Professional Documents
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TRNG I HC KHOA HC
KHOA HA
....
Nguyn Th Hoa
Kha 2008 2012
Hu, 5/2012
1
I HC HU
TRNG I HC KHOA HC
KHOA HA
....
Hu, 5/2012
1
TM TT
X hi ngy mt vn minh, i sng con ngi ngy cng pht trin. Do vy,
nh gi cht lng thc phm l mt trong nhng vn m con ngi lun quan
tm.
Vi trnh khoa hc k thut ngy cