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Khoa:Cng ngh ha
B CNG THNG
TRNG I HC CNG NGHIP H NI
H Ni 5-2013
LI CM N
GVHDiNguyn Thi Thoa
Page 1
SVTH:Ph Th Nga
Khoa:Cng ngh ha
Page 2
SVTH:Ph Th Nga
MC LC
T VN
Nc l mt ti nguyn thin nhin v cng quan trng i vi con ngi, sinh
vt. Ngoi nhng ng dng ca n trong i sng sinh hot hng ngy, n cn c
ngha to ln trong nhiu lnh vc khc nh: giao thng, xy dng, ha hc, y t, sn
xut,...Trong phi ni n tm quan trng ca nc ct. Nc ct c s dng rng
ri trong ngnh y t, gio dc, cc phng th nghim,...nh pha ch thuc tim, thuc
ung, bit dc, ra dng c y t, ra vt thng, pha ch ha cht, ra dng c th
nghim, tin hnh phn tch cc ch tiu ha hc,...Hin nay vic ch to ra nc ct
ch yu c thc hin bng cc thit b dng in hoc nhit nn ch ph nng lng
v lng pht thi gy nhim mi trng tng cao. a s phng th nghim ca cc
trng hc u c my ct nc bang in cung cp nc ct ti ch cho hc sinh, sinh
vin hc tp v tin hnh th nghim. Ti phng th nghim ca trng i Hc Cng
Nghip H Ni cng ang s dng phng php iu ch nc ct ny. Thc t hin
nay vn nng lng ti Vit Nam ni ring v th gii ni chung ang l vn
c quan tm hng u. Chnh v vy vn c nhiu ngi quan tm l nghin
cu cc phng php x l nc n gin li khng gy nh hng ti mi trng, tit
kim c chi ph nng lng, nng cao hiu qu kinh t, c th p dng c cho mt
s phng th nghim nh dng nng lng t nhin, phng php trao i ion bng
nha ionit,... Trong bi lun vn tt nghip ny em la chn ti phn tch nc trc
v sau x l qua ct lc ionit v so snh vi nc ct 1 ln.
Bi kha lun ny em tm hiu v trnh by mt s vn sau:
Khoa:Cng ngh ha
Page 5
SVTH:Ph Th Nga
Khoa:Cng ngh ha
thnh phn lng vt; phi c sn xut, v d nh bng cch chng ct nhiu ln,
hoc bng cch kh ion ha hoc thm thu ngc sau chng ct.
Nc loi 3:
Ph hp vi hu ht cc phng th nghim lm vic theo phng php t v
iu ch cc dung dch thuc th; phi c sn xut bng cch chng ct mt ln,
kh ion ha hoc thm thu ngc. Neu khng c quy nh no khc, loi ny c
dng cho phn tch thng thng.
Ch thch: ngun nc cung cp ban u l nc ung c v sch. Nu nc b
nhim ban nng v bt k phng din no, cng cn phi c x l trc.
- Yu cu
Nc phi tho mn y cc hn mc v yu cu trong bng sau. Cch th
c tin hnh bng cc phng php quy nh phn di.
STT
1
110c , tnh
bng
Mc cc
loi ch tiu
mg/kg,
ln hn Loi 2
Loi khng
1
Tn ch tiu
pH 25c phm
vi bao hm
dn in 25c
tnh bng mS/cm,
khng ln hn
Loi 3
5,0-7,5
0,02
Khng quy
nh
0,5
*Ch thch:
Cht oxi ha, hm
o Do nhng
khn trong vic gi tr pH ca nc tinh khit cao v gi tr o
lng oxi(O) tnh Khng
p dngkh
(xem
0,08
0,4
cthch
khng
bng mg/1, khng ln
ch
3) chc chan, nn khng quy nh gii hn pH ca nc loi 1 v
loi 2.
hn
o
Gi
tr dn in ca nc loi ! v loi 2 ng vi nc va iu ch xong;
hp th
trong bo qun nc c th b nhim bn bi cacbon trong kh quyn v cht
254nm,chiu dy lem,
Khng
quy
kim
ca bao b thu tinh0,01
tan vo nc,
dn ti
nhng thay i dn in.
0,001
tnh bang n v hp
nh
o Khng quy nh gii hn cht oxy ha c v cn sau khi bay hi ca nc
th, khng ln hn
loi I v kh c php th ph hp mc tinh khit ny. Tuy nhin, cht lng
ca nc c bo m do s ph hp vi cc yu cu khc v do phng
Hm lng cn sau Khng p dng (xem
1
2
php iu ch.
khi bay hi
ch thch 3)
- Ly mu
Ly t' l nc ln mt mu nc i din khng t hn 21 kim tra theo quy
nh ny.
Ch thch:
o Mau ny c dng kim tra dn in ca nc loi I v loi 2. o Mau
phi trong mt binh cha thch hp, sch s, kn ch dnh ring ng mu
GVHDiNguyn Thi Thoa
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SVTH:Ph Th Nga
Khoa:Cng ngh ha
nc, c kch thc sao cho mu cha y hon ton. Phi gi gn cn thn
trnh mi nguy c nhim bn mu. o C th dng cc bnh cha g ha (c
ngha l bnh cha c luc si t nht 2h trong dung dch axit clohydric C(HC1) 1 mo 1/1; sau hai ln mi ln lh trong nc ct; lm bng thu tinh bosilicat
cng nh cc bnh cht do tr thch hp. (V d polietilen polypropylen) nhng
ch yu phi m bo mu khng b nh hng do bo qun, c bit l i vi
cht oxy ha v hp th.
