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Cac Phuong Phap Phan Tich Nuoc Bien (XAC DINH DO MAN)
Cac Phuong Phap Phan Tich Nuoc Bien (XAC DINH DO MAN)
on B
ON B
HO HC BIN
Cc phng php
phn tch ho hc nc bin
(Gio trnh dng cho sinh vin chuyn ngnh Hi dng hc)
MC LC
M U ................................................................................................................................. 6
CHNG 1. XC NH MUI NC BIN ............................................................. 8
1.1. XC NH CLO V MUI NC BIN BNG PHNG PHP
CHUN BC NITRAT (PHNG PHP KNUDSEN).............................................. 8
1.1.1. Gii thiu chung ..................................................................................................... 8
1.1.2. Phng php Knudsen .......................................................................................... 10
1.1.3. Thit b v dng c ............................................................................................... 13
1.1.4. Cc ho cht.......................................................................................................... 15
1.1.5. Ly v bo qun mu nc ................................................................................... 17
1.1.6. Qu trnh xc nh................................................................................................. 18
1.1.7. Tnh ton kt qu .................................................................................................. 22
1.1.8. Th t cng vic ................................................................................................... 24
1.2. XC NH CLO CA VNG NC NHT VEN B..................................... 25
1.2.1. Gii thiu chung ................................................................................................... 25
1.2.2. Phng php xc nh........................................................................................... 26
1.2.3. Thit b v dng c ............................................................................................... 26
1.2.4. Ho cht ................................................................................................................ 26
1.2.5. Ly v bo qun mu nc ................................................................................... 27
1.2.6. Qu trnh xc nh................................................................................................. 28
1.2.7. Tnh ton kt qu .................................................................................................. 29
1.2.8. Th t cng vic ................................................................................................... 30
CHNG 2. XC NH CC KH HO TAN TRONG NC BIN.......................31
2.1. XC NH KH XY HO TAN BNG PHNG PHP CHUN IT
(PHNG PHP VINCLER) ............................................................................................ 31
2.1.1. Gii thiu chung ................................................................................................... 31
2.1.2. Phng php Vincler ............................................................................................ 32
2.1.3. Thit b v dng c ............................................................................................... 35
2.1.4. Ho cht ................................................................................................................ 36
2.1.5. Ly mu nc v c nh xy ho tan ................................................................. 39
2.1.6. Qu trnh xc nh................................................................................................. 39
2.1.7. Tnh ton kt qu .................................................................................................. 42
2.1.8. Th t cng vic ................................................................................................... 45
2.2. XC NH OXY HO TAN TRONG NC BIN KHI C KH SUNFUHYDRO45
2.2.1. Phng php xc nh........................................................................................... 45
2.2.2. Thit b v dng c ............................................................................................... 46
2.2.3. Ho cht ................................................................................................................ 46
2.2.4. Ly v bo qun mu nc ................................................................................... 47
2.2.5. Qu trnh xc nh v tnh ton kt qu ................................................................ 47
2.3. XC NH KH SUNFUHYDRO HO TAN TRONG NC BIN ...................... 48
2.3.1. Gii thiu chung ................................................................................................... 48
2.3.2. Phng php xc nh........................................................................................... 49
2.3.3. Thit b v dng c ............................................................................................... 51
2.3.4. Ho cht ................................................................................................................ 51
2.3.5. Ly mu nc v c nh H2S .............................................................................. 52
LI NI U
Gio trnh HO HC BIN, phn 2: Cc phng php phn tch ho
hc nc bin c bin son ging dy cho sinh vin chuyn ngnh Hi
dng hc, i hc Quc Gia H Ni. y cng l ti liu tham kho tt cho
sinh vin cc ngnh Thu vn, Thu ho v Mi trng ca cc trng i hc
khc c lin quan n lnh vc nghin cu bin, ng thi cng l ti liu tham
kho i vi cc th nghim vin ang lm cng tc phn tch ho hc nc bin
Vit Nam.
tp trung vo nhng kin thc thuc v phn tch ho hc nc bin,
gio trnh ch trng gii thiu c s nhng phng php ho hc v quy trnh
thu mu, phn tch mu nc bin xc nh cc hp phn ho tan trong n.
y khng i su v chi tit vo cc cch pha ch dung dch, cch cn, ong,
cch ty v lm sch ho cht, cch s dng cc dng c, thit b phn tch...
Nhng kin thc ny sinh vin c trang b t cc chuyn trc , t
cc t thc tp Vt l i cng, Ho hc i cng v Ho hc phn tch,
hoc tm hiu trong cc ti liu chuyn mn. Bi vy, yu cu i vi sinh vin
khi hc gio trnh ny l phi c cc kin thc c bn v Ho hc bin (phn 1),
Ho hc i cng v Ho hc phn tch. Trong qu trnh hng dn sinh vin
hc tp, gio vin c th nhc li v m rng thm nhng kin thc c lin quan.
Tc gi rt mong nhng gp b sung v hon thin gio trnh. Cc
kin xin gi v a ch B mn Hi dng hc, Trng i hc Khoa hc T
nhin, i hc Quc Gia H Ni.
Tc gi
M U
Ngy nay, cc nghin cu ho hc bin khng ch dng li vic xem xt
hin trng phn b cc yu t ho hc ti vng bin nghin cu m i su vo
c ch v bn cht ca cc qu trnh v hin tng, l ngun gc hnh thnh
cc hp phn ho hc nc bin, quy lut phn b v bin ng ca chng, mi
quan h gia cc yu t vi nhau v vi mi trng, vi sinh vt, vi qu trnh
tng tc bin-kh quyn-thch quyn-sinh quyn, vi chu trnh vt cht v chu
trnh sinh-a-ho. Cc nghin cu ho hc bin vi quy m v ni dung nh
vy gip ch rt nhiu cho cc nghin cu vt l, ng lc, sinh hc, sinh
thi, ti nguyn v ngun li sinh vt v phi sinh vt... ca vng bin, c bit
trong vic nghin cu v kim sot mi trng bin.
Thc t, Hi dng hc ngy nay v ang s dng mt s my mc,
thit b c th o trc tip t nc bin mt vi tnh cht v hp phn ho hc
nh mui, dn in, c, xy ho tan, pH... vi chnh xc cao. C
thit b nh CTD-Rosette, RCM-9, RCM-12 hoc Aquashuttle, Nvshuttle... cn
o c ng b mt s yu t theo cu trc thng ng v c th ghi s liu
vo bng t, rt tin li cho vic x l kt qu trn my tnh. Tuy nhin xc
nh nng ca phn ln cc yu t ho hc nc bin, hin ti vn phi s
dng cc phng php phn tch ho hc truyn thng nh chun mu nc,
so mu ca mu vi dung dch chun... Ch khc l nu trc y vic phn tch
ho hc nc bin c thc hin hon ton bng cc thao tc th cng th ngy
nay Hi dng hc c cc thit b ph tr (my so mu quang in, ph
quang k, sc k kh, quang ph hp th nguyn t...) gip cho vic phn tch
c nhanh chng, chnh xc v loi b c cc sai s ch quan ca ngi
phn tch. Song vi phng chung nn kinh t ca t nc hin nay, cc my
mc, thit b o v phn tch hin i nh vy thng khng ph hp vi ngun
ti chnh ca cc ti, d n v cc c s o to v nghin cu khoa hc bin.
Trong i a s cc trng hp, phng php phn tch ho hc truyn thng
vn l hu hiu i vi cc nghin cu ho hc bin nc ta v nhiu nc
trn th gii, ngay c khi c cc thit b o hin i i km.
Chng 1
XC NH MUI NC BIN
1.1. XC NH CLO V MUI NC BIN BNG PHNG PHP
CHUN BC NITRAT (PHNG PHP KNUDSEN)
10
11
(1.1)
3
(1.2)
(1.I)
12
(1.II)
13
thit b ny vi vic thit lp vch "0" nh van 2 ng. Khi dung dch c bm
vo Biuret (hoc ht vo Pipet) cc l van c ng m bng tay mt cch hp
l sao cho dung dch chim ton b th tch Biuret (hoc Pipet) ti vch s
"0".
Ngy nay cc Biuret v Pipet bin c cu trc n gin m vn t c
chnh xc cao. Vch s "0" c thit lp t ng nh mt ng mao dn hnh
"m hc" nm phn trn cng ca thit b. S "0" ca thang chia ng vi
u mt ca m hc, l thot ca m hc c ng knh khong 1mm. Pipet
bin s dng ring cho mc ch phn tch Clo c dung tch chnh xc bng
15 ml. Mun ly y dung dch vo Biuret (hoc Pipet), ch cn bm (hoc ht)
dung dch vo thit b cho ti khi c mt t trn qua m hc (d nhin lng trn
qua ny phi c thu gom vo mt bnh cha no ). Nh vy vch s "0"
c thit lp m khng cn c thao tc g thm.
Nt c bit th 2 ca Biuret bin dng xc nh Clo l mi chia
nguyn ca n c th tch ng bng 2 ml v c vch du thnh 20 phn u
nhau. Nh vy th tch mi phn l 0,1ml v khong cch gia hai vch lin
nhau l 0,05 chia. iu ny cho php c bng mt thng v tr mt khum
ca dung dch trong Biuret chnh xc ti 0,01 chia.
Biuret v Pipet bin nht thit phi c bng kim nh km theo. Vic s
dng chng bt buc phi tun th mt cch nghim ngt cc quy trnh, ng tc
v cc iu kin lm vic (s nu phn sau).
Ngoi Biuret v Pipet t ng, cn c thm cc dng c sau:
- Cc chun th tch khong 300 ml, s dng loi cc t bnh thng.
- My khuy c hoc my khuy t. Trng hp khng c my khuy c
th dng a khuy thu tinh nhng u a phi bc cao su trnh va p vo
thnh cc chun lc lm vic.
- ng nh git (dng cho dung dch cht ch th).
- Cc bnh v chai l xm mu cha dung dch Bc Nitrat (th tch t 3
14
15
16
thit, lc u xo trn dung dch. Nc ct pha dung dch phi tht tinh
khit v khng c ln Clo. Dung dch pha ch xong phi hon ton trong sut,
nu khng trong sut phi t vo ch ti cho n khi hon ton trong sut mi
c s dng. Tu theo s lng mu cn phn tch, c th chun b sn t 3
n 5 lt v bt ng trong bng ti vi ba ngy.
Ch rng dung dch Bc Nitrat rt d bin i nng khi tip xc vi
nh sng nn ngoi vic dng cc bnh thu tinh mu cha chng, mi bin
php cch ly dung dch vi nh sng (bc vi en dy, ni ti) l rt cn thit.
Dung dch cht ch th Kali Crommat 10% (K2CrO4)
Vi mc ch l ch th mu cho thi im tng ng, nng dung dch
K2CrO4 khng cn thit phi c chnh xc cao. Tuy vy, ch phm pha ch
dung dch phi tinh khit, khng c ln tp cht c th tc dng c vi Bc
Nitrat hoc lm i mu hn hp lc chun .
Dng cn k thut ly 10 gam mui K2CrO4 sch v ho vi 90 ml nc
ct, ta c dung dch Kali Crommat 10%.
Ngoi 3 ho cht trn, cn c hn hp ra Crm + axt Sunfuric long (gi
l nc Crm) ra dng c, m bi trn cc van ca Biuret, Pipet v mt
vi ho cht ty ra thng thng khc.
1.1.5. Ly v bo qun mu nc
Khi thit b ly nc bin c ko ln boong tu, cc kho st vin bt
u thc hin cng vic ly mu. Vi mc ch ly mu xc nh Clo, c th
s dng chai l bt k (bng thu tinh hoc nha), nhng phi sch v c nt kn
trnh bay hi nc. Mu xc nh Clo c ly sau cc mu xc nh
pH v Oxy ho tan.
Cc chai l s dng ln u cn c ra cn thn bng nc Crm v
nc ngt, sau ngm bng nc bin t 1 n 1,5 thng v ch nc ang
ngm chai l i trc lc s dng. Trc khi ly mu nc vo l cn phi trng
l 2-3 ln bng chnh nc cn ly. Khng nn ly nc y l trnh bt nt
17
18
19
(1.3)
(1.4)
20
21
=-0,145
=-0,140
=-0,135
=-0,130
a=
a=
a=
a=
a=
22.90
23.03
23.17
22.65
22.78
22.92
23.06
23.20
-0.27
...
...
...
...
...
-0.26
19.38
19.52
19.67
19.82
19.97
-0.15
19.06
19.21
19.36
19.51
19.66
-0.14
18.74
18.89
19.04
19.19
19.35
-0.13
18.42
18.57
18.72
18.87
19.03
-0.12
18.08
18.23
18.39
18.54
18.70
-0.11
...
...
...
...
...
-0.10
13.38
13.57
13.76
13.95
14.14
12.78
12.98
13.18
13.38
13.58
k=
23.14
-0.28
22
+0.01
(1.5)
S %o
17,5
Cl %o
S %o
17,5
18.00
32.52
26.13
24.84
18.50
33.42
26.86
25.53
.01
.54
.14
.85
.51
.44
.87
.54
.02
.56
.16
.86
.52
.46
.88
.55
...
...
...
...
...
...
...
...
18.10
32.70
26.27
24.97
18.60
33.60
27.00
25.66
.11
.72
.29
.99
.61
.62
.02
.68
.12
.74
.30
25.00
.62
.64
.03
.69
...
...
...
...
...
...
...
...
18.20
32.88
26.42
25.11
18.70
33.78
27.15
25.80
.21
.90
.43
.13
.71
.80
.16
.82
.22
.92
.45
.14
.72
.82
.18
.83
.23
.94
.46
.15
.73
.84
.19
.84
...
...
...
...
...
...
...
...
18.30
33.06
26.56
25.25
18.80
33.96
27.29
25.94
.31
.08
.58
.26
.81
.98
.31
.96
.32
.10
.59
.28
.82
34.00
.32
.97
23
V d:
- clo ca nc bin tiu chun l N = 19,380
- S c trn Biuret khi chun nc bin tiu chun ln th nht l
A1=19,52, hiu chnh s c ng vi 19,52 l 0,00; ln th hai l A2=19,53, hiu
chnh s c ny l -0,01. S c trung bnh ( c hiu chnh) sau 2 ln
chun nc bin tiu chun l A=(19,52+0,00+19,53-0,01):2=19,52.
- Gi tr = N-A = 19,38-19,52 =-0,14 chng t dung dch Bc Nitrat ny
t yu cu chun mu nc.
- S c trn Biuret khi chun mu nc l 18,82, hiu chnh s c ca
Biuret ng vi 18,82 l +0,03. S c thc l a = 18,82 + 0,03 = 18,85.
- S k tm c t bng bng 1.1 theo v a l k=-0,12.
- Clo ca nc bin l Cl=a+k = 18,85-0,12=18,73%o.
- Tra bng 1.2 ta c S=33,84%o, o = 27,19 v 17,5 = 25,84.
y mt ln na nhc li rng cng thc Knudsen v cc bng tnh sn
ch p dng c vi nc i dng v cc bin h. Nhng bin kn, vng,
vnh...v cc khu vc lu thng km vi i dng hoc nhng vng nc chu
nh hng mnh ca dng lc a th phi s dng cc cng thc hoc cc bng
ring.
1.1.8. Th t cng vic
Bc 1: Kim tra s sch s ca dng c, trong trng hp cn thit phi
ra li.
Bc 2: Np dung dch AgNO3 vo y Biuret sau khi trng n bng
chnh dung dch ny. Tip kim tra chun ca dung dch Bc Nitrat theo
nc bin tiu chun, nu cha t yu cu phi hiu chnh li (xem mc 1.1.6.
chng ny).
