Vi mu nc h: Abs = 0,751
Cx =

0,751 0,0026
0,6275

[NO3-]

mu mi trng

= 1,1927 (mgN/l)
=

1,1927.25.50
10.20

= 7,4544 (mgN/l).

7: Nhn xt kt qu
- Theo QCVN 08: 2008/BTNMT - Quy chun k thut quc
gia v cht lng nc mt. Hm lng NO3- trong mu
nc h laf 2,9818 (mgN/l) nm trong gii hn ca loi
nc A2. C th s dng cho mc ch ti tiu, thu li
v cc mc ch khc c yu cu thp hn.
8: Ch
- Bt s cn c trng ra cn thn v sy kh.
- Khi un dung dch trn bp cch ct cn ch khng
chy mu.
I: Xc nh NH4+ bng phng php o quang ph hp th phn
t vi Phenol v hypochlorite ( phng php indo - phenol ).
1: Nguyn tc
Phenol
+
NH4
+
natri nitropruesside
Hypochlorite

phc mu xanh m

o hp th quang ti bc sng 510 nm

2: Ho cht, dng c

 Ho cht;
- Dung dch Phenol: Ly 10 (g) phenol cho vo bt s hoc
cc un nng chy cho phenol tan ra ( nhit nng chy
43c ). Ly ly 2,8 ml phenol cho vo 22,5 ml cn etylic
95, trn u. Dung dch ny bn trong 1 tun.
+ Ch : Phenol rt c nn khi pha dung dch ny phi ch
trong t ht, cn bo v tay v mt.
- Dung dch xc tc Natri nitroprusside Na2[Fe(CN)5NO].2H2O
0,5%: Cn 0,5 (g) pha trong 100ml nc ct. Dung dch ny
s dng c 1 thng.
- Dung dch Natricitrat : 200 (g) Natricitrat + 10 (g) NaOH
pha trong 100ml nc ct.
- Dung dch NaClO 5%: cn 0,5 (g) pha trong 100 ml nc
ct. Dung dch c mu xanh sm c 2 thng.
- Dung dch hn hp: Trn ln 100 ml dung dch Natricitrat
( pha trn ) v 25 ml dung dch NaClO
- Dung dch mui xenhet ( Kalinatritactarat ): 30(g)/l.
- Dung dch NH4Cl chun gc 1gN/l: 100ml
-> mNH4Cl =

1.53,5.0,1
14

= 0,382 (g)

Cn 0,382 (g) NH4Cl sy kh 105 C trong 1h ri ho

tan trong 100ml nc ct.
- Dung dch NH4+ lm vic 5 (mgN/l) : pha long dung dch
gc 200 ln.
Dng c
ng nghim, pipet, qu bp, ng nghim, bnh tia, cc cn.
3: Tin hnh
- Xy dng ng chun :
Chun b 5 ng nghim, nh s t 0 -> 4. Tin hnh cho
cht chun, thuc th v cc ho cht khc theo th t:
Stt
Dung dch NH4+ lm vic
(ml)
Nc ct 2 ln (ml)
Dung dch phenol (ml)
Dung dch xc tc (ml)
Dung dch hn hp (ml)
C mgN/l
Abs

0
0

1
0,1

2
0,2

3
0,3

4
0,4

5
0,2
0,2
0,5
0
0

4,9
0,2
0,2
0,5
0,1
0,04
5

4,8
0,2
0,2
0,5
0,2
0,08
4

4,7
0,2
0,2
0,5
0,3
0,12

4,6
0,2
0,2
0,5
0,4
0,15
6

- Phn tch mu mi trng

Ht 5 ml mu cho vo ng nghim. Thm cc ho cht lm
tng t nh nh dy chun.
- Mu kim tra: c pha long 10 ln. Sau ht 0,2ml
pha long cho vo ng nghim. Thm nc ct n 5ml,
sau thm cc ho cht khc nh dy chun.
- dy chun v mu mi trng n nh mu trong 2h.
Sau em i o hp th quang ti bc sng 640 nm.
4: Tnh kt qu

Abs = a.Cx + b -> Cx =

Abs b
a

- Cx: Nng NH4+ trong mu mi trng tnh theo ng

chun
-> [NH4+] mu mi trng =

Cx.Vdm
Vmu

- Vi mu mi trng: Mu nc ngm Abs =0,00

- Vi mu kim tra: Abs 0,453
- Y = 0,387x + 0,0036
- R2 = 0,9977
Vi mu kim tra: Vmu = 0,2 ml
Cx =

0,453 0,0036
0,387

[NH4+]mu kim tra =

= 1,161 (mgN/l)
1,161.5
0,2

= 29,025 (mgN/l).

Mu kim tra c pha long 10 ln

-> [ NH4+]MKTthc t = 29,025 . 10 = 290,25 (mgN/l)

Vi mu mi trng Abs = 0,00 -> khng c NH4+ trong mu

nc ngm.