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TRNG I HC CNG NGHIP TP.

HCM
KHOA CNG NGH HA HC

N CHUYN NGNH
KHO ST, CC YU T NH HNG N QUY TRNH
XC NH COD TRONG NC BNG PHNG PHP
PERMANGANAT V KALIDICROMAT

GVHD: Th.S L THANH TM


SVTH: NGUYN TN PHC
NGUYN TH KIM THOA
Lp:

CDPT9LT

Kho:

2010 2012

Tp. H Ch Minh, thng 02 nm 2012

TRNG I HC CNG NGHIP TP. HCM


KHOA CNG NGH HA HC

N CHUYN NGNH
KHO ST, CC YU T NH HNG N QUY TRNH
XC NH COD TRONG NC BNG PHNG PHP
PERMANGANAT V KALIDICROMAT

GVHD: Th.S L THANH TM


SVTH: NGUYN TN PHC
NGUYN TH KIM THOA
Lp:

CDPT9LT

Kho:

2010 2012

Tp. H Ch Minh, thng 02 nm 2012

TRNG I HC CNG NGHIP TP.HCM

CNG HA X HI CH NGHA VIT NAM

KHOA CNG NGH HA HC

c lp T do - Hnh phc

----- // -----

----- // -----

NHIM V N CHUYN NGNH


H v tn sinh vin:

NGUYN TN PHC

MSSV: 10355461

NGUYN TH KIM THOA

MSSV: 10355471

Chuyn ngnh: Ha Phn Tch


Lp: CDPT9LT
Tn n hc phn: Kho st, cc yu t nh hng n quy trnh xc nh COD trong
nc bng phng php permanganat v kalidicromat.
Nhim v ca n:
1. Tm hiu v nc v nc thi.
2. Tm hiu v COD v cc ch tiu xc nh COD.
3. Tm hiu v cc quy trnh ly mu v bo qun mu nc.
4. Tm hiu cc phng php xc nh COD trong nc.
5. cng thc nghim v d ton chi ph quy trnh xc nh COD.
6. nh hng pht trin n
Ngy giao n: ngy thng . nm ..
Ngy hon thnh n: ngy thng nm
H tn gio vin hng dn: L Thanh Tm
Tp. H Ch Minh, ngy . thng ..nm
Trng b mn

Gio vin hng dn

Th.S Trn Nguyn An Sa

Th.S L Thanh Tm

LI M U

Nh chng ta bit nc chim ti 3/4 din tch b mt tri t. Khng ch vy nc


cn l mt phn ti quan trng v khng th thiu trong cuc sng ca con ngi v nc
cng chim mt phn rt quan trng trong c th. trong c th con ngi nc chim ti
75%.
Nc cng chim mt phn quan trng trong cc hot ng sn xut nng nghip nh:
thy li, ti tiu cung cp nc ti cho cy trng .., trong cng nghip nc l mt
ngun nng lng khng l (hi triu, thy nng) phc v cho cc cng trnh thy in,
cung cp nc sn xut trong cc nh my, x nghip v cc cung cp nng lng trong
cc hot ng sinh hot khc trong i sng ca con ngi .v.v.
Ngoi ra nc cn l cht mang vt liu, tc nhn iu ha kh hu, thc hin cc chu
trnh tun hon vt cht trong t nhin. C th ni nc l yu t hng u ca tt c s
sng trn hnh tinh chng ta.
Nhng hin nay cng vi s pht trin khng ngng ca khoa hc k thut, cc ngnh
cng nghip cc khu cng nghip, cc nh my, x nghip ngun nc trn tri t ni
chung v nc ta ni ring ang b nhim trm trng iu ny ang trc tip e da n
i sng ca con ngi v cc loi ng thc vt cng nh tt c cc sinh vt sng trn hnh
tinh chng ta.
Chnh v vy chng ta cn phi bit cch phn tch, kim tra, kim sot, tm ra nguyn
nhn, tc nhn trc tip gy nhim ngun nc nhm x l, tm ra phng hng ti u
nht ci thin, gim thiu ti a s nhim ngun nc, ci thin, nng cp ngun nc
m bo cho cc hot ng sinh hot trong i sng ca con ngi ngy mt tt hn.

LI CM N

Chng em xin chn thnh cm n cc thy, c trong Khoa Cng Ngh Ha Hc ca


trng i Hc Cng Nghip Thnh Ph H Ch Minh. c bit l ch nhim b mn Trn
Nguyn An Sa v GVHD L Thanh Tm cn k, gip chng em trong sut thi gian
hc tp ti trng, truyn t cho chng em nhng kin thc, kinh nghim sng v lm vic.
Qua y chng em cng xin gi li cm n su sc n gim c Khoa Cng Ngh
Ha Hc cng gio vin b mn khc trong Khoa Cng Ngh Ha Hc, nhit tnh gip
, v to iu kin thun li nht cho chng em c mt mi trng lm vic l tng trong
sut thi gian thc nghim ti Khoa Cng Ngh Ha Hc.
Chng em xin chn thnh cm n !!!

NHN XT CA GIO VIN HNG DN

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Tp. H Ch Minh, ngy .. thng .. nm 20..
Gio vin hng dn

L Thanh Tm

MC LC

Nhim v n hc phn
Li ni u
Li cm n
Nhn xt ca gio vin hng dn
MC LC..............................................................................................................................1
PH LC...............................................................................................................................1
Chng
TNG

1
QUAN

NC,

NC

THI

CCH LY MU, BO QUN MU NC....................................................................1


1.1. Tng quan v nc thin nhin v nc thi...................................................................1
1.1.1. Nc thin nhin.......................................................................................................1
1.1.2. Nc thi...................................................................................................................2
1.2. Cc tp cht v nh hng ca cc tp i vi nc thin nhin & nc thi................4
1.2.1. Cc mui canxi v magie .........................................................................................4
1.2.2. Mui NaCl v Na2SO4.............................................................................................4
1.2.3. Mui st ....................................................................................................................4
1.2.4. Hp cht cha nit ...................................................................................................4
1.2.5. Hp cht silic ...........................................................................................................4
1.2.6. Hp cht hu c .......................................................................................................5
1.2.7. Cc kh ha tan .........................................................................................................5
1.2.8. Cc cht keo .............................................................................................................5
1.2.9. Nhng cht huyn ph .............................................................................................5
1.2.10. Cc kim loi ...........................................................................................................5
1.3. Cc ch tiu phn tch nc thin nhin v nc thi......................................................6
1.3.1. Xc nh pH..............................................................................................................6
1.3.2. Xc nh hm lng cn khng tan...........................................................................6
1.3.3. Xc nh cng......................................................................................................6