Bo qun
Trong bo qun, nc c th b nhim bn do ho tan nhng thnh phn d tan
ca bnh cha bng thy tnh hay cht do hoc do hp th cacbon dioxit v
cc tp cht khc ca kh quyn trong phng th nghim. V l do trn, khng nn bo
qun nc loi I v loi 2: nc sau khi iu ch c dng ngay nh quy nh 2: nc
sau khi iu ch c dng ngay nh quy nh. Tuy nhin, nc loi 2 c th c iu
ch vi lng va phi v bo qun trong cc bnh cha thch hp, tr, sch, kn, y
v c trng bng nc cng loi.
Vic bo qun nc loi 3 khng phc tp, nhng cc bnh cha v iu kin bo
qun phi ging nh vic b qun nc loi 2.
Bnh cha bo qun chi nn dnh ring cho mt loi nc.
Phng php th
Cc php xc nh quy nh trong mc ny phi c tin hnh trong mt kh
quyn khng c bi, sch v phi c nhng bin php thn trng thch hp ngn
nga mi nhim bn mu v cc phn mu th.
o pH +
Thit
b
Thit b thng thng trong phng th nghim v pH mt, c trang b mt in
cc thu tinh v mt in cc so snh AglAgCl.
+ Cch tin hnh
Chun ha pH mt theo hng dn ca ngi sn xut, dng cc dung dch m
c gi tr pH t 4,0 n 8,0. Chuyn mu th nghim vo cc v iu chinh nhit ca
nc n 25 1 c. Nhng cc in cc v xc nh pH.
dn in +
Thit b
Tht b thng thng trong phng th nghim.
>
Bnh nn, c mt ng bo him cha cc ht vi-xt h ch th.
> My o dn in vi bnh o dch chuyn c, l loi binh o dn in
trc tip c b chinh nhit t ng, o nc loi 1 v loi2.
GVHDiNguyn Thi Thoa
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SVTH:Ph Th Nga
Khoa:Cng ngh ha
Page 8
SVTH:Ph Th Nga
Khoa:Cng ngh ha
Page 9
SVTH:Ph Th Nga
Khoa:Cng ngh ha
ngui, ra cht nng chy dnh mt di ca np bng nc nng, thu vo chn; sau
ho tan khi nng chy bng nc nng, ngui, chuyn dch dung dch vo mt
bnh nh mc dung tch 1000 mi, pha long n vch v lc k.
Chuyn dung dch vo bnh cht deo bo qun 1 ml dung dch chun ny cha
1 mg SO.
>
Silic dioxit dung dch chun II (dung dch long).
Chuyn 5,0 rnl dung dch chun silic dioxit (6.6.1.1) vo mt bnh nh mc dung
tch 1000 ml, pha long n vch v lc k.
lml dung dch chun ny cha 0,005 mg Si02. Khi no dng mi pha dung dch ny.
>
Amon molip t trong mt hn hp 80ml nc v 20ml dung dch axit sunurc
(6.6.1.5), khng un nng. Bo qun trong bnh cht do.
>
4-metylamino phenol sunat (Metol) dung dch ch th.
Ho tan 0,2 g metol v 20 g kali disunit (kali metabisunt) trong 100 ml nc,
khng un nng, bo qun trong chai cht do.
Loi b dung dch sau 4 tun hoc khi bt u c du hiu phn hy.
'r Axit sunfuric,C(H2S04) khong 2,5 tnol/1 - sunfuric, d = 1,84 g/ml vo nc va
c 1000 ml dung dch. Bo qun trong binh cht do.
>
Axit oxalic, dung dch 50 g/1.
+ Thit b
Thit b ca phng th nghim thng thng
>
a bng bch kim, c dung tch khong 250 ml
>
Cc ng Netsle ging nhau, dung tch 50 ml
>
L nung c th t 300 400c.
>
Bp cch thu, c th t khong 60QC.
+ Cch tin hnh
>
Mu th
Ly 520 ml nc loi 1 hoc 270 ml nc loi 2.
>
Th
Cho bc hi mu th trong a lin tip tng t mt c c mt th tch nc
cui cng l 20 ml. Thm vo 1 ml dung dch amoni molipdat. Sau ng 5 pht, cho
thm lml dung dch axit oxalic v trn k. sau 1 pht, thm vo lml dung dch metol v
un nng trong 1 pht trn bp cch thu, gi khong 60c. Chuyn dung dch vo
mt trong cc ng Netsle.
Chun b mt dung dch mu chun theo cng cch tin hnh nhng dng mt
hn hp 19,0 ml mu v 1,0 ml dung dch chun silic dioxit thay cho 20ml c c do
lm bc hi mu th. Chuyn dung dch vo mt ng Nesle khc.
Page 10
SVTH:Ph Th Nga
Khoa:Cng ngh ha
Nhn thng t trn xung, kim tra cng mu xanh to nn trong dung
dch th khng vt qu cng mu to nn trong dung dch chun. Bin bn th
nghim
Mi bin bn phi bao gm cc c trng sau y:
K hiu mu.
Thm 0,1 ml dung dch xanh bromothymol (TT) vo 10 ml ch phm. Dung dch
khng c c mu xanh lam.
Amoni: khng qu 0,2 phn triu. Ly 20 nil ch phm, thm 1 ml thuc th
Nessler (TT), sau 5 pht kim tra bng cch nhn theo chiu dc ng nghim. Dung
dch khng c c mu m hn mu ca dung dch i chiu c tin hnh ng
thi bng cch thm 1 ml thuc th Nessler (TT) vo hn hp gm 4 ml dung dch
amoni mu 1 phn triu v 16 ml nc khng c amoni.
Clorid: ly 10 ml ch phm, thm 1 ml dung dch acid nitric long (TT) v 0,2
ml dung dch bc nitrat 2% (TT). Dung dch khng c thay i trong t nht 15 pht.