Bc 3: Np dung dch AgNO3 t yu cu vo y Biuret.
24
25
26
27
ca phng.
1.2.6. Qu trnh xc nh
Th nghim nh tnh
Trc ht phi lm php th nh tnh xem cn phi s dng dung dch
Bc Nitrat loi no. Mun vy, ly 5 ml mu nc cn phn tch cho vo bnh
tam gic, cho tip 2 git ch th mu v sau chun mu bng dung dch
Bc Nitrat loi 1. n thi im tng ng (l thi im mu da cam n nh
sau 20-25 giy - xem mc 1.1), nu th tch dung dch Bc Nitrat dng (k
hiu l V) ln hn 2 ml, iu c ngha l hm lng cc halogen trong mu
(k hiu Cl) ln hn 1000 mgCl/l - ta c th p dng phng php Knudsen nh
i vi nc bin. Nu 1ml < V 2ml, ngha l 500 mgCl/l < Cl 1000 mgCl/l
ta cn dng dung dch Bc Nitrat loi 1 phn tch mu nc, nu V 1 ml ta
cn dng dung dch Bc Nitrat loi 2.
Kim tra nng dung dch Bc Nitrat
V dung dch Bc Nitrat rt hay bin i di tc dng ca nh sng v
nhit nn kim tra nng ca n l vic lm rt cn thit v thng xuyn.
Dung dch Bc Nitrat loi no th dng chun loi kim tra.
Ly 25 ml (hoc 20 ml) dung dch chun cho vo bnh tam gic ri b sung
nc ct n 100 ml (c th dng bnh chia thay cho bnh tam gic). Sau
cho thm 1 ml ch th mu v chun hn hp bng dung dch Bc Nitrat
tng ng vi chun ly. Ch l tt c cc Biuret, Pipet trc khi s dng
phi tht sch v phi trng n bng chnh dung dch cn ly. Trong khi chun
phi khuy lin tc. Vic chun s kt thc ti thi im tng ng.
Ghi li s c trn Biuret v lm li th nghim ly s c ln th hai. Gi tr
s c trung bnh ca hai ln chun s c s dng tnh ton kt qu.
Nng tht ca dung dch Bc Nitrat tnh tng ng theo lng Clo,
k hiu l TAgNO3 (mgCl-/ml), c xc nh theo cng thc sau:
TAgNO3 (mgCl-/ml) = (V +v).[Cl-]/(n + n)
28
(1.6)
(1.7)
29
30
Chng 2
XC NH CC KH HO TAN TRONG NC BIN
2.1. XC NH KH XY HO TAN BNG PHNG PHP CHUN IT
(PHNG PHP VINCLER)
mui (%o)
(oC)
10
20
30
35
10.29
9.97
9.65
9.00
8.36
8.04
9.03
8.75
8.49
7.94
7.40
7.13
10
8.02
7.79
7.56
7.09
6.63
6.41
15
7.22
7.02
6.82
6.43
6.03
5.83
20
6.57
6.40
6.22
5.88
5.52
5.35
30
5.57
5.42
5.27
4.95
4.65
4.50
mui Mangan2 (nh MnCl2 hoc MnSO4) v sau l dung dch Natri kim
(NaOH), hoc Kali kim (KOH), th lp tc chng s phn ng vi nhau ngay
trong lng mu nc to ra kt ta Mangan2 hydroxuyt mu trng Mn(OH)2.
V d:
MnCl2 + 2NaOH = Mn(OH)2 + 2NaCl
(2.I)
(2.II)
(2.III)
33
(2.IV)
34
No12
146,5
l
Hnh 2.1. L xy
35
36
37
38
39
ht, trng Biuret bng chnh dung dch Thyosunfit chun b, sau np dung
dch vo y Biuret. Cn phi thy r vch s "0" ca Biuret c thit lp v
trong thnh Biuret khng c bt kh bm vo, nu khng t c hai yu cu
ny th phi lm li.
Tip theo, ly 10 ml dung dch KI 10% v 50 ml nc ct cho vo bnh nn
(c th ho tan trc tip 10 gam KI sch vi 50 ml nc ct ngay trong bnh
ny). Sau dng Pipet t ng ly tht chnh xc 15 ml dung dch K2Cr2O7
0,02N (hoc dung dch KH(IO3)2 0,02N) v 10 ml dung dch H2SO4 1:4 (hoc
dung dch HCl 2:1) cho vo bnh nn k trn. o lc cn thn hn hp trong
bnh, khi It c gii phng theo phn ng sau:
K2Cr2O7 + 6 KI + 14HCl = 8 KCl + 2 CrCl3 + 7 H2O + 3 I2
phn ng ny Cr+6 b kh thnh Cr+3 bi axit Iotuahydro (HI) c to ra
trong qu trnh trung gian, cn anion It b xy ho thnh It phn t. Hin
nhin ta bit trc c lng It t do to ra trong phn ng trn v bit
c th tch (15 ml) v chun (0,02 N) ca dung dch K2Cr2O7.
Chun hn hp trong bnh nn bng dung dch Thyosunfit t Biuret
trong khi khng ngng o lc bnh. Khi cht lng c mu vng ti th b sung
thm vo 1 ml dung dch tinh bt v 50 ml nc ct. Lc cht lng s c
mu xanh lam do It b nhum mu. Tip tc chun hn hp tht cn thn
cho n mu xanh l cy nht (l mu ca Cr+3). Ti thi im ny - thi im
tng ng, trong bnh nn khng cn It t do na. Khi ghi s c trn
Biuret chnh xc ti 0,01 ml vo s chuyn mn.
Ton b qu trnh trn c lm li 2-3 ln vi iu kin lm vic hon
ton tng t. Nu s c ca mi ln khc nhau khng qu 0,05 ml th s c
trung bnh c s dng tnh ton kt qu. Nu s sai khc vt qu 0,05 ml
th cc dung dch chun b cha tt, cc ho cht khng c tinh khit. Cn
phi khc phc bng vic pha ch li cc dung dch.
Nu dng dung dch 0,02N Kaliiotua oxuyt (KIO3) xc nh h s hiu
chnh cho dung dch Thyosunfit, th cng vic cng hon ton tng t nh
40
N = 0,02 KNa
(2.1)
(2.2)
41
(2.3)
42
(2.4)
(2.5)
43
44
45
(2.V)
(2.VI)
46
47
48
Vi khun
49
(2.VII)
(2.VIII)
50
51
52
53
Thyosunfit
Cc bc tin hnh nh sau:
Bc 1: Np kh CO2 vo y bnh nh mc (dung tch ca bnh khong
200-250 ml v c xc nh chnh xc t trc). C hai cch np kh CO2
vo bnh nh mc nh nu mc 2.3.5.
Bc 2: Cho thm vo bnh nh mc k trn 10 ml dung dch 0,02N It
trong KI. Nu trc bnh c np kh CO2 t bnh thp th tip tc cho thm
vo bnh 1 ml dung dch HCl 1:1. Nu phi to kh CO2 t NaHCO3 v HCl th
khng cn thm dung dch HCl na (v trong bnh c sn).
Bc 3: Sau khi trong bnh nh mc c 3 loi ho cht trn (gm
CO2, hn hp dung dch 0,02N It trong KI v dung dch HCl 1:1) th b sung
nc bin khng c H2S (nc tng mt c lc k) vo bnh cho n vch
mc. ng nt bnh tht cht v lc u.
Bc 4: dung dch trong bnh nh mc vo bnh tam gic ri chun
n bng dung dch Thyosunfit hiu chnh chun. Khi cng vic gn kt
thc ( l lc mu vng It ca hn hp cn r nt), ta b sung vo hn hp
ang b chun mt t dung dch tinh bt th hn hp s chuyn thnh mu
xanh. Tip tc chun cn thn cho n khi hn hp khng mu.