1.3.4. Xc nh kim ca nc.......................................................................................6


1.3.5. Xc nh axt ca nc.........................................................................................7
1.3.6. Xc dnh SO42- trong nc sinh hot bng sc k ion..............................................7
1.4. Tiu chun v mc cht lng cc loi nc..................................................................7
1.4.1. Nc sinh hot .........................................................................................................7
1.4.2. Nc trong sn xut cng nghip .............................................................................7
Chng

TNG QUAN V COD.........................................................................................................9


2.1. nh ngha nhu cu oxi ha hc (COD)..........................................................................9
2.2. ngha mi trng..........................................................................................................9
2.3. Cc phng php xc nh hm lng COD...................................................................9
2.3.1. Phng php KMnO4 (Phng php Manganat).....................................................9
2.3.2. Phng php K2Cr2O7 (Phng php Dicromat)....................................................9
2.4. Cch ly mu nc v bo qun mu nc...................................................................10
2.4.1. Cch ly mu...........................................................................................................10
2.4.1.1. Ly mu b mt ...................................................................................................10
2.4.1.2. Ly mu su nh ...................................................................................10
2.4.1.3. Ly mu nc t cc vi ca h thng cp nc ................................................10
2.4.1.4. Ly mu t cc ging bm tay, bm my ...........................................................10
2.4.1.5. Ly mu nc ung .............................................................................................10
2.4.2. Bo qun mu..........................................................................................................11
2.4.3. Mt s hnh nh ly mu nc sng ti sng Bnh Li..........................................13
Chng

CNG THC NGHIM V D TON CHI PH ..................................................16


3.1. Mc tiu ti...............................................................................................................16
3.2. Ha cht, dng c v thit b thc nghim....................................................................16
3.2.1. Ha cht xc nh hm lng COD........................................................................16
3.2.2. Dng c v thit b thc nghim.............................................................................17
3.3. Thc nghim..................................................................................................................17
3.3.1. Phm vi p dng......................................................................................................17
2

3.3.2. Nguyn tc...............................................................................................................17


3.3.2.1. Nguyn tc xc nh COD bng phng php Kali Permanganat.......................17
3.3.2.2. Nguyn tc xc nh COD bng phng php Kali Dicromat.............................17
3.3.3. Kho st cc yu t nh hng v khc phc.........................................................18
3.3.3.1. i vi phng php Manganat (KMnO4)..........................................................18
3.3.3.2. i vi phng php Kali dicromat....................................................................18
3.3.4. Tin hnh kho st...................................................................................................18
3.3.4.1. Kho st xc nh mu tht bng phng php Kali Permanganat......................18
3.3.4.2. Kho st xc nh mu tht bng phng php Kali dicromat............................19
3.3.5. Tnh ton kt qu.....................................................................................................19
3.3.5.1 Tnh ton kt qu bng phng php Kali Permanganat......................................20
3.3.5.2. Tnh ton kt qu bng phng php Kali Dicromat...........................................20
3.4. Bng kt qu phn tch...................................................................................................21
3.4.1. Bng kt qu phn tch ca phng php Kali Permangant....................................21
3.4.2. Bng kt qu ca phng php Dicromat...............................................................21
3.5. Hnh nh phn tch mu.................................................................................................22
Chng

KT LUN V KIN NGH..............................................................................................28


4.1 Kt lun...........................................................................................................................28
4.2 Kin ngh:........................................................................................................................28
TI LIU THAM KHO....................................................................................................29

PH LC

Chng 1
TNG QUAN V NC, NC THI V
CCH LY MU, BO QUN MU NC

1.1. Tng quan v nc thin nhin v nc thi


1.1.1. Nc thin nhin
Gm cc loi nc ca cc ngun thin nhin nh: sng ngi, ao h, sui, mch nc
ngm, bin, i dng C th ni nc thin nhin l mt h d th nhiu hp phn,
nc thin nhin cha nhng no cc cht tan v khng tan c ngun gc v c cng
nh hu c. Cc cht ri hoc a vo t kh quyn, t t v t nn, t b v cc
ngun cha hoc cc mch nc chy qua. Cc cht cn c to thnh do hot ng
sng v b hy dit ca cc c th ng vt, thc vt sng trong nc hoc y cc ngun
nc. Ty theo hm lng v tnh cht cc tp cht trn, ngi ta s dng nc vo cc
mc ch khc nhau. Theo ngun pht sinh ngi ta chia nc thin nhin thnh cc loi
sau: nc ma, nc mch (nc ngm), nc trn mt tri t.
Nc ma: thng ha tan mt lng kh CO2, O2, N2 v mt s kh khc. Do s
ha tan kh cacbonic, vng nhiu vi lu i sinh ra hang ng, ngoi kh ha tan
ra, trong nc ma cn c ln bi bm v vi trng, nc ma thuc loi nc mm, sch
mt khi mi hng.
Nc mch, nc ngm: do nc thm trong lng t, lu i to thnh nhng
mch chy trong lng t, v c chc lng qua nhiu tng t, nc mch thuc hai loi
nc mm, trong mt dng sinh hot rt thun tin.
Nc trn mt tri t nh nc ca ao, h, sng bin nc cc i dng. c
im ca loi nc ny thng cha nhiu cc tp cht khc nhau.
Tm li:
Cc tp cht tn ti v ha tan trong nc, gm cc mui ha tan to vi nc thnh
dung dch, cc hp cht khng tan lm cho nc c v cc hp cht hu c sinh ra huyn
ph, cc trng thi keo l lng, chng lm cho nc c mi, ngoi ra cn c loi kh ha