Nitrat: khng qu 0,2 phn triu. Ly 5 ml ch phm vo mt ng nghim, ngm
su trong nc , thm 0,4 ml dung dch kali clorid 10% (TT), 0,1 ml dung dch
diphenylamin (TT) v 5 ml acid suluric m c khng c nit (TT) (va nh tng
git va lc), trong cch thu 50 c trong 15 pht. Dung dch thu c khng c
c mu xanh m hn mu ca dung dch i chiu c tin hnh trong cng iu
GVHDiNguyn Thi Thoa
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SVTH:Ph Th Nga
Khoa:Cng ngh ha
Page 12
SVTH:Ph Th Nga
Khoa:Cng ngh ha
Page 13
Khoa:Cng ngh ha
Page 14
Khoa:Cng ngh ha
Mt s thit b do dn in
Page 15
Khoa:Cng ngh ha
Page 16
Khoa:Cng ngh ha
Khong o p sut ring phn: 0 ... 200.0 mbar / 0 ... 1250 mbar
phn gii: 0 . 1 / 1 mbar
chnh xc (1 dgit): 0.5%
Chc nng b tr' nhit , mn v p sut khng kh 500 ... 1100 mbar
- Khong o nhit : -10.0c ... +120c
- chnh xc (1 digit): 0.1 c
2.3.3.2.
THIT B O DN IN EC 215
EC 215 l thit b o dn in a phm vi b nhit t ng cng vi bn phm
v o m bo phn gii v chnh xc cao nht p ng yu cu ca bn.
Hiu chun c thc hin n gin bng tay ln n im 1 ch bng cch iu
chnh mt nt bm trn mt trc ca thit b o. Vi mt h s nhit do ngi s
dng la chn v cm bin nhit kt hp
trong vic thm d, b nhit hin th s.
Bao gm dng c o ny l phn ng
nhanh chng vic thm d ca HI 76303.
Vic thm d ny c trang b mt b cm
bin bch kim 4 vng, cm bin nhit tch
hp bn trong v Im dy (3,3T). Thit b ny
c th c s dng o tnh axt, mau kim,
hoc nhit cao.
Thng s k thut:
Page 17
Hiu chun
1 im bng tay
T ng, 0 - 5 0 (32 - 122F) vi B iu
chnh 0 - 2.5%/C
H 76303, cm bin bch kim 4 vng, cm
Khoa:Cng ngh ha
bin nhit , 1 m dy (3.3') (bao
gm)
0.0 - 199.9 pS/cm; 0 - 1999 pS/cm; 0.00 Thit
b tch hp0.0
12-Vdc
(bao
gm)
19.99mS/cm;
199.9
mS/cm
dn in
0 - 50C (32 - 122F); RH ti a 95%
B nhit
Cc d
Kha lun tt nghip
Ngun in
Thang o
Mi trng
Kch thc
Trng lng
0.1kgpS/cm;
1.0
(2.2 lb.)
1 uS/cm; 0.01 raS/cm; 0.1 mS/cm
phn gii
chnh
xc
2.3,3.3. THTT B O DN IN
BN MODEL: YSI3100 HNG SX: YSI M
YSI 3100 c thit k dng trong phng th
nghim, cung cp kt qu c chnh xc v tin
cy cao o nc siu tinh khit, ch b nhit
t ng. Hiu chun a im. Cc chi tiu phn tch gm dn in, sut in tr, tng
cht rn ha tan TDS, mn v nhit .
Hiu chun
a im, ln ti 5 im
Cnh bo m thanh
Kt ni cm bin
0.001 ti 100 cm
Chng ch
UL, CSA, CE
ng h
Luu tr d liu
100 im
Kch thc
Kch thc
Khi lng
1.1 kg
Mn hnh
Graphic LCD
Mi trng hot ng
m 95%
Page 18
Khoa:Cng ngh ha
Cng kt ni
RS-232
Ngun in
B nhit
Phng php
10
H s nhit
- 100 c
Chng thm nc
Bo hnh
0.1
chnh xc
0 - 9.999 k
0.30% ton thang
0.20% ton thang
0 -99.99 k
0.10% ton thang
phn gii
0.1% ton thang
0.0001 pS
0.001 pS
0.1% ton thang
0.01 iS
Tn s
0.001 k
40 Hz
80 Hz
0.01 k
290 Hz
95.0 -999.9 pS
100.0 - 999.9 k
0.10% ton thang
1.00 -9.99 M
10.0-29.9
Mton thang
0.10%
1%gS
ton thang
10100.1 k
Hz 0.01 M
10100.1 M
9.50 - 99.99 Ms
Ch tiu
Thang o
0.10% ton thang
95.0 - 999.9 mS
mn
0 ti 80 ppt (NaCl)
0.30% ton thang
0.1 mS
dn in
Thang o
0 -0.9999 pS
0.950-9.999 pS
9.50 pS-99.99 pS
TDS
0.95 - 3.00 s
0.01 mS
0 ti 19,999 mg/L
Nhit
ton thang
-5 ti 100c
1.0%
0.01
Sut in tr'
Thang o
chnh xc
phn gii
0-9.999 Q
0.001
0 -99.99 Q
0.01 Q
Page 19
1010
Hz
1010
chnh xc
Hz
1460
.l ppt
Hz
0.50%
1460
0.1 C
Hz
Hz
1010
Hz
1010
Hz
290 Hz
80 Hz
40 Hz
phn
gii
0.1 ppt
1 mg/L
0.01
Tn s
1460
Hz
1460
Hz
SVTH:Ph Thi Nga
Khoa:Cng ngh ha
Page 20
Khoa:Cng ngh ha
3.1.2.