Bc 5: Rt mt t dung dch khng mu ngc tr li bnh nh mc
trng bnh, ri li chuyn phn nc trng bnh sang bnh tam gic. Lc ny hn
hp li c mu xanh nhng cng rt yu (nu khng c mu xanh th vic
chun bc 4 trc c th b qu). Tip tc chun tht thn trng
hn hp cho n khi mt mu hon ton, ghi li s c trn Biuret chnh xc ti
0,01 ml.
Bc 6: Lp li ton b 5 bc k trn ln th hai. Nu s c trn Biurt
ca hai ln chun khng chnh nhau qu 0,05-0,1 ml th s c trung bnh
c s dng tnh ton kt qu. Nu s sai khc vt gii hn ny th phi
lm li th nghim ln th 3 ly hai ga tr gn nhau nht.
54
Xc nh H2S trong mu nc
Mu nc sau khi c nh H2S cn phi c phn tch ngay, cng sm
cng tt. Nu lu, lng It cn li trong mu s bay hi v kt qu phn tch
trong trng hp ny s khng chnh xc.
mu nc c nh H2S qua bnh tam gic ri chun n bng chnh
dung dch Thyosunfit s dng trong php xc nh tng quan. Qu trnh
chun mu nc tng t nh bc 4 v bc 5 m t trn. Ghi li kt
qu chun .
2.3.7. Tnh ton kt qu
Theo quy c, nng H2S (thc cht l tng nng ca c h
Sunfuhydro, k hiu S) c biu din tng ng qua s mililit kh H2S (xt
iu kin chun) c trong 1 lt nc bin. T cc phng trnh phn ng gia
It vi H2S (2.VII) v gia It vi Thyosunfit (2.VIII), rt ra rng 1 ng
lng gam It, v do 1 ng lng gam Na2S2O3 tng ng vi 1/2 phn t
gam H2S. Trng lng phn t ca H2S l 34,08 nn 1/2 phn t gam H2S s l
17,04. 1ml kh H2S ti iu kin chun nng 1,5393 mg. T suy ra cng thc
sau:
S ( mlH 2 S / l ) =
17 , 04 .( m n ). N .K . 1000
( V d ). 1, 5393
(2.6)
S(mlH 2S / l) =
221.(m n )..K
(V d)
55
(2.7)
(2.8)
V d:
- xc nh chun thc ca dung dch Thyosunfit, ta dng Pipet dung
tch 10ml c s hiu chnh +0,03 v ly c 10,03 ml dch chun K2Cr2O7
0,02N. S c trung bnh trn Biuret sau 2 ln chun Thyosunfit vo cng
lng dung dch chun ny l 10,18, hiu chnh s c ny l 0,00. Vy h s
hiu chnh chun dung dch Thyosunfit l K=10,03/10,18 = 0,985.
- Dng chnh Pipet k trn ta ly c 10,03 ml dung dch chun 0,02N It
trong KI v dng Pipt khc ly 2 ml dung dch HCl 1:1 cho vo bnh nh mc
c dung tch V=250 ml, b sung nc bin khng c H2S n vch mc ca
bnh. Khi chun hn hp trn bng dung dch Na2S2O3 kim tra chun,
ta tm c s c trn Biuret l: ln th nht m1=9,98, ln th hai m2=9,96,
trung bnh cho 2 ln c l 9,97, hiu chnh s c ny l +0,01 nn s c thc
l m=9,98.
- Khi xc nh lng H2S trong mu nc bin tng ng vi lng It cn
li, ta ly 250 ml mu nc chun bng dung dch Thyosunfit (mu nc
c sn 2ml dung dch HCl 1:1 to kh CO2). S c trn Biuret trong
trng hp ny l n=6,86. T (2.7) ta c:
S ( mlH 2 S / l ) =
56
cc vic sau:
- Np kh CO2 vo y bnh nh mc. Ly 10 ml dung dch chun 0,02N
It trong KI v 1 ml dung dch HCl 1:1 cho vo bnh nh mc k trn. C th
thay cng vic ny bng cch cho vo bnh nh mc sch 2 ml HCl 1:1 v cho
tip vo mt lng 0,2 g NaHCO3, sau cho vo 10 ml hn hp dung dch
It trong KI.
- B sung nc bin khng c H2S n vch mc ca bnh.
- Chuyn dung dch t bnh nh mc sang bnh tam gic v chun n
bng dung dch Thyosunfit kim tra chun.
Bc 4: Ly mu nc v c nh H2S, gm cc vic sau:
- Chun b lot bnh nh mc ly mu. S lng bnh tng ng vi s
tng cn ly mu.
- Np kh CO2 vo cc bnh bng mt trong hai cch nu.
- Ly mt lng nht nh (thng l 10 ml) dung dch 0,02N It trong KI
v nu bnh c np kh CO2 t bnh thp th ly thm 1 ml dung dch HCl 1:1
cho vo cc bnh mu chun b. y nt v bo qun chng ni mt.
- Khi my ly nc c a ln boong tu kho st th tin hnh ly nc
mu vo bnh cho n vch mc v chuyn ngay n ni phn tch.
Bc 5: Chun mu nc bng dung dch Thyosunfit kim tra
chun v xc nh tng quan vi It. Ghi kt qu chun vo s chuyn
mn.
Bc 6: Lp li bc 5 cho mu khc.
Bc 7 Vic tnh ton kt qu c th thc hin sau khi phn tch xong lot
mu hoc cui ngy lm vic. Kt qu tnh ton phi c ngi th hai kim
tra li.
57
Chng 3
XC NH CC THNH PHN
CA H CCBNT TRONG NC BIN
3.1. XC NH PH NC BIN BNG PHNG PHP SO MU
hay
K[H2O] = [H+].[OH-]
58
59
60
61
Th tch cn ly (ml)
pH
Th tch cn ly (ml)
mong mun
H3BO3
Na2B4O7
mong mun
H3BO3
Na2B4O7
7.60
8.50
1.50
8.10
6.92
3.08
62
pH
Th tch cn ly (ml)
pH
Th tch cn ly (ml)
mong mun
H3BO3
Na2B4O7
mong mun
H3BO3
Na2B4O7
7.65
8.38
1.62
8.05
6.72
3.28
7.70
8.24
1.76
8.20
6.50
3.50
7.75
8.10
1.90
8.25
6.28
3.72
7.80
7.95
2.05
8.30
6.06
3.94
7.85
7.80
2.20
8.35
5.82
4.18
7.90
7.64
2.36
8.40
5.57
4.43
7.95
7.47
2.53
8.45
5.32
4.68
8.00
7.30
2.70
8.50
5.06
4.94
8.05
7.12
2.88
8.55
4.79
5.21
63
Hnh 3.1
Comparat dng so mu xc
nh pH nc bin
3.1.4. Ly mu nc v xc nh pH
Vi mc ch xc nh pH, mu nc cn c u tin ly trc cc mu
khc v ly ngay sau khi ko my ly nc t di bin ln. S u tin ny
nhm hn ch kh nng thm nhp CO2 t kh quyn vo mu.