tan. Ring cc mui v c khi ha tan trong nc th phn ly thnh ion nn khi phn tch
mu nc thng phn tch dng ion.
1.1.2. Nc thi
Cng vi s pht trin vn minh ca nhn loi nhu cu v nc ngy cng nhiu, cc
hot ng ca con ngi trong cc lnh vc khc nhau ca sn xut v i sng hng ngy
cng nh hng n thnh phn ca nc thin nhin. S bn phn ci to t bng cc
ha cht, cc ph thi ca nh my, cc khu cng nghip, c bit l nc thi cng nghip
v nhng hot ng khc ca con ngi cng a vo nc thin nhin nhng cht v c
v hu c, gy nhim ng k n nc b mt v mi trng.
Nc thi a vo b mt cc loi ha cht khc nhau t trng thi tan n dng
huyn ph, nh tng cho n cc loi vi khun Do tng tc ha hc ca cc cht ,
do s thay i pH ca mi trng nn cc sn phm th cp c to thnh. Cc cht kt
ta v huyn ph c trong nc ngn cn s pht trin ca cc loi vi khun tham gia vo
qu trnh lm sch nc. Cc cht huyn ph lm cn tr s m xuyn ca nh sng mt
tri xung ngun nc, do hn ch qu trnh quang hp ca thc vt di nc c bit
l cc loi rong bin, m di tc dng ca nh sng li to ra c oxy cn thit cho qu
trnh oxy ha cc cht bn hu c.
Mt s cht v c v hu c tan trong nc c nh hng c hi n s pht trin
cc vi sinh vt trong nc. Trong s cc cht v c phi k n cc ion v hp cht ca ch,
arsen, flo, crom, ng c tc dng c hi v chng s lm thay i pH ca nc. Cc
khong pH nh hn 6,8 v ln hn 8,0 l nhng khong hn ch s pht trin mt s loi vi
khun cn thit cho s lm sch nc.
Trong nhng nm gn y nguy c lm nhim mi trng do cc cht hu c, c
bit cc sn phm ca cng nghip v khai thc ch bin du m gy ra ngy cng tng ln.
S c mt trong nc cc loi thuc tr su, dit c, cc cht ty ra tng hp cng l mi
e da ng k n s tn ti ca mt s loi thy sinh. Cc cht c v cht phng x thi
ra t cc phng th nghim v cc nh my cng nh cc sn phm to thnh trong cc v
th ht nhn cng l nhng nguyn nhn gy nhim ng k n ngun nc thin nhin.
Kh c th c c mt thng k v s phn loi r rng v thnh phn ha hc ca
cc loi nc thairnvif iu ph thuc rt nhiu vo qu trnh sn xut v sinh hot trong
2

nc c thi ra. C th ni nc thi l mt h d th phc tp bao gm rt nhiu cht


tn ti di cc trng thi khc nhau. Nu nh nc thi cng nghip cha rt nhiu cc
ha cht v c v hu c th nc thi sinh hot li cha rt nhiu cc cht bn di dng
protein, cc cacbon hydrat, m, cc cht thi ra t ngi v ng vt, ngoi ra cn phi k
n cc loi rc ri nh giy, g, cc cht hot ng b mt.
c th c mt nh hng v thnh phn ha hc ca mt s loi nc thi, chng
ti xin dn ra di y mt s cht ch yu thng c trong nc thi ca mt s qu trnh
sn xut:
-

Khai khong: cc kim loi, cc acid c c.

Gia cng g: flo, km.

gm: bari, cadimi, liti, mangan, selen

da: canxi, sunphuahydro, sunfua natri, crom, km, niken

Luyn cc: amoniac, sunfua hydro, cc kim

Cng nghip sn: bari, clorat, cadimi, coban, ch, km, amoniac, xt, cc acid, cc
cht hu c

Luyn kim: cc hp cht amoni, cc acid, kim loi, sunfua hydro, sunfat, clo,
photphat

K ngh x phng: bari, xt, sunfua hidro

Ha du: cc acid, kim loi, clorua, sunfat, cc cht hu c

Thuc tr su: bari, cadimi, ng, arsen, silic, tetraflorua, flo, clo, mt s cht c
hu c

Cao su: Borat, nitrit, selen, lu hunh, antimon

Thy tinh: acid boric, kali, mangan, ng arsen, sunfua, nitrit, florua, thic, selen,
sunfua hidro

K thut dt: cc hp cht amoni, thic, ch, flo, kim, kali, ng, km

Phn bn: kali, amoniac, nitrat, photphat, cc acid, cc kim loi

Ha dc: boran, brom, mui amoni, kali, cc acid, cc kim loi, kim, cc cht hu
c

Giy: xt, cc kim loi, clo, sunfat, sunfit, sunfua


3

Trong cc hp cht gy nhim bn k trn th thy ngn, berili, cadimi, ch, arsen,
selen c tnh cht c nht.
Nc thi sinh hot c thnh phn ha hc n gin hn, ch yu l cc kim loi sau:
kali, natri, st, ng, ch, km, niken, mangan, thy ngn, bc, coban.
1.2. Cc tp cht v nh hng ca cc tp i vi nc thin nhin & nc thi
1.2.1. Cc mui canxi v magie
Ch yu di dng bicabonat, clorua, sunfat gy ra s ng cn khi un si, x phng
t bt, gy ra nhiu phn ng vi cc ha cht khi pha chng trong nc. Ngi ta gi l
tnh cng ca nc. Tnh cng ny thay i theo hm lng cc mui canxi v magie c
trong nc, c nh hng ln n nc sinh hot cng nh sn xut cng nghip.
Ty theo tr s cng m ta phn bit cc loi cng nh bng sau:
Loi nc

Rt mm

Mm

0 1,5

1,5 3,0

cng chung
(mg/l)