Phng php quang ph hp th nguvn t
3.1.2.1.
Nguyn tc
e gim s nhiu, thm lantan clorua (nu dng ngn la khng kh/axetylen) trc khi
o bng phng php quang ph hp th nguyn t. i vi Ca s hp th o
422,7nm v Mg 285,2nm.
3.1.2.2.
iu kin tin hnh
Phng php ny dng phn tch nc ngun v nc ung v c th dng
phn tch nc c hm lng canxi ln ti 50 mg/1, magie ln ti 5 mg/1. i vi
mu c hm lng canxi v magie cao hn th th tch mu ly phn tch phi
nh hn.
Dng ngn la ca hn hp khng kh/axetylen thm lantan clorua. Dng ngn la
ca hon hp oxit nito/axetylen th thm cesi clorua.
Cc mu sau khi axit ha phi lc trnh tc h thong mao qun.
Dng ngn la ca hn hp khng kh/axetylen khong tt nht t 3 - 50 i vi
caxi v t 0,9 - 5 i vi magie. Dng ngn la oxit nito/axetylen khong tt nht
t 2 20 i vi canxi v t 0,2 2 oi vi magie,
3.1.2.3.
Cch tin hnh
Chun b dung dch th cho thit b: chun b mt s bnh nh mc lOOml. Nu
dng ngn la khng kh/axetylen thi thm vo mi bnh lOml dung dch lantan
clorua cha 20g La/1, hoc lOml dng dch cesi clorua cha 20g Cs/1 nu dng
ngn la oxit nito/axetylen.
Thm lng mu ph hp vi khong nng vo bnh.
Thm HC1 0,1 mol/1 ti vch.
Tin hnh o bc sng 422,7 nm vi canxi v 285,2 i vi magie. Tin hnh
tng t vi mu trng.
Lp th hiu chnh i vi canxi nng t 0; 0,5; 1,0;...5,0 v magie nng
t 0; 0,05; 0,1; . ..;0,5.
3.1.2.4.
Tnh kt qu
Hm lng canxi (PCAI)V magie (pMgl), mg/1 theo cng thc:
Page 21
^l
Vn
pMgl - PMg2 v
PCal = PCa2 ,,
Khoa:Cng ngh ha
Trong :
PCA2 ' nng ca canxi, mg/1 (theo th hiu chnh) p Mg2 l nng ca magie, mg/1
(theo th hiu chnh)
f: h s pha long bi vic thm HC1, p=l,l8g/ml vo mu th (thng thng l 1,008)
v0 l th tch ca mu th gc, ml
V] l th tch ca bnh nh mc, ml (lOOml)
Hm lng ca canxi (Cca) v magie (CMg), mmol/1 c tnh theo cng thc:
Pca
P-Cai
40,1
_ p- Mgi
PMg 24,3
3.2.1.
Phng php chng ct v chun
3.2.1.1. Nguyn tc
iu chinh pH ca phn mu th n khong 6,0 - 7,4. Thm magi oxit to
mi trng kim yu, chng ct amoniac c gii phng v thu vo binh cha c sn
dung dch axit boric. Chun amoni trong phn ct c bang dung dch chun axit
boric/ch th.
3.2.1.2. iu kin tin hnh
p dng cho nc cha x l, nc ung, nc thi nng amoni tnh theo nito
ti I Omg/I.
u ra ca ong sinh hn phi nhng ngp vo dung dch hp th.
Phi lm sch my chng ct mi khi my ngng lm vic trong t ngy Lng
axit trong bnh hng phi lun du so vi lng amoni
3,2.1.3, Cch tin hnh
Chn the tch phn mu th nu bit s b hm lng amoni gn ng trong mu
theo bng sau:
Nng amoni CN (mg/1)
Th tch phn mu th (ml)
250
0-10
10-20
20-50
50-100
100
50
25
Page 22
Khoa:Cng ngh ha
CN = LMG/1
CNHJ= LMG/1
CNH4 = LMG/1
CNH3
MG/1
4+ MG/1
0, 823
1,216
1
1,288
1,059
0,777
0,944
Page 23
C(MH4+)
MMOL/1
71,4
58,7
55,4
C(NH4+)- lmg/1
0,014
0,017
0,018
Khoa:Cng ngh ha
Th d:
Nng ion amoni CNH4 1 mg/1 tng ng vi nng nit l 0,777mg/l.
3.2.2.
Phng php trc ph dng thuc th Nessler
3.2.2.1. Nguyn tc
Khi thuc th Nessler c cho vo dung dch th amoni s phn ng rt nhanh vi
tc nhn ny to ra phc mu vng nu. Tuy nhin khng phi ton b lng amon u
phn ng ngay lp tc cho nn cn c thi gian dung dch pht trin mu ti a.
Cng mu t l thun vi hm lng amoni ong dung dch th. o hp th
quang bc sng = 400nm.
Phng trnh phn ng:
2NH + 2K [Hgl 1 = Hg NH I + 4K + NH !
3
2 L & 4 J &2
23
-fC
Trong :
CNH4+ l nng amoni trong mu, mg/1 f l h s
pha long nu axit bo qun mu. c l nng
amoni tnh theo ng chun, mg/1 v0 l th tch mu,
ml
V1 l th tch bnh nh mc
Page 24
Khoa:Cng ngh ha
3.3. XC NH HM LNG Fe
3.3.1.
Phng php so mu
3.3.1.1. Nguyn tc
Trong mi trng axit, ion st (III) to vi ion CNS' phc mu , em so mu
bng mt dung dch mu vi dung dch tiu chun.
3.3.1.2. iu kin tin hnh
Phi iu chnh mi trng pH v khong axit.