Trc ht cn chun b sn b ng nghim sch, kh ly mu, s lng
ng nghim tng ng s mu cn ly (cc ng nghim ly mu phi hon ton
tng t cc ng nghim ca bng mu). Lp ng dn nc vo my ly nc
v m van trng ng dn v cc ng nghim. Sau khi trng ng nghim 23 ln bng chnh nc mu cn ly, dng Pipet ly mt lng ch th mu theo
ch dn ghi trong h s hp bng mu (thng l 0,5 ml) cho vo ng nghim
64
65
Nc ct
Nc bin c mu t nhin
v khng c cht ch th
Chun 2
Chun 1
Mu phn
tch
66
pHs
S%o
pHs
S%o
pHs
S%o
pHs
0,2
+0,20
-0,09
19
-0,20
30
-0,24
0,4
+0,18
-0,11
20
-0,20
31
-0,25
67
S%o
pHs
S%o
pHs
S%o
pHs
S%o
pHs
0,6
+0,16
10
-0,12
21
-0,21
32
-0,25
0,8
+0,14
11
-0,13
22
-0,21
33
-0,26
+0,12
12
-0,14
23
-0,22
34
-0,26
+0,06
13
-0,15
24
-0,22
35
-0,26
+0,02
14
-0,16
25
-0,23
36
-0,26
-0,01
15
-0,17
26
-0,23
37
-0,26
-0,04
16
-0,18
27
-0,23
38
-0,26
-0,06
17
-0,19
28
-0,24
-0,08
18
-0,19
29
-0,24
68
Bng 3.3: S hiu chnh pHT theo nhit bng mu (Tb) ti thi im phn tch (so vi lc
ch to ti 18oC)
Tb
pHQT
(oC)
7,7
7,8
7,9
8,0
8,1
8,2
8,3
8,4
8,5
8,6
16
0,01
0,01
0,01
0,01
0,01
0,01
0,01
0,01
0,01
0,02
18
0,00
0,00
0,00
0,00
0,00
0,00
0,00
0,00
0,00
0,00
20
-0,01
-0,01
-0,01
-0,01
-0,01
-0,01
-0,01
-0,01
-0,01
-0,02
22
-0,01
-0,01
-0,02
-0,02
-0,02
-0,02
-0,02
-0,02
-0,03
-0,03
24
-0,02
-0,02
-0,03
-0,03
-0,03
-0,03
-0,03
-0,04
-0,04
-0,04
26
-0,03
-0,03
-0,03
-0,04
-0,04
-0,04
-0,05
-0,05
-0,05
-0,05
28
-0,03
-0,04
-0,04
-0,04
-0,05
-0,05
-0,06
-0,06
-0,06
-0,06
30
-0,04
-0,05
-0,05
-0,05
-0,06
-0,06
-0,07
-0,07
-0,07
-0,08
Crezol-
Thymol-xanh
tb - tw' (oC)
Crezol-
Thymol-xanh
0,01
0,01
11
0,10
0,09
0,02
0,02
12
0,11
0,10
0,03
0,02
13
0,12
0,10
0,04
0,03
14
0,13
0,11
0,04
0,04
15
0,14
0,12
0,05
0,05
16
0,14
0,13
0,06
0,06
17
0,15
0,14
0,07
0,06
18
0,16
0,14
0,08
0,07
19
0,17
0,15
10
0,09
0,08
20
0,18
0,16
69
Tw' - Tw
(oC)
7,6
7,7
7,8
7,9
8,0
8,1
8,2
8,3
8,4
0,01
0,01
0,01
0,01
0,01
0,01
0,01
0,01
0,01
0,02
0,02
0,02
0,02
0,02
0,02
0,02
0,02
0,02
0,03
0,03
0,03
0,03
0,03
0,03
0,03
0,03
0,03
0,03
0,04
0,04
0,04
0,04
0,04
0,04
0,04
0,05
0,04
0,04
0,05
0,05
0,05
0,05
0,05
0,06
0,06
0,05
0,05
0,06
0,06
0,06
0,06
0,06
0,07
0,07
0,06
0,06
0,07
0,07
0,07
0,07
0,07
0,08
0,08
0,07
0,07
0,07
0,08
0,08
0,08
0,08
0,09
0,09
0,08
0,08
0,08
0,09
0,09
0,09
0,10
0,10
0,10
10
0,09
0,09
0,09
0,10
0,10
0,10
0,11
0,11
0,11
11
0,09
0,10
0,10
0,11
0,11
0,11
0,12
0,12
0,12
(3.1)
70
(3.2)
7.6
7.7
7.8
7.9
8.0
8.1
8.2
8.3
8.4
8.5
8.6
(10-4)
86
90
93
96
100
103
106
110
113
116
120
71
72
nh sau:
Alk = [HCO3-] + 2[CO3-2] + [H2BO3-] + [HSiO3-] +
[H2PO4-] + 2[HPO4-2] + [HS-] + ([OH-]-[H+])
y cn phn bit r khi nim kim vi tnh cht mi trng kim
(yu) ca nc bin. Mi trng mang tnh cht kim, trung tnh hay axit c
quyt nh bi nng ion Hydro (pH), cn kim l tng nng cc anion
ca cc axit yu c mt trong nc bin.
Trong s cc thnh phn to nn kim chung ca nc bin nh trn, c
ngha nht chnh l cc anion HCO3- v CO3-2 ca axit Cacbonic (H2CO3) v
anion H2BO3- ca axit Boric (H3BO3) bi chng c hm lng ln nht. Cc
anion khc c hm lng khng ng k nn thng b b qua, ch c tnh
n trong mt s trng hp cn thit. Do kim chung ca nc bin
c coi gn ng l tng ca kim Ccbonat v kim Borac:
Alk = AlkC + AlkB
Trong :
73
(3.I)
74
75
(3.3)
76
Thuc ch th mu hn hp
Ly 32 mg Metyl , kh trn vi 1,18 ml NaOH 0,1N trong chn m no
hoc chn s. Sau khi nghin k hn hp thnh mt th thng nht th ra chn
bng 80 ml ru Etylic 96%, sau cho thm vo hn hp thu c 4,8ml cn
c cha 0,1% Metylen xanh. Cn c cha 0,1% Metylen xanh c chun b
bng cch ho 0,1g Metylen xanh kh vi 100 ml ru Etylic 96%.
Thuc ch th mu hn hp phi trung tnh, tc l phi c mu gia xanh l
cy nht v nu. Nu thuc c mu xanh l cy nht, ngha l n qu kim, ta
phi nh dung dch HCl 0,1N vo cho n mu qui nh, nu c mu nu qu axit, ta phi cho thm dung dch NaOH 0,1N vo n.
Thuc ch th mu hn hp rt hay b mt phm cht nn khng c chun
b qu nhiu. Khi thy c s sai lch (i mu, vn c) th phi chun b thuc
mi. Thuc c bo qun trong bnh xm mu.
Vi ti xt
Ho cht ny dng loi kh Cacbonic ra khi lung khng kh thi vo
cht lng trong qu trnh chun . Vi ti xt phi kh v cn c ry k, lc
bi tr thnh dng bt, ht nh v mn. Ho cht c bo qun trong bnh c
nt bc, mt ngoi nt c hn kn bng Parafin hi nc trong khng kh
khng lm hng n.
kim tra cht lng vi ti xt, ngi ta cho n vo mt ng thu tinh,
nhng mt u ng vo nc Bari v thi khng kh qua trong vng 5-10
pht. Nu nc Bari khng i mu th ch phm tt. Nc Bari c chun b
t 4 gam Ba(OH)2 ho vi 100 ml nc ct khng c CO2 (l nc ct mi c
un si trong vng na gi). Nc Bari thu c phi trong sut, nu c phi
lng ng v gn ly phn trong.