Cng trung
bnh
3,0 4,5

Hi cng

Cng

4,5 6,5

6,5 11,0

Rt cng
11,0

1.2.2. Mui NaCl v Na2SO4


Hu nh iu c mt trong cc loi nc thin nhin. Cc mui ny khng th hin
tnh cng ca nc v a s cc trng hp khng gy tc hi cho vic s dng nc. Tuy
nhin trong nc cha nhiu cc mui trn, khi s dng nc trong ni hi thng gy ra
p sut cao v n lm cho hp cht hu c tan trong nc d.
1.2.3. Mui st
Trong nc thng tn ti dng Fe(HCO3)2. Khi nng mui st ln, thng lm
cho nc vng c mi tanh kh chu khi tip xc lu vi khng kh, mui st trn d b oxy
ha t mui Fe2+ thnh mui Fe3+ v gy ra cn Fe(OH)3 lm cho nc c. v th vic xc
nh mui st trong nc khi s dng l iu cn thit.
1.2.4. Hp cht cha nit
D sinh huyn ph, c mi khi nng nit cao, trong nc tn ti cc dng v
c nh cc mui NH4+, NO3-, NO2- v dng hu c.
1.2.5. Hp cht silic
4

Thng c trong nc thin nhin vi lng nh, dng mui ha tan Na2SiO3,
K2SiO3 v dng keo H2SiO3 (hay dng huyn ph ln vi t ct). Hp cht silic ny cng
ln lm cho nc cng mm, nhng l hp cht d sinh cu bn trong nc.
1.2.6. Hp cht hu c
Tn ti trong nc dng keo nh nhng cht thc vt b thi ra, hoc trng thi
ha tan. S c mt cc hp cht hu c lm cho nc c tnh kh ngha l th hin kh
nng oxy ha hay conn gi l oxy ha bng KMnO4 ca nc. Nhng khi xc nh
oxy ha ca nc, cn ch n cc hm lng kh trong nc nh mui Fe2+, NO2-.
1.2.7. Cc kh ha tan
Kh nit v CO2 tan trong nc lm cho nc c v mt, c li cho nc sinh hot.
Nhng nc dng trong cng nghip nht l trong ni hi, sn xut cc ha cht th O2 v
CO2 d sinh ra an mn. Kh H2S i khi c trong nc, do s v c ha cc hp cht hu
c c cha lu hunh. Kh c ny tn ti trong nc d n mn thit b, trong nc sinh
hot khng c c kh H2S v y l c t cao.
1.2.8. Cc cht keo
Trong nc thin nhin phn ln l do ng thc vt ln men, phn hy to thnh
cng thc chung ht keo dng hu c vi phn t ln. Thng (C6H4O3) y n 8 cc
cht keo ny lm nc c phn ng vi axt, c tc dng n mn kim loi khi tip xc lu.
Cc cht keo trong nc, cn c th l nH2SiO3.
1.2.9. Nhng cht huyn ph
c to thnh trong nc l do nhiu ngun khc nhau, c th l do cc hp cht v
c hoc hu c. Chng lm nc vn c, d to thnh cn b trong ni hi, trong ng dn
lm vn c cc dng c, thit b ra.
Nc thin nhin, ty loi (h, ao, sng, ngi,) v tng vng m hm lng cc tp
cht trn c th thay i. Nn thnh phn cc tp cht thin nhin ni chung phc tp v
nh hng n vic s dng nc vo mc ch khc nhau, v th trc khi s dng, cn
phn tch cc thnh phn ha hc ca nc l iu cn thit.
1.2.10. Cc kim loi
c to thnh do nhiu ngun khc nhau
5

1.3. Cc ch tiu phn tch nc thin nhin v nc thi


1.3.1. Xc nh pH
Thng xc nh bng phng php in th.
Phng php ny c u im l khng b cn tr bi mt lot cc yu t nh mu sc,
c ca dung dch phn tch, s c mt ca nhiu cht oxy ha kh v cc cht l khc.
1.3.2. Xc nh hm lng cn khng tan
Tp cht khng tan trong nc c cc loi sau:
-

Loi cn kh: l cc tp cht d tan, c xc nh bng cch lc qua giy lc


bng xanh, sau em sy v cn.

Loi cn sau khi nung gm cc tp cht tan v khng tan, c xc nh bng cch
bc kh mu nc 105oC sau em sy v nung.
Cht rn tng cng (TS) c trong nc bao gm cht rn ha tan (DS) v cht rn l

lng (SS), cng c th xem cht rn tng bao gm cht rn bay hi (VS) v cht rn n
nh (FS).
Da trn phng php trng lng sau khi cho bay hi mu nhit v thi gian
thch hp, cht rn cn li c xc nh bng phng php cn.
1.3.3. Xc nh cng
cng ca nc do cc kim loi kim th ha tr 2, ch yu l canxi v magie gy
nn. cng chung ca nc biu th bng tng lng mui ca canxi v magie c trong
mt lt nc
cng c xc nh chun to phc Ca2+ v Mg2+ vi dung dch EDTA tiu
chun bng m pH = 10 vi ch th ETOO. im tng ng nhn c khi dung dch
chuyn t mu sang xanh chm.
1.3.4. Xc nh kim ca nc
kim ca nc l hm lng ca cc cht phn ng vi axt mnh, tc l phn
ng vi ion hydro. xc nh kim ca nc ngi ta p dng phng php trung
ha, dng dung dch axt mnh chun .
kim c biu th bng s mg axt tiu tn ng vi 1 lt nc.
6