Thc hin so mu vi dy mu tiu chun, cc ng so mu hnh tr phi ng nht,
c cng kch thc, mu sc.
Lng dung dch vo cc ng phi tng i bng nhau.
Nng ca st trong mu phi nm trong khong nng ca dy mu tiu
chun.
Thc hin so mu bng mt.
3.3. L3.Cch tin hnh
Ht mu vo cc thy tinh, thm dung dch HNO3 ri un si khong 5 pht.
Chuyn ht sang bnh nh mc, nh mc ti vch.
Ht mt th tch xc nh dung dch va nh mc vo ng so mu.
Thm cc iu kin hin mu ri tin hnh so mu.
3.3.1.4.
Tnh kt qu
Hm lng st (III) c tnh theo cng thc:
Trong :
X l nng st trong mu, mg/1
c l nng st trong ng so mu c cng mu bng vi ng mu, mg/1 VI l th
tch bnh nh mc, ml V2 l th tch mu th, ml
3.3.2.
3.3.2.1. Nguyn tc
Thm dung dch 1.10- phenantrolin vo lng mu v o hp thu ca phc cht
mu da cam- bc sng bng 510 tim. Nu xc nh lng st tng hoc tng st
ho tan, thm hydroxyl- amoni clorua d kh st (II) n st (III). Nu c st khng tan,
oxyt st hoc phc cht st, cn phi x l s b ho tan cc cht . Phc cht st
(II)-1.10- phenantrolin bn trong khong pH t 2,5 n 6 v mu sc t l vi hm
lng Fe(II). Quan h gia nng st v hp th l tuyn tnh vi nng st nh
hon 5,0 Itig/l, hp thu cao nht khi o X - 510 ran.
GVHDiNguyn Thi Thoa
Page 25
Khoa:Cng ngh ha
CFe=F(A|-Ao)
Trong :
F l dc ca ng chun Ai l
hp th ca mu Ao l hp
th ca mu trang
3.4. XC NH HM LNG CLORA
3.4.1.
Xc nh Cl bng thy ngn thyoxyanate
3.4.1.1. Nguyn tc
Nguyn tc l ion thyocyanat ca mui thy ngn thyoxyanat b chim ch bi
ion clorit v gii phng ra ion thyoxyanat t do. vi s c mt ca ion
Fe III trong dung dch s to ra phc c mu mu. Cng mu ca phc st vi
thyoxyanat tng ng vi hm lng ion clorit trong dung dch.
2C1' + Hg(SCN>2 + 2Fe3+ = HgCl2 + 2IFe(SCN)I2*
3.4.1.2. Diu kin tin hnh
Phng php cho php xc nh lng vt anion clorit trong dung dch. Dung dch
sau khi hin mu, nh mc phi yn 10 pht ri mi em i o quang bc
sng ?i=460nm.
3.4.1.3. Cch tin hnh
Ht mt th tch chnh xc mu vo hnh nh mc
Thm cc iu kin hin mu, nh mc ti vch bang nc ct.
e yn dung dch 10 pht ri o quang bc sng =460nm.
GVHD:Nguyn Thi Thoa
Page 26
Khoa:Cng ngh ha
Trong :
X l nng clorua trong mu, mg/ml c l nng
clorua tnh theo ng chun, mg/ml V1 l th tch bnh
nh mc, ml Vo l th tch mu, ml
3.4.2.
Phng php chun vi cht chun Ag+
3.4.2.1. Nguyn tc
Phn ng ca ion cloma vi ion thm vo to thnh kt ta bc clorua khng ha
tan. Vic thm d 1 lng nh ion bc to thnh cromat mu nu vi ion cromat c
thm lm cht chi th. Phn ng ny c dng bit im kt thc. Mi trng pH
thch hp cho php chun ny l t 6,5-7.
Cc phn ng xy ra trong qu trnh chuan :
Ag+ + Cl" -^AgCl ''trng
Ag~ + Cr042' ->Ag2Cr04 '4'nu
Page 27
Khoa:Cng ngh ha
Chun dung dch bng dung dch AgN03 tiu chun n khi dung dch
chm mu nu .
3.4.2.4. Tnh kt qu
Nng clorua(Pcl), tnh bng mg/l
C.f.(V s -V b )
Fcl
~' V
Trong :
Pci: nng clorua, mg/I va:
th tch mu, ml
vb:th tch dung dch bc nitrat dng chun mu trng, ml vs;
th tch dung dch bc nitrat dng chun mu th, ml C: nng
thc ca bc nitrat, mo 1/1 f: h s chuyn i, 135453 mg/mol
3,4,3,
Phong php chun iot xc nh clo tng s
3.4.3.l.
Nguyn tc
Clo tng s phn ng vi kali iodua trong dung dch axit gii phng iot t
do.Iot va sinh ra b kh ngay bng dung dch chun thiosunfat bit, c thm
vo dung dch. Chun lng hiosunfat cha phn ng bng dung dch chun kali
iodat.
Phng trnh chun ;
KI03+Na2S203^KI+NaI+Na2S406+I2
3.4.3.2.
Page 28
Khoa:Cng ngh ha
Trong : M l khi lng mol ca clorua (M = 70,91 g/mol), tnh bng g/mol
0,0-199,9/0-1999
0,00-19,99/0,0-199,9
iu kin lm vic
Loi pin/tu th
Kch thc
Khi lng
Khoa:Cng ngh ha
cp ni c bc bo v
di lm
0-50 c m tng i
cc i 95%
9V( pin kim)/100 gi
s dng lin tc
185x82x45 mm
355g
1.1.2.2.
Thao tc s dng
- Ra sch u d bng nc ct ri dng giy mm lau kh.
- Nhng u d vo dung dch cn o sao cho dung dch ngp qua 4 l nh trn u d.
Khuy nh ui ht bt kh cn bm li trn u d
- Bt nt on/off, chn n v o ph hp vi dung dch cn o.
- i n khi gi tr hin th trn mn hnh n nh th c kt qu o
- Ghi li gi tr va o c.
1.1.3.
Cn phn tch
- Cm ngun in
- Bt 4,on/ofF\ i n khi mn hnh hin th v 0.
- M ca cn a b cn vo cn
- Khi mn hnh hin th gi tr ca b cn, nhn 4,Tare tr b
- a cht cn cn vo cn ri mang ra ngoi
- ng ca cn li
- Bm nt on/off tt
- Rt ngun in
1.1.4.
Cc dng c thng thng trong phng th nghim
V d: buret 25ml, cc thy tinh (50ml, lOOml, 250ml, ...), bnh tam gic 250ml, bnh
tam gic 500ml, b pipet 0,1 ml - 50ml, bp in, phu lc, uac thy tnh,...
1.2. Ha cht
1.2.1.
Dung dch H2SO4 c
1.2.2.
Dung dch HNOj c
1.2.3.
Dung dch NH- c
1.2.4.
m amon
Cn 9,14g NH4CI ha tan trong 500ml nc ct v ht 80ml NH4OH 25%, nh mc
bng nc ct ti 1 OOOml.
1.2.5.
Dung dch EDTA chun 0,01 M
Sy mui Na^EDTA 80c trong vng 2h, ngui trong bnh ht m. Cn
3,725g ha tan trong nc ri nh mc thnh lOOOml, bo qun trong bnh PE.
GVHD:Nguyn Thi Thoa
Page 30
Khoa:Cng ngh ha
1.2.6.
Ch thi modan en l(ETOO)
Ha tan 0,5g modan en 11, dng mui ca natri axit l(l-hydroxy-2- naphtylazo)-6nitro-2-naphtol-4-simfonic
(CSiiIisKiO-SNa)
trong
lOOml
trietanolamin[(HOCH2CH2)3N] c th thay 25ml trietanolamin bng th tch n 25ml
etanol gim nht dung dch.
1.2.7.
Dung dch chun CaC03 0,01 M
Sy CaC03 105c trong 2h ri ngui trong bnh ht m. Cn 1,001 g, tm t
bng nc, thm tng git HC1 n tan hon ton ri cho thm nc, un si vi pht
ui C02, lm ngui n nhit phng ri thm vi git metyl . Thm dung dch
NH3 cho en dung dch chuyn mu da cam. Chuyn nh lng vo bnh nh mc
lOOOml.
1.2.8.
Dung dch chun AgN03 0,02M
Cn 3,404g AgN03 ha tan vi nc, nh mc lOOOml. dung dch bo qun trong
bnh thy tinh sm mu.
1.2.9.
Dung dch K2Cr04 100g/l
Cn lOg KCrOha tan trong nc, pha long thnh lOOml
1.2.10.
Dung dch NaCl 0,02
Cn l,1688gNaCI c sy kh, ha tan v pha long thnh lOOOml
1.2.11.
Dung dch HNO3 0,1 M
Ht 3,3 ml HNO3 c pha long thnh 500ml
1.2.12.
Dung dch NaOH 0,1M
Cn nhanh 2,084g NaOH ha tan, pha long thnh 500ml
1.2.13.
Dung dch m axetat
Cn 68g CH3COONa ha tan trong 500ml nc ct v ht 72ml CH 3COOH
99,5%, nh mc bng nc ct n lOOOml
1.2.14.
Dung dch NH2OH.HCl 100g/l
Cn 50g NH2OH.HCI ha tan trong nc ct, pha long thnh 500ml
1.2.15.
Dung dch chun Fe2+ 0,lg/l
Cn 0,503g FeS04.7H20 tm t bng lml H2SO4 c, nh mc lOOOml bng
nuc ct
1.2.16.
Dung dch chun Fe2+ 10mg/l
Ht chnh xc 10ml dung dch Fc2 0,1 g/1 pha long nh mc ti lOOml bng
nc ct
1.2.17.
Dung djch 1.10-phenantrolin (C2H8N2.H20)
Cn 0,lg ch th, ha tan trong lOOml nc ct, khuy v gia nhit ti 80 c, khng
c un si. Trong trng hp khng un si th thm 2 git HC1 c khuy u cho
n khi tan ht
Page 31
Khoa:Cng ngh ha
Page 32
Thi gian
28/03/2013
dn in (pS/cm)
930
1010
920
8
9
29/03/2013
01/04/2013
02/04/2013
03/04/2013
04/04/2013
05/04/2013
08/04/2013
09/04/2013
10
10/04/2013
1120
1
2
3
4
5
1260
920
930
1340
1400
1370
Mau
Thi gian
Tc dng ra
(ml/pht)
30
40
Lu lng (lt/h) dn in
(pS/cm)
71,7
1,8
2,4
90,8
50,6
1,68
70,4
1,8
2
3
4
24/04/2013
25/04/2013
26/04/2013
27/04/2013
28/04/2013
40
2,4
91,6
6
7
05/05/2013
06- 14/05/2013
44
30
2,64
1,8
100,8
67,2
28
30
*Nhn xt: Ga tr o c nm trong khong 50-100 |j,s/cin nh hn rt nhiu so vi nc ct. Theo tiu chun Vit Nam 4851-89
(ISO 3696-1987) t yu cu v dn in ca nc loi 2, loi 3. Tuy nhin gi tr o c c n nh km.