3.2.5. Ly v bo qun mu nc
Mu nc bin xc nh kim thng c ly sau cc mu xc nh
pH v xy ho tan. Bnh ng mu bng thu tinh mu xanh hay da cam (v
77
(3.4)
79
Alk (meg / l ) =
(3.5)
(3.6)
2,2.10 5.Cl %o
Alk B =
1 + a(H + ) / K B*
(3.7)
T=5oC
10 oC
15 oC
20 oC
25 oC
30 oC
16
0.112
0.129
0.144
0.158
0.174
0.191
17
0.117
0.132
0.148
0.166
0.182
0.200
80
Clo %o
T=5oC
10 oC
15 oC
20 oC
25 oC
30 oC
18
0.123
0.138
0.155
0.174
0.191
0.204
19
0.126
0.141
0.158
0.178
0.195
0.214
20
0.132
0.148
0.166
0.182
0.204
0.224
21
0.135
0.151
0.170
0.191
0.209
0.229
25
0.158
0.178
0.200
0.219
0.240
0.257
81
82
Quang
hp
hp
+ HCO3-
OH +
H+
+ CO3-2
Sinh vt
+
CaCO3 (ho tan) Ca+2 (hoc Mg+2...)
y bin
CaCO3 (rn)
Hnh 3.4: S h cacbonat trong bin
83
(3.8)
[H+].[CO3-2]/[HCO3-] = K2 = 4,2.10-11
(3.9)
84
(3.10)
+
2
a ( H + ).a (CO 3 2 ) a ( H ) f CO3 CO 3
=
= K2
a ( HCO 3 )
f HCO3 HCO 3
(3.11)
(3.12)
(3.13)
pK1*= -0,48.10-4H
pK2*= -0,18.10-4H
85
(3.14)
(3.15)
(3.16)
(3.17)
Bng 3.8: Gi tr hng s nng K1* v K2* ca axit Cacbonic trong nc bin (trch t
bng Hi dng)
Nhit (oC)
Cl
%o
10
12
14
16
18
20
22
24
26
28
30
K1* (10-8)
15
0.74
0.77
0.80
0.83
0.86
0.89
0.92
0.95
0.97
0.99
1.01
16
0.75
0.78
0.81
0.84
0.87
0.91
0.93
0.96
0.99
1.01
1.03
17
0.76
0.79
0.82
0.86
0.89
0.92
0.95
0.98
1.00
1.02
1.05
18
0.77
0.81
0.84
0.87
0.90
0.93
0.97
0.99
1.02
1.04
1.06
19
0.79
0.82
0.85
0.88
0.92
0.95
0.98
1.03
1.05
1.06
1.08
20
0.80
0.83
0.87
0.90
0.93
0.97
1.00
1.04
1.06
1.07
1.10
K2* (10-9)
86
Nhit (oC)
Cl
%o
10
12
14
16
18
20
22
24
26
28
30
15
0.60
0.63
0.66
0.69
0.73
0.76
0.79
0.83
0.86
0.90
0.93
16
0.63
0.67
0.71
0.74
0.78
0.81
0.85
0.88
0.92
0.96
0.99
17
0.67
0.71
0.74
0.78
0.83
0.86
0.90
0.93
0.97
1.01
1.05
18
0.71
0.75
0.79
0.83
0.87
0.91
0.95
0.99
1.03
1.07
1.11
19
0.75
0.79
0.83
0.88
0.92
0.96
1.01
1.05
1.10
1.14
1.18
20
0.80
0.84
0.89
0.93
0.98
1.02
1.07
1.12
1.16
1.21
1.26
(3.18)
(3.19)
kim
%o
Alk
AlkC
35
20
2.38
2.28
pH
8.20
[H2CO3 + CO2]
[HCO3-]
[CO3-2]
mg/l
mM/l
mg/l
mM/l
mg/l
mM/l
0.228
0.0102
1.740
1.740
0.540
0.270
87
S
%o
T
o
kim
Alk
AlkC
35
2.38
2.28
30
20
2.05
1.97
pH
[H2CO3 + CO2]
[HCO3-]
[CO3-2]
mg/l
mM/l
mg/l
mM/l
mg/l
mM/l
8.15
0.423
0.0190
1.970
1.970
0.306
0.153
8.17
0.233
0.0104
1.585
1.585
0.380
0.190
T bng 3.9 thy rng trong mi trng hp, hp phn HCO3- lun lun
chim u th v hp phn (H2CO3+CO2) c nng b nht. Tuy nng
(H2CO3+CO2) nh b nhng n li l nhn t c bn nh hng n trng thi
cn bng ca h cacbonat trong bin. iu ny c th hin r trn s h
cacbonat hnh 3.4.
88
Chng 4
XC NH CC HP PHN DINH DNG V C V CC
CHT HU C TRONG NC BIN
4.1. NGHA V NGUYN TC CHUNG PHNG PHP SO MU XC
NH CC HP PHN DINH DNG V C TRONG NC BIN
4.1.1. ngha
Theo cch gi, cc cht dinh dng v c trong bin bao gm rt nhiu
nguyn t cn thit i vi i sng sinh vt, nh H, C, O, P, N, Si, S, Mg, Ca,
K... Tuy nhin trong mi trng hp, 3 nguyn t P, N, Si bao gi cng l
khng th thiu c i vi s sng.
Cc hp cht v c ca Phtpho, Nit, Silic tn ti trong nc bin vi
nng rt nh v rt hay bin i theo c khng gian v thi gian. S bin i
ca chng ph thuc cht ch vo qu trnh quang hp, bi trong qu trnh ny
thc vt phi s dng cc cht dinh dng v c tng hp nn cht hu c
u tin trong bin.
Phtpho dinh dng v c tn ti trong nc bin di dng axit
Phtphoric (H3PO4) cng cc dn xut phn ly ca n (H2PO4-, HPO4-2, PO4-3),
gi chung l cc Phtphat. Trong nc bin, axit Photphoric c th kt hp vi
mt vi phn t nc to nn nhng phn t phc tp hn, ch yu l dng
H3PO4.2H2O. Nng tng cng cc Phtphat trong nc bin c th bin i
t 0-100 mgP/m3.
Nit dinh dng v c trong nc bin tn ti cc dng lin kt khong.
l Amni (NH4+), Nitrit (NO2-) v Nitrat (NO3-). Trong 3 dng lin kt
khong ny th Amni l dng u tin v Nitrat l dng cui cng ca qu trnh
89
90
(4.1)
91
92
Mu xanh Molipden
Heteropolyaxit
(mu vng)
+ Thic Clorua
+ Mui Mor
(xc nh Phtphat)
Mu xanh Molipden
(xc nh Silicat)
93
100
90
80
70
60
50
40
30
20
Gng phng
Hnh 4.2: Cp ng tr Hener
94
4.2.3. Ho cht
Hn hp dung dch Amoni Molipdat trong axit Sunfuric
Ho trn mt th tch dung dch 10% Amoni Molipdat (a) vi ba th tch
dung dch 50% axit Sunfuric (b). Cc dung dch (a) v (b) chun b nh sau:
Dung dch a: Ly 25 gam Amoni Molipdat tinh th ho vi nc ct
thnh 250 ml. Nu dung dch thu c b c th phi un nng cn thn n.
Trong trng hp cn thit phi lc qua phu thu tinh sch, c ra bng
axit Sunfuric long v nc ct.
Dung dch b: Pha long cn thn 1 th tch H2SO4 m c vo mt th tch
nc ct. Ch ch c b sung t t axit vo nc m khng lm ngc li.
Cc dung dch (a) v (b) phi c bo v cn thn trong cc bnh ring
bit v ch ho trn chng trc khi s dng. Sau khi ho trn theo t l dn,
dung dch Amoni Molipdat trong axit Sunfuric phi c bo qun trong bnh
thu tinh xm mu v t ni ti.
Dung dch Thic Clorua
Ly 25 gam bt thic sch ho hc (hoc thic l) cho vo ng nghim c
vch mc 10 ml, sau cho thm vo 2 ml axit Clohydric m c v thn
trng hm nng trn hi nc. Sau khi thic tan ht th nng th tch dung
dch ln ti vch bng nc ct. ng nghim cha Thic Clorua c y kn
bng nt qua cm sn Pipet hoc ng ht. Dung dch Thic Clorua cn
phi lun lun mi, khng c s dng dung dch chun b qu 24 gi
xc nh Phtphat.
Dung dch chun Kali dihydro photphat (KH2PO4)
a. Dung dch chun chnh KH2PO4
Dung dch chun chnh c chun b t ch phm tinh khit ho hc.