kim do cc axt amin ca axt yu khi thy phn sinh ra CO32-, HCO3-, HPO42-,
OH-, HS-
Chun mu nc bng HCl tiu chun theo ch th phenolphtalein gi l kim
phenol ( kim t do), chun theo ch th MO ta c kim metyl da cam ( kim ton
phn).
1.3.5. Xc nh axt ca nc
i vi cc loi nc thin nhin a s cc trng hp, axt ph thuc vo hm
lng kh CO2 trong nc. Cc cht mn v cc axt hu c yu c trong nc cng to
nn mt phn ca axt. Trong tt c cc trng hp pH ca nc thng khng <
4,5.
i vi cc loi nc thi, hm lng cu axt mnh t do thng kh ln, khng
nhng vy trong nc thi thng cha cc mui to thnh bi baz yu v axt mnh, nn
axt nc cng cao, pH ca nc thng khng > 4,5 c gi l axt t do.
Dng dung dch km mnh NaOH chun axt c trong nc do s hin din ca
cc axt v c mnh, axt yu hoc axt hu c bng cc ch th thch hp.
1.3.6. Xc dnh SO42- trong nc sinh hot bng sc k ion
Mi loi ion c gi li trong ct vi cc thi gian khc nhau, do ta c th nhn
danh c cc ion trong hn hp ca chng khi i qua ct sc k trao i ion nh vo thi
gian lu c trng ch tng loi ion. Ngoi ra khi so snh din tch ca peak chun vi
mu, ta c th xc nh c hm lng ca ion cn xc nh.
1.4. Tiu chun v mc cht lng cc loi nc
Ty theo pham vi s dng ngi ta cn chun ha cc loi nc, nc thin nhin
khng tha mn cc yu cu chung nn ngi ta cn tin hnh x l nc bng cc phng
php khc nhau, lm cho nc trong v gim cc tp cht ha hc trong sn xut cng
nghip v cng nghip ha nhit in,
1.4.1. Nc sinh hot
Phi mt, trong sut, khng mu khng mi v, thnh phn ca nc phi t thay i
theo thi gian. Nc dng trong sinh hot khng c hoc rt t theo quy nh v c t v
cc tp cht c hi.
1.4.2. Nc trong sn xut cng nghip
7

Trong sn xut cng nghip nc c dng vi nhiu mc ch khc nhau nh dng


trong ni hi, ng c hi nc, lm dung mi ra bn hoc ha tan,
Ring nc dng trong ni hi, ta c cc yu cu v cht lng ca nc nh
cng, lng O2 v CO2 ha tan, oxy ha tan, oxy ha, dn in, tp cht u m,

Xem thm cc tiu chun v mc cht lng nc theo TCVN.

Chng 2
TNG QUAN V COD

2.1. nh ngha nhu cu oxi ha hc (COD)


L lng oxy cn thit oxy ha ht cc hp cht hu c c trong nc. Nc
nhim bn s c oxy ha cao phi tn nhiu ha cht cho cng tc kh trng
2.2. ngha mi trng
y l ch tiu thng c s dng trong quan trc mi trng nh gi mc
nhim hu c i vi ngun nc mt thuc nhng thy vc nc ngt. i vi nc
thi cng nghip y l ch tiu khng th thiu khi nh gi mc nhim. COD cn l
ch tiu quan trng lm c s tnh ton v thit k cc cng trnh x l nc thi.
2.3. Cc phng php xc nh hm lng COD
2.3.1. Phng php KMnO4 (Phng php Manganat)
Cc hp cht hu c trong mu b xy hoa bng KMnO4 trong mi trng acid 96
98oC trong b nhit (water bath) trong khong 20 pht. Lng permanganat d s tip tc
oxy ho lng I- thm vo v sinh ra lng I2 tng ng trong mi trng acid, sau
lng I2 ny c xc nh bng cch chun bng S2O32- vi ch th h tinh bt.
Phng trnh phn ng :
10I- + 2MnO4- + 16H+ 2Mn2+ + 5I2 + 8H2O
I2 + 2S2O32- 2I- + S4O62Lu : Nu mu l mu nc bin, nc l th oxy ha trong mi trng trung tnh
hoc kim, cc mu nc cn li ta xc nh trong mi trng acid.
2.3.2. Phng php K2Cr2O7 (Phng php Dicromat)
Tng hm lng cht hu c c trong nc thi s b oxy ha bi tc nhn oxy ha
mnh K2Cr2O7. Cc hp cht hu c trong nc s b oxy ha hon ton bi K2Cr2O7 trong
mi trng H2SO4 m c iu kin un nng khong 2 gi.
Cho d chnh xc mt lng K2Cr2O7 oxy ha hon ton tng hm lng hp cht
hu c, sau chun lng K2Cr2O7 d c chun bng dung dch chun Fe2+ vi ch th
9

Ferroin. im tng ng nhn c khi dung dch chuyn t mu xanh lam sang mu
nu .
Phng trnh phn ng:
CnHaObNc + dCr2O72- + (8d+c)H+ nCO2 +

a + 8d - 3c
H2O + cNH4+ + 2dCr3+
2

6Fe2+ + Cr2O72- + 14H+ 6Fe3+ + 2Cr3+ + 7H2O


2.4. Cch ly mu nc v bo qun mu nc
2.4.1. Cch ly mu
2.4.1.1. Ly mu b mt
Ly mu cch mt nc khong 20 cm, ch cn nhng bnh, ca hoc x vo dng
sng, sui,.. Sau cho nc vo bnh cha mu.
2.4.1.2. Ly mu su nh
Khi ly mu trng hp ny cn phi dng thit b ly mu c bit nh thit b c
ng h, bm hoc ly mu t ng,
2.4.1.3. Ly mu nc t cc vi ca h thng cp nc
Chn nhng vi cp nc trc tip t cc ng ng chnh, khng nn ly t thng
hay bn cha. M cc vi tht ln v chy ra ngoi t 2 3 pht, thi gian ny nhm
ra sch h thng vi trc khi ly mu, gim tc vi nc ly mu vo trong cc
bnh cha mu.
Nu mu c ly t h thng phn phi nc ca thnh ph, khi cc vi nc
cn c x trong mt thi gian nhng cht r st c loi b ht, nh th mi m
bo mu ly c tiu biu.
2.4.1.4. Ly mu t cc ging bm tay, bm my
Bm ra vi 5 pht trc khi ly mu. Nu ging o c trang b my bm,
cng thc hin tng t nh my bm tay. Trong trng hp ging o khng c my
bm, mu c ly trc tip t ging bng cch buc chai ly mu vo 1 vt nng ri th
xung y ging. Phi cn thn vi vt nng trnh nhim bn.
2.4.1.5. Ly mu nc ung