2,1.3.1. Nc ct ln
Mau th
1
2
3
4
5
6
7
8
9
10
Thi gian
14/03/2013
15/03/2013
18/03/2013
19/03/2013
20/03/2013
21/03/2013
22/03/2013
dn in (pS/cm)
6,9
10,4
5,4
6,5
12,7
16,5
25/03/2013
26/03/2013
27/03/2013
22,8
24,6
7,3
8,0
*Nhn xt: Ga tr o c nm trong khong 5-25 pS/cm t yu cu v dn in ca nc loi 2 theo tiu chun Vit Nam
4851-89 (ISO 3696-1987) v nh hn,n nh hn so vi nc qua ct ionit.
Ngy
11/03/2013
12/03/2013
13/03/2013
14/03/2013
15/03/2013
18/03/2013
19/03/2013
20/03/2013
21/03/2013
22/03/2013
Vedta
tiu tn (ml)
7,0
7,0
7,0
7,0
7,1
7,1
6,85
7,0
7,0
7,0
(rag/1)
173,751
173,751
173,751
173,751
176,233
176,233
170,028
173,751
173,751
173,751
CcaCQ3
*Nhn xt: Hm lng CaCOj trong nc cp tng i n nh. Theo QCVN 01 - 2009/BYT, cng tnh theo CaC3 gii
hn l 300mg/l. Nh vy, tt c cc mu nc sinh hot ny u t QCVN 01 : 2009/BYT oi vi nc sinh hot.
2.1.2.2. Nc chy qua ct ionit
Mau
Ngy
Vedta tiu tn (ml)
CcaCQ3 (iug/l)
1
24/04/2013
25/04/2013
26/04/2013
29/04/2013
30/04/2013
1,8
8
9
01/05/2013
02/05/2013
03/05/2013
06/05/2013
1,8
1,8
1,75
10
07/05/2013
2
3
4
5
6
7
1,8
1,8
1,7
1,7
1,8
1,8
4,664
4,644
4,664
2,162
2,162
4,664
4,644
3,403
4,644
4 644
Mau
1
2
3
4
5
6
7
Ngy
VEDTA tiu tn (ml)
11/03/2013
1,7
12/03/2013
1,8
13/03/2013
1,75
14/03/2013
1,7
15/03/2013
1,75
18/03/2013
1,75
19/03/2013
1,8
8
9
20/03/2013
21/03/2013
10
22/03/2013
1,8
1,8
1,8
CcaCO (ntg/1)
2,162
4,644
3,403
2,162
3,403
3,403
4,644
4,644
4,644
4,644
*Nhn xt: Hm lng Ca CO; phn tch c ca cc mu tng i n nh v gn tng ng so vi nc qua ct ionit, nh hn
rt nhiu so vi nc cp.
2.2. Hm lng clorua
2.2.1.
Cch tin hnh
Dng pipet ht lOOml mu th vo bnh nn dung tch 250ml. Neu mu th l nc ct 1 ln th ht 200ml mu vo binh nn c dung
tch ln hn.
iu chnh mi trng pH ca mu nam trong khong 6,5-7 bng dung dch HNO3 0,1M v dung dchNaOH 0,1M. Ghi li VnNcuv
VNaQH dng.
- Thm lml dung dch ch th K2C1O4 100g/l.
Chun dung dch bng cch thm tng git AgN03 vo n khi dung dch chm chuyn mu hi nu .
- Ghi li VAgN03 tiu tn.
2.2.2.
Kt qu
2,2,2,1.
Nc cp (nu'c sinh hoat tai trng)
Mau
1
2
3
4
5
6
7
8
9
10
Ngy
25/03/2013
26/03/2013
27/03/2013
28/03/2013
29/03/2013
01/04/2013
02/04/2013
03/04/2013
04/04/2013
05/04/2013
1,9
1,8
1,8
1,8
1,9
Cciorua (mg/l)
12,763
14,181
13,472
14,181
12,763
13,472
12,763
12,763
12,763
13,472
*Nhn xt: Hm lng clorua trong nc cp ri vo khong 2-14 mg/1, n nh tng i, t yu cu i vi nc sinh hot.
2.2.2.2.
Nc ehv qua ct ionit
Mau
1
2
3
4
5
6
7
8
9
10
Ngy
24/04/2013
25/04/2013
26/04/2013
29/04/2013
30/04/2013
01/05/2013
02/05/2013
03/05/2013
06/05/2013
07/05/2013
1,15
1,2
1,2
1,2
1,15
1,15
1,2
1,2
Cciorua(mg/l)
7,091
7,799
8,154
8,509
8,509
8,509
8,154
8,154
8,509
8,509
*Nhn xt: Hm lng clorua gim khong mt na so vi nc cp, n nh ca cc mu tng i tt nhng li cao hn so
vi cc mau nc ct phn tch.
2.3.2.3NUC ct 1 ln
03/04/2013
0,55
1,950
Ngy
VAgN03 tiu tn
(ml)
Cciorua (mg/1)
9
04/04/2013
1,773
25/03/2013
2,127 0,5
0,6
10 0,5 05/04/2013
1,773
26/03/2013
1,773 0,5
2
3
27/03/2013
2,127
0,6
4
28/03/2013
0,5
1,773
"Nhn 5xt: Hm
lng
clorua
phn
tch
c
gim
nhiu
ln
so
vi nc cp, n inh ca cc mu tt v c hm lng nh
29/03/2013
0,5
1,773
han nc qua ct
ionit.
01/04/2013
2,127
6
0,6
7 2.3. Hm
02/04/2013
0,5
1,773
lng amoni
Mu
2.3.1.