Dng cn phn tch ly chnh xc 1,097 gam KH2PO4 tinh th v chuyn lng
cn ny vo bnh cu dung tch 1 lt qua phu thu tinh. Ra chn cn v phu
95
nhiu ln bng nc ct. Th tch cui cng ca dung dch l 1 lt. bo qun
dung dch cn phi cho thm vo 2 ml Clorofooc (CHCl3). Bnh ng dung
dch phi tht sch v c nt mi tht tt. Dung dch ny c th s dng trong
thi gian 2-3 thng. Dung dch chun chnh c chun b nh trn c nng
250 mgP/l tc l 1 ml dung dch c 0,25 mg Phtpho nguyn cht.
b. Dung dch chun lm vic KH2PO4
Dng pipet ly 1 ml dung dch chun chnh cho vo bnh cu dung tch 100
ml v nng th tch ti vch mc bng nc ct. Mt mililit dung dch chun
lm vic c 0,0025 mg Phtpho nguyn cht. Dung dch chun lm vic ch
chun b trc lc lm vic.
Nc bin khng c Phtpht
loi tr nh hng ca mui, ngi ta khng dng nc ct chun
b dung dch chun lm vic nh va m t m phi s dng nc bin khng c
Phtpht. Mun c nc bin khng Phtphat, phi chun b mt ho cht ph
sau y: Ly 0,3 ml dung dch xyt nitrat st 1,0N (hoc mt xyt st khc) ho
vi 0,3 ml dung dch kim (KOH hoc NaOH) 1,0N, th tch chung c nng
ln n 100 ml bng nc ct. Ho cht ph ny khi thm vo nc bin tng
mt mt lng khng nhiu s kt ta c Phtphat ca nc bin di dng
Phtpht st. Khi kt ta ng yn, gn ly phn trong sut bn trn v lc n
qua mt phu mn c ra s b bng axit Sunfuric long (1:20) v nc
ct. Nc bin khng Phtphat thu c bng cch trn vn c th cha mt
lng Phtphat khng nhiu, lng ny s c xc nh nh "th nghim trng"
s ni phn sau.
4.2.4. Ly v bo qun mu nc
Sau khi trng l v nt bng chnh nc bin cn ly, mu nc c
ly y vo l (ti thiu l 200 ml) v chuyn n vo phng th nghim mt thi
gian thch hp n c c nhit ca phng. Vic xc nh Phtpht cn
c tin hnh cng sm cng tt nhng khng c qu 6 gi k t khi ly
mu. Nu mu lu hn na th Phytoplankton trong mu c th thc hin
96
97
40, 50 v 60 gP/l.
To mu cho thang chun v lot mu phn tch
Thm ng thi vo mi mt ng tr cha mu nc phn tch v mi mt
ng tr ca thang chun mt lng 2 ml dung dch Amoni Molipdat trong Axit
Sunfuric v 2 git Thic Clorua. y nt cc ng tr li v khuy trn chng
bng cch o ngc. Khi dung dch c Photphat, mu xanh Molipen s hin
ln, cng ca mu t l vi nng Photpht trong cc dung dch. Trong
khong 5 pht k t khi khuy trn, mu s hin ln hon ton v n nh trong
vng 25-30 pht. Ta ch c php so mu ca chun v mu trong khong thi
gian ny. Sau thi gian n nh, mu ca c mu v chun u b bin i. V
vy, s lng mu trong lot mu chun b cn phi thch hp vic so mu
chng ch thc hin trong vng 25-30 pht.
Cn bng mu ca dung dch chun v mu
Vic so mu c tin hnh trong cp ng tr Hener. Trc ht, rt mt t
mu nc phn tch hin mu hon ton vo mt ng tr Hener, ng tr cn
li rt mt t dung dch chun c mu gn nht vi mu ca mu nc phn tch.
Cn bng mu ca chng bng cch cho chy t t qua van ca ng Hener dung
dch no c mu m hn (thng l mu nc), cho n khi mu 2 ng tr
nh nhau. Trong qu trnh cn bng mu, mt ngi phn tch lun nhn t pha
trn cc ng tr thng theo chiu dy cc dung dch.
Kt qu ch c chp nhn khi chiu cao ca cc cht lng trong hai ng
tr Hener khng khc nhau nhiu lm (khng c vt qu t l 1: 0,6-0,7).
Nu s khc nhau vt qu gii hn ny th phi thay th dung dch chun khc
c mu gn hn na vi mu ca mu.
Ghi kt qu so mu vo s chuyn mn bao gm chiu cao v nng
dung dch chun, chiu cao mu (theo s c trn thang chia ca ng Hener).
Sau ra sch cc ng Hener tip tc so mu mu khc. Trong trng hp
nng Phtphat ca cc mu trong lot mu chun b xp x nhau, tc l
mu ca cc mu gn tng t nhau th c th ch cn s dng mt dung dch
98
99
(4.2)
(4.3)
Trong X l nng Photphat trong nc bin khng Photphat, h1' chiu cao ct cht lng trong ng tr Hener cha dung dch chun c nng
yu nht v a' l nng ca n, h2'- chiu cao ct nc bin khng Photphat c
ho cht trong ng tr Hener cn li.
" bn" tng cng c tnh theo cng thc:
Z=X+Y
()
100
(4.5)
(4.6)
Bng 4.1: H s hiu chnh theo mui khi xc nh nng Phtphat trong nc bin bng
phng php so mu
S%o
0
k
1.00
S%o
8
k
1.18
S%o
16
k
1.25
S%o
24
k
1.31
S%o
32
k
1.34
1.04
1.19
17
1.26
25
1.31
33
1.34
1.05
10
1.20
18
1.26
26
1.32
34
1.35
1.09
11
1.22
19
1.27
27
1.32
35
1.35
1.11
12
1.23
20
1.28
28
1.32
36
1.35
1.12
13
1.23
21
1.29
29
1.32
37
1.36
1.14
14
1.24
22
1.29
30
1.33
38
1.36
1.16
15
1.25
23
1.30
31
1.33
39
1.37
101
102
hoc sau ngy lm vic. Kt qu tnh phi c ngi th hai kim tra.
4.3. XC NH SILICAT TRONG NC BIN
103
104
4.3.4. Qu trnh xc nh
V Silic v c thng tn ti trong nc bin vi nng ln, c th ti
hng nghn gSi/l, nn c hai cch so mu p dng cho hai trng hp khc
nhau: trng hp th nht khi nng Silic ca nc bin ln hn 500 gSi/l
v trng hp th hai - nh hn. Vic nhn bit nh tnh gi tr ny v la chn
cch so mu thch hp ph thuc rt nhiu vo kinh nghim ca ngi nghin
cu.
Trng hp th nht: Khi nng Silic ca mu ln hn 500 gSi/l
- Chun b lot mu: Ly 100 ml mi mu nc cho vo cc ng tr c
vch mc 100 (ng tr phi c trng bng nc mu), ghi li s hiu ng tr
tng ng vi s hiu mu.
- iu ch thang chun: Thang chun trong trng hp ny phi c nng
ln hn 500 gSi/l v gn vi nng d kin ca mu. Nu ly 1 ml dung
dch chun lm vic (nng 50 mgSi/l) ho vi nc bin khng silic thnh
100 ml th nng ca chun ny l 500 gSi/l. Cn chun b thang chun c t
4-5 dung dch chun vi nng khc nhau nhng gn vi nng Silic d
kin ca mu.
- To mu cho chun v mu: Sau khi c thang chun, cho thm ng
thi vo lot ng tr cha mu chun b v cc ng tr c dung dch chun 4
git H2SO4 50% (nu khi ly mu nc thm H2SO4 bo qun mu ri th
lc ny khng phi cho thm axit vo mu na). Tip theo cho thm vo tt c
cc ng tr 2 ml Amoni Molipdat 10% v y nt cc ng tr li, khuy u
bng cch o lc.
- So mu ca mu vi chun: Sau 20 pht khuy o cc dung dch, mu
vng ca chun v mu hin r th tin hnh so mu cc ng tr Hener, ging
nh m t khi xc nh Phtphat. Kt qu so mu c ghi vo s. Tip tc
so mu mu khc cho ht s mu c trong lot mu chun b.