10

Ly mu giai on ca qu trnh sn xut, cc v tr phn phi mu nc ung phi


chn lc m bo s tch lu ca h thng trong sut mi thng. V tr ly mu c th l
cc vi nc cng cng, cc ni kinh doanh ngnh thc phm, hay vi nc gia nh.
i vi nc ao h, cc mc ch s dng s quyt nh phng thc ly mu, v
nc ao h thay i theo ma, su, lu lng...
c bit vi nc thi, nng cht bn cn c kh nng thay i theo gi sinh hot,
gi sn xut ca nh my, sn phm, lu lng, mc pha long. Do ly mu tng
hp (ly mu nhiu v tr khc nhau) l tt nht nh gi mc nhim quanh vng
kho st.
2.4.2. Bo qun mu
mu nc khi phn tch vn gi c trng thi ban u ca n, tc l c thnh
phn, hm lng ca cc thnh phn ca cc hp cht v cc tnh cht vn ging nh khi
ly n ti thi im v a im ly mu.
Nhit v pH ca nc l hai i lng b bin i nhanh nht, v vy hai ch tiu
ny phi c kim ngay ti ch.
Hm lng ca cc kh ha tan trong nc nh O2, CO2, H2S, Cl2... cng thay i rt
nhiu v chng s b bay khi nc trong qu trnh vn chuyn v bo qun mu. V vy
hm lng ca cc kh cng cn c xc nh ngay.
Khi khng phn tch mu ngay th phi chn nhng bnh ng quy cch ng mu
nh bnh bng PE ti
Bng 1.5.2. Cch bo qun mu nc
Thng s

pH

TSS
c

Loi bnh

K thut bo qun

Ni phn tch

Poliester,

Thp hn nhit khi

o ti ni ly mu,

thu tinh

ly mu

phng th nghim

cha

Poliester,
thu tinh
Poliester,
thu tinh

Thi gian
bo qun
Phn tch
cng sm
cng tt

Phng th nghim

48 gi

Phng th nghim

Bo qun
lnh trong

11

Thng s

Loi bnh
cha

K thut bo qun

Ni phn tch

Thi gian
bo qun
24 gi

dn

Poliester,

in

thu tinh

DO

COD
BOD
Amoniac
Nitric

Nitrat
Photphat
Clorua
Sunphat

Chai DO

2 5oC

o ti ni ly mu,

gi ni ti

phng th nghim

Acid ho n pH<2

thu tinh

bng H2SO4, 2 5oC

thu tinh

Phng th nghim

24 gi

Phng th nghim

24 gi

Phng th nghim

24 gi

Phng th nghim

24 gi

2 5oC

Phng th nghim

1 tun

2 5oC

Phng th nghim

1 tun

2 5oC

Phng th nghim

24 gi

Phng th nghim

24 gi

Phng th nghim

24 gi

2 5oC

Poliester,

Acid ho n pH<2

thu tinh

bng H2SO4, 2 5oC

Poliester,

Lc ti ch bng mng

thu tinh

lc 0.45 m, 2 5oC

Poliester,
thu tinh

acid,

Poliester,

kim

thu tinh

Nhm

Poliester

St

Thu tinh

cng tt

5 ngy

bng H2SO4, 2 5oC

thu tinh

cng sm

Phng th nghim

2 5oC

thu tinh

Poliester,

Phn tch

24 gi

Acid ho n pH<3

thu tinh

24 gi

Phng th nghim

Poliester,
Poliester,

phng th nghim

C nh oxy ti ch v

Poliester,
Poliester,

o ti ni ly mu,

Lc ngay khi ly mu,


acid ho n pH<2
Lc ngay khi ly mu,
acid ho n pH<2
12

Thng s

Loi bnh
cha

Canxi,

Poliester,

Magie

thu tinh

K thut bo qun

Ni phn tch
Phng th nghim

2.4.3. Mt s hnh nh ly mu nc sng ti sng Bnh Li

Hnh 1. 1 Sng Bnh Li

Hnh 1. 2 a ch ly mu

13

Thi gian
bo qun
24 gi

Hnh 1. 3 V tr ly mu 1

Hnh 1. 4 V tr ly mu 2

Hnh 1. 5 V tr ly mu 3

14

Hnh 1. 6 V tr ly mu 6

Hnh 1. 7 S v tr ni ly mu

15

Chng 3
CNG THC NGHIM V D TON CHI PH

3.1. Mc tiu ti
Kho st cc yu t nh hng n quy trnh xc nh hm lng COD trong nc
bng phng php permanganat v kalidicromat.
3.2. Ha cht, dng c v thit b thc nghim
3.2.1. Ha cht xc nh hm lng COD
-

Kali Dicromat (K2Cr2O7)

12,2620g

Kali Permanganat (KMnO4)

3,1764g

St (II) Amoni Sunfat [(NH4)2Fe(SO4)2.6H2O]

100g

St (II) Sunfat (FeSO4.7H2O)

0.7g

Acid Oxalic (H2C2O4.2H2O)

6,303g

1-10 Phenantrolin (C12H8N2.H2O)

1,485g

Bc Sunfat (Ag2SO4)

10g

Thy Ngn Sunfat (HgSO4)

80g

Acid Sunfuaric [H2SO4 (d = 1,84)]

1500Ml

Dung dch KMnO4 0.01N: Cn chnh xc 3.19 g KMnO4 P.a, pha trong 1 L nc
ct. un nng nh dung dch v yn khong 24 gi, sau lng, gn y phn
dung dch pha trn cho vo chai ti, bo qun ni ti. Trc khi s dng phi chun
li bng acid oxalic (H2C2O4).

Dung dch chun Kali dicromat: Dung dch K2Cr2O7 0,0167M. Cn 4,931g
K2Cr2O7 c sy 103oC trong 2 gi ngui n nhit phng trc , ha
tan vi 500mL nc ct, thm 167mL H2SO4 v 33,3g HgSO4, pha long ri
ngui sau thm nc ct cho 1000mL.

Dung dch FAS chun: FAS 0,25M: Cn chnh xc 98g Fe(NH4)2(SO4).6H2O ha


tan trong mt t nc ct v 20mL H2SO4, lm ngui v nh mc cho 1L. nh
phn li trc khi s dng pha long 10mL dung dch K2Cr2O7 0,0417M thnh 100mL

16

vi nc ct, thm vo 30mL dd H2SO4, lm ngui trc khi dng dd FAS nh phn,
ch th mu ferroin (2-3 git).
-

Ch th mu ferroin: Ha tan 1,485g 1,10-phenathrolin monohydrate v 0.695g


FeSO4.7H2O trong nc ct cho 100mL.