Cch tin hnh
2.3.1.1. Lp ng chun
Chn b 11 bnh nh mc c cng dung tch 25ml c nh s th t T dung dch tiu chun NH,+ 10mg/l, ht chnh xc cc
th tch tng dn cho vo cc binh nh mc nh bng di:
Bnh
10
11
VNH4
10mg/l
CNH4
(mg/1)
Rock
Nessler
Nc
ct
0,5
1,0
1,5
2,0
2,5
3,0
3,5
4,0
4,5
5,0
0,2
0,4
0,6
0,8
1,0
1,2
1,4
1,6
1,8
2,0
10
11
0,285
0,330
0,368
0,401
2m
Iml
nh mc ti 25ml
0 0,038
0,076
4
0,123
5
0,164
6
0,209
- V ng chun
2.3.1.2. Xc nh NH/
Ht 20ml mu vo bnh nh mc 25ml
Thm 2ml dung dch Rock 10%
Thm lmLNessler
nh mc ti vch bng nc ct, lc u
e yn dung dch 10-15 pht ri em o mt quang k=400nm
2.3.2.
Kt qu
7
0.250
06/05/2013
07/05/2013
A2-X
A3-2
08/05/2013
09/05/2013
10/05/2013
11/05/2013
6
2.4.1,3. Nc ct 1 ln
Mu
1
2
3
4
5
6
Ngy
06/05/2013
07/05/2013
08/05/2013
09/05/2013
10/05/2013
11/05/2013
0,297
0,306 c
^amoni
0,301
(mg/1)
0,302
0,297
0,299
(nig/1)
0,839
0,827
0,827
0,797
0,858
0,839
Camoni
0,498
0,496
0,498
0,498
0,500
0,499
A3.2
A_x
0,312
0,315
0,312
0,313
0,311
0,312
0,21!
0,149
0,187
0,181
0,218
0,202
'-'amoni
0,498
0,496
0,498
0,498
0,500
0 499
(mg/l)
0,120
0,095
0,120
0,114
0,134
0,124
nh mc ti vch bng nc ct
yn dung dch 10" 15 pht
o mt quang ca cc ong tiu chun =51 Onm
Lp bng:
Bnh
0,5
0,7
1,5
1,7
VFez+
0
0,2
1,0
1,2
2,0
1 Omg/1
0,40 0,48
Cbc
0
0,08 0,20 0,28
0,60 0,68 0,80
(mg/1)
A
0,013 0,037 0,057 0,081 0,094 0,117 0,134 0,154
0
V ng chun:
0.18
2.5.1.2.
Xc nh Fe tng
Ht 25ml mu vo cc c m I OOml
Thm lml HC1 v 0,5ml NHiOH.HCl
un si cn mt na, ngui
Chuyn nh lng vo bnh nh mc 25ml
Thm 5ml m axetat
Thm Iml phenantrolin ri nh mc bng nc ct ti vch
- yn 10-15 pht roi em o quang bc sng =51 Onm
Lm tng t vi mu trng
2.5.2. Kt qu
2.5.2.1.
Nc ct 1 ln
Mu
A2-X
0,15
0,151
0,152
A3.2
0,236
0,235
0,235
CFe, mg/1
0,037
0,029
0,024
09/05/2013
0,147
10/05/2013
0,15
11/05/2013
0,151
6
2,5.2,2 Nc chy qua ct ionit
0,236
0,236
0,234
0,053
0,037
1
2
3
Ngy
06/05/2013
07/05/2013
08/05/2013
4
5
Mu
Ngy
A2-X
06/05/2013
0,146
1
07/05/2013
0,15
2
3
08/05/2013
0,151
4
09/05/2013
0,15
5
10/05/2013
0,149
11/05/2013
0,145
6
2.5.2,3. Nc cp (nc sinh hot ti trng)
Mu
1
2
3
4
5
6
Ngy
06/05/2013
07/05/2013
08/05/2013
09/05/2013
10/05/2013
11/05/2013
A3-2
0,236
0,235
0,235
0,236
0,236
0,234
A
0,03
0,029
0,035
0,031
0,03
0,03
0,026
Cie. mg/1
0,058
0,034
0,029
0,037
0,042
0,056
CFe, mg/1
0,153
0,147
0,179
0,158
0,153
0,153
Mu
Nc ct
Nc chy
qua ct
ionit
Nc
cp
0.095-
(-1 2+
Upe ,
mg/1
0.026-
0.134
0.053
0.149-
0.029-
0,218
0.058
12,763-
0.797-
0.147-
14,181
0.858
0.179
n
in
CcaCO g/l
Cciorua?
mg/1
5,0-25,0
2,162-4,644
1,773-2,127
2,162-4,644
7,091-8,509
920-
170,028-
1400
176,233
50,0100,0
CNH4
mg/1
Dc in 4
TCVN 6224-1996
TCVN 6201-1995
TCVN 3797:83
TCVN 6225-3:2011
Hng dn th nghim Ha phn tch (Trn Bnh, Nguyn Ngc Thng. Nh xut bn i Hc Quc Gia H Ni)
Ha hc phn tch cng c (Quc Gia - Tng Hp)____________________________
Gio trnh c s ha hc phn tch ( Hong Minh Chu, T Vn Mc, T Vng Nghi. Nh xut bn Khoa hc v k thut)
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Gio trnh Phn tch cng nghip (Nguyn Th Thu Phng, Phm Th Mai Hng, V Th Thn, Nguyn c Hi, Nguyn Th
Thoa. Nh xut bn Gio Dc)
Gio trnh Ha v c (Hong Nhm. Nh xut bn Gio dc)
Gio trnh Pha ch ha cht (i hc Cng Ngh ng Nai)
Gio trnh Phn tch cng c ( Trn T Hiu, T Vng Nghi, Nguyn Vn Ri, Nguyn Xun Trung. Nh xut bn Khoa hc v k
thut)
Mt s trang web trn internet.