Sau khi phn tch ht lot mu, tip tc chun b lot mu mi v thang
105
106
(4.7)
107
SO2(OH)
C6H4
SO2(OH)
HNO2
C6H4
NH2
+ H2O
N = NOH
(Axit Sunfonic)
(Fenidinitro-Sunfoniaxit)
SO2(OH)
C10H7NH2 C6H4
N = NOH
(Sunfoniaxit)
+ H2O
N = N - C10H6NH2
( )
(mu )
108
- Naphtylamin C10H7NH2
Ly 0,4 gam sch (c mu pht hng) ho vi vi git axit Axetic c ri
trn vi 300 ml Axit axetic 12%. Dung dch thu c phi trong sut, nu c
mu ti (c tp cht) th cn phi iu ch li n bng cch ly 0,4 gam ho
vi 20-30 ml nc ct, un nng hn hp cho n si. Sau khi ngui, tp cht s
ni ln trn mt dung dch di dng kt t mu tm xm. Lc ly phn trong
sut v ho n vi 300 ml axit Axetic 12%.
Hn hp Gris
Ho trn dung dch axit Sunfonic v - Naphtylamin chun b nh trn
theo t l 1:1. Hn hp Gris nhn c phi khng mu. Ch l c hai ho
cht axit Sunfonic v - Naphtylamin c chun b ring v bo qun trong
bng ti. Ch trc khi s dng mi ho trn chng vi nhau to thnh hn
hp Gris.
Dung dch chun chnh Natri Nitrit (hoc Kali Nitrit)
Ly 4,9270 gam NaNO2 kh sch ( c sy nhit 105-110oC cho
n trng lng khng i) ho vi nc ct thnh 1 lt. Sau cho thm 2
git Clorofooc bo v n. Dung dch ny tng i n nh v c th gi n
c 2-3 thng. i vi KNO2 th lng cn ly l 6,0770 gam. Nng Nitrit
(biu din qua nguyn t Nit) ca dung dch ny l 1 gN/l.
Dung dch chun trung gian
Pha long 100 ln dung dch chun chnh bng cch ly 1 ml chun chnh
ho vi nc ct thnh 100 ml. Nng dung dch chun trung gian l 0,01
gN/l hay 1 ml dung dch c 0,01 mg Nit. Dung dch ny c th gi c trong
7 ngy.
109
110
(4.8)
111
CH
2 HC
H
C
HC = CH
HC
mt 2H+
CH
CH
HC = CH
Mi trng H2SO4
(Diphelinamin (C6H5)2NH)
HC - CH
HC
HC =CH H
C-N=C
HC=CH
HC CH
C=N-C
CH
HC=CH
HC =CH
H HC=CH
HC=CH
Mi trng H2SO4
HC - CH
HC
HC =CH
C-N=C
HC=CH
HC=CH
C = C
HC =CH
HC=CH
HC CH
C=N-C
O
HC=CH
O = S =O
Hynoit-Ymol - tm xanh
112
OH
CH
113
114
115
116
20, 30, 40, 50, 60, 70, 80, 100 gN/l. Khi phi chun b thang chun c nng
cao t 500 g N/l tr ln th c th iu ch n trc tip t dung dch chun
chnh. Thang chun ch chun b trong ngy lm vic, khng s dng n ngy
hm sau.
4.5.4. Ly v bo qun mu nc
Ly mu xc nh Nitrt tng t nh ly mu xc nh Phtphat v
Silic. Mu c phn tch cng sm cng tt. Nu khng phn tch c ngay
trong vng 6 gi k t khi ly mu th phi bo qun mu bng cch thm 3-4
git Clorua thu ngn bo ho (hoc Clorofooc) cho 100 ml mu.
4.5.5. Qu trnh xc nh
Bt u mt ngy lm vic, ta chun b dung dch chun lm vic v thang
chun nh m t. Tip chun b lot mu nc phn tch vi s lng
thch hp.
To mu cho chun v mu
ong tht chnh xc 2 ml mi mt chun ca thang chun (k t nng
nh n ln) v cho ln lt vo cc ng nghim sch kh. Pipet phi c
trng 2 ln bng chnh chun cn ly. Sau ong 2 ml mi mu nc cn phn
tch cho ln lt vo cc ng nghim sch v kh khc (Pipet cng phi c
trng bng chnh mu nc cn ly). Tt c cc ng nghim phi hon ton nh
nhau v trnh nhm ln, chng phi c nh s tng ng vi cc chun
v s hiu cc mu. Tht cn thn, thm tip 5 ml Diphenilamin vo tt c cc
ng nghim c dung dch chun v mu nc. Khuy trn hn hp trong cc
ng nghim bng que thu tinh ln lt t nng nh n ln. Trc que
khuy phi lun lun c gi trong ng nghim c y axit Sunfuric 3:2 (60
ml H2SO4 m c ho vi 40 ml H2O).
Nn chun b c chun s "0" vo mt ng nghim m ch c 2 ml
nc ct v 5 ml Diphenilamin. Chun s "0" dng xc lp hiu chnh "
bn" ca ho cht Diphenilamin.
117
118
(4.9)
119
120
121
(4.10)
122
quang hc cho tng dung dch chun v tng mu ca lot mu chun b. Ghi
kt qu o vo s chuyn mn.
Bc 4: Lp li t bc 1 cho lot mu khc v thang chun khc.
Bc 5: Vic tnh ton kt qu c thc hin sau khi phn tch ht lot
mu hoc sau ngy lm vic. Cn c bit ch l mi mt lot mu u c
thang chun ring ca n nn khng c s dng tng quan D-C ca lot mu
ny cho lot mu khc.
4.7. XC NH HM LNG CHT HU C TRONG NC BIN QUA
NHU CU XY HO HC (COD)
123
c gi l " xy ho ca nc bin".
Ngun cung cp cc cht hu c cho nc bin ch yu l do qu trnh
phn hu tn tch hu c v cc sn phm ca qu trnh hot ng sng ca
ng thc vt bin, cc xc ng thc vt cht... Ngoi ra, cht hu c cn c
cung cp t cc dng lc a, t ngun nc thi ca cng nghip v sinh hot
(c bit l cng nghip ch bin c, giy v du la). Chnh v vy, COD ca
nc bin cn c coi l mt ch tiu ca nhim mi trng. Nghin cu
COD ca nc bin cng c ngha l nghin cu lng cht hu c trong bin,
l mt thng s quan trng trong vic tnh ton chu trnh chuyn ho vt cht
v nng lng trong h sinh thi bin.
4.7.2. Phng php xc nh COD nc bin
xy ho c ht cc cht hu c c trong 1 th tch nc bin, ngi
ta cho th tch nc bin y tc dng vi mt cht xy ho hot ng ho hc
cao. Tr s "nhu cu xy ho hc" ca nc bin c xc nh bng lng cht
xy ho tiu th trong qu trnh ny v biu din bng s miligam xy ca
cht xy ho .
Phng php xc nh COD ca nc bin theo nguyn tc trn c B.
A. Skopinshev xut nm 1948-1950 vi ni dung "xy ho nc bin bng
Kali Pemanganat" (cn gi l phng php Skopinshev). V nguyn tc, khi cho
KMnO4 tc dng vi cc cht hu c (trong nc bin) th Mangan ho tr 7 c
th chuyn thnh ho tr 4, 3 hoc 2 tu thuc vo iu kin ca mi trng xy
ra phn ng l axt, trung tnh hay kim.
Mn+7 + 3e- Mn+4 + e- Mn+3 + e- Mn+2
C th, nu mi trng l axt tnh (c nhiu H+) th Mangan7 ca KMnO4
s chuyn thnh Mangan2. V d phn ng gia KMnO4 v cht hu c l axt
Oxalic H2C2O4 xy ra trong mi trng axit nh sau:
2KMnO4+5H2C2O4+3H2SO4 K2SO4+2MnSO4+8H2O+10CO2
Hoc vit dng ion l:
124
(4.I)
(4.II)
125
126
127
128
129
COD(mgO2 / l ) =
(4.11)
130
131