Dung dch H2SO4: Trong 500mL H2SO4 thm 5,5g AgSO4, yn 1-2 ngy cho
n khi tan hon ton.

3.2.2. Dng c v thit b thc nghim


Dng c bp ph mu COD v mt s dng c thy tinh thng thng phng th
nghim
3.3. Thc nghim
3.3.1. Phm vi p dng
Ch p dng cho mu nc nhim nh v nng clorua < 300 mg/L (EC < 1200
S/cm).
3.3.2. Nguyn tc
3.3.2.1. Nguyn tc xc nh COD bng phng php Kali Permanganat
Da vo kh nng oxy ha mnh ca KMnO4 trong mi trng acid. Da vo lng
KMnO4 cho vo mu nc th ban u v lng KMnO4 cn li sau phn ng ta c th
xc nh c lng cht hu c c trong mu nc th.
MnO4- + 5e + 8H+ = Mn2+ + 4H2O
Lng MnO4- cn d sau phn ng c xc nh bng dung dch (COOH)2
2MnO4- + 5(C2O4)2- + 16H+ = 2Mn2+ + 10CO2 + 8H2O
3.3.2.2. Nguyn tc xc nh COD bng phng php Kali Dicromat
Dng phng php chun oxy ha - kh xc nh COD. Trong mi trng acid
H2SO4 m c cc hp cht hu c s b oxy ha hon ton bi K2Cr2O7 vi iu kin un
nng mu nhit 105oC trong 3 gi, trong mi trng acid. Bng cch cho mt lng
K2Cr2O7 d chnh xc oxy ha hon ton tng hm lng hp cht hu c. Chun lng
d K2Cr2O7 bng dung dch chun Fe2+ vi ch th ferroin, im tng ng nhn c khi
dung dch chuyn t mu xanh lam sang mu nu .
Phng trnh phn ng
17

CnHaOb + cCr2O72- + 8cH+ nCO2 +

(a + 8c)
H2O + 2cCr3+
2

Vi c = (2n + a/2 + 4c)/7


3.3.3. Kho st cc yu t nh hng v khc phc
3.3.3.1. i vi phng php Manganat (KMnO4)

Phn ng cng b nh hng bi ion Cl- (ln hn 300 mg/L) , Cl- s phn ng vi
KMnO4 to thnh Cl2 .V th khng th p dng phng php permanganat cho nhng
mu nc l hay nc mn.
-

2+

10Cl + 2MnO4 + 16H 2Mn + 5Cl2 + 8H2O

Cc hp cht v c (H2S, Fe2+) c th phn ng vi permanganat


2+

2+

3+

5Fe + MnO4 + 8H Mn + 5Fe + 4H2O


3.3.3.2. i vi phng php Kali dicromat
-

Cc hp cht bo thng, hydrocacbon nhn thm v pyridine khng b oxy ha.


Khc phc: Cn cho thm Ag2SO4 vo phn ng xy ra d dng hn vi hiu sut
ln ti 85 - 90% tuy nhin ch oxy ha c ru v hydrocarbon mch thng.

Ion Cl- cng l mt yu t gy tr ngi cho phn ng cng c th b oxy ha theo


phn ng sau:
6Cl- + Cr2O72- + 14H+ 3Cl2 + 2Cr3+ + 7H2O
Khc phc: cho thm HgSO4 vo mu vi t l HgSO4 : Cl- l 10:1 trc khi un

Ngoi ra cn c ion nitric, Fe2+, SO32- cng gy cn tr cho qu trnh xc nh COD.


Nhng nh hng ny khng thng xuyn v cng khng ng k nn c th b qua

3.3.4. Tin hnh kho st


3.3.4.1. Kho st xc nh mu tht bng phng php Kali Permanganat
Cho vo erlen 250mL ( ra sch v sy kh) 50mL mu nc , thm vo 5mL
H2SO4 1:2, thm ng 10mL dung dch KMnO4 0,01N (mu nc c mu hng). Sau
un si 10 pht trn bp in, nhc xung ch cho nhit h xung 80 - 90 oC ri thm
vo 10mL dung dch (COOH)2 0,01N lc u cho mu nc mt mu ri dng dung dch
18

KMnO4 0,01N chun cho n khi mu nc chuyn t khng mu sang mu hng


nht th kt thc chun . Ghi th tch lng KMnO4 tiu tn: V1.
Thay mu nc th bng 50mL nc ct th nghim mt mu trng. Cc bc tin
hnh th nghim c thc hin nh trn. Th tch tiu tn ca KMnO4 mu trng V2.
3.3.4.2. Kho st xc nh mu tht bng phng php Kali dicromat
-

Ra ng COD v np bng dd H2SO4 20% trc khi s dng

Chn th tch mu v ha cht theo bn hng dn sau:


Kch thc ng

Vmu tht (mL)

DD K2Cr2O7
(mL)

H2SO4 (nL)

Vtng cng (mL)

16 x 100 (mm)

2,5

1,5

3,5

7,5

20 x 150 (mm)

5,0

3,0

7,0

17,0

25 x 150 (mm)

10,0

60,0

14,0

30,0

ng chun 10 mL

2,5

1,5

3,5

7,5

Cho vo ng nghim: mu, dd K2Cr2O7 0,1N v H2SO4. Lu phn ng xy ra mnh


nn cn cho acid cn thn, chy dc theo ng nghim. sau lc mu tht u

Lm tng t mu trng (thay mu bng nc ct)

Cho ng nghim vo my COD, nung nhit 150oC trong vng 2 gi.


Ch : nung km theo 1 ng mu trng nhit 150oC.

ngui n nhit phng, ra erlen, thm 2 git ch th ferroin v nh phn


bng FAS 0,1N. Kt thc phn ng khi dung dch chuyn t mu xanh lc sang nu
.

Thay th tch mu nc tht nh bng trn bng nc ct th nghim mu trng.


Cc bc tin hnh th nghim c thc hin nh trn. Th tch tiu tn ca FAS
tiu tn mu trng V2.

3.3.5. Tnh ton kt qu


19

3.3.5.1 Tnh ton kt qu bng phng php Kali Permanganat


Hm lng COD c trong mu nc c tnh theo cng thc sau:
[COD] =

(V2 - V1 ) N S 1000
(mg/L)
V

Trong :
V1: Lng th tch KMnO4 tiu tn lc chun mu tht (mL)
V2: Lng th tch KMnO4 tiu tn lc chun mu trng (mL)
N: Nng ca dung dch KMnO4
S: ng lng gam ca oxy
V: Th tch mu nc thi ly phn tch (mL)
3.3.5.2. Tnh ton kt qu bng phng php Kali Dicromat
Hm lng COD c trong mu nc c tnh theo cng thc sau:
[COD] =

(V2 - V1 ) N S 1000
(mg/L)
V

Trong :
V1: Lng th tch FAS tiu tn lc chun mu tht (mL)
V2: Lng th tch FAS tiu tn lc chun mu trng (mL)
N: Nng ca dung dch FAS
S: ng lng gam ca oxy
V: Th tch mu nc thi ly phn tch (mL)

20

3.4. Bng kt qu phn tch


3.4.1. Bng kt qu phn tch ca phng php Kali Permangant
Ngy phn tch

7/3/2012

9/3/2012

12/3/2012

21/3/2012

Ngy ly mu

7/3/2012

9/3/2012

12/3/2012

21/3/2012

Ni phn tch

F2.05

F2.05

F2.05

F2.05

Nhit phng (oC)

30oC

29.5oC

30oC

29oC

50

50

50

50

V 2 (mL)

9.53

9.73

9.57

9.6

V 1 (mL)

9.03

8.93

8.63

8.8

Kt qu

0.8

1.28

1.504

1.28

Vly mu (mL)

Nhn xt
3.4.2. Bng kt qu ca phng php Dicromat
Ngy phn tch

14/3/2012

Ngy ly mu

14/3/2012

Ni phn tch

F2.05

F2.05

F2.05

F2.05

Nhit phng (oC)

31oC

31oC

31oC

31oC

Vly mu (mL)

2.5

5.0

10.0

2.5

V2 (mL)

5.8

10.2

5.7

V1(mL)

6.5

7.4

5.8

Kt qu

64

60

56

72

Nhn xt
Ngy phn tch

21/3/2012

Ngy ly mu

21/3/2012

Ni phn tch

F2.05

F2.05

F2.05

F2.05

Nhit phng (oC)

30oC

30oC

30oC

30oC

2.5

5.0

10.0

2.5

Vly mu (mL)

21

V2 (mL)

7.2

11

5.8

V1(mL)

5.8

8.6

Kt qu

80

56

48

64

Nhn xt
3.5. Hnh nh phn tch mu

Hnh 2. 1 Mu acid ha chun b un

Hnh 2. 2 Nhit phng

22

Hnh 2. 3 o pH trc khi un

Hnh 2. 4 ang un mu trng

Hnh 2. 5 un mu c vi pht
23

Hnh 2. 6 Nhit si u tin ca mu

Hnh 2. 7 Mu sau khi un

Hnh 2. 8 Ch h nhit 80 - 90oC

24

Hnh 2. 9 Cho acid H2C2O4 mu t mu hng chuyn thnh khng mu

Hnh 2. 10 Bt u chun bng KMnO4

Hnh 2. 11 Chun gn ti im tng ng

25

Hnh 2. 12 Kt thc chun mu t khng mu chuyn sang mu hng nht

Hnh 2. 13 o pH sau chun

Hnh 2. 14 Th tch tiu tn chun mu trng

26

Hnh 2. 15 Bp ph mu COD

27

Chng 4
KT LUN V KIN NGH

T nhng nghin cu v kho st trnh by, chng ta rt ra kt lun v kin ngh nh


sau:
4.1 Kt lun
Qua kho st 2 phng php ta thy phng php Kali dicromat s cho kt qu chnh
xc cao hn v:
Cc hp cht bo mch thng, hydrocacbon nhn thm v pyridine khng b oxy ha,
mc d phng php Kali dicromat hu nh oxy ha hon ton hn so vi phng php
dng KMnO4. Cc hp cht bo mch thng b oxy ha d dng hn khi thm Ag2SO4 vo
lm cht xc tc, nhng bc d phn ng vi cc ion h halogen to kt ta v cht ny
cng c th b oxy ha mt phn.
Khi c kt ta halogen, c th dng HgSO4 to phc tan vi halogen trc khi un
hon lu. Mc d, 1 g HgSO4 cn cho 50 ml mu, nhng c th dng t hn khi hm lng
chloride < 2.000 mg/l
4.2 Kin ngh:
Ty vo mu nc ta c th dng phng php Kali dicromat hay Kali permanganat,
mc d phng php Kali dicromat thi gian phn tch lu hn phng php Kali dicromat.
Tuy nhin thc t ngi ta vn dng phng php Kali dicromat nhiu hn v phng php
ny s cho ra sai s ch hn v hn ch c cc yu t nh hng nhiu hn so vi
phng php Kali permangat.

28

TI LIU THAM KHO

[1]

TCVN 5981-2 (ISO 6107-2), Cht lng nc Thut ng - Phn 2

[2]

TCVN 6491 : 1999 (ISO 6060 : 1989), Cht lng nc Xc nh nhu cu oxi ha
hc

[3]

TCVN 4565 88, Nc thi Phng php xc nh oxy ha

[4]

TCVN 5945 2005, Nc thi cng nghip Tiu chun thi

[5]

TCVN 6772 : 2000, Cht lng nc Nc thi sinh hot Gii hn nhim cho
php

[6]

TCVN 1609 : 1988 Dng c o dung tch bng thu tinh dng trong phng th nghim
Buret.

[7]

ISO 385 -1 : 1984 Dng c thu tinh phng th nghim Buret Phn 1 : Yu cu
chung.

[8]

ISO 5790 : 1979 Sn phm ho cht v c dng trong cng nghip Phng php
chung xc nh hm lng clorua Phng php thu ngn.

[9]

Th.s Hunh Th Minh Hin, Gio trnh phn tch cng nghip 3, Khoa Cng Ngh
Ha Hc, Trng H Cng Nghip Tp.HCM

29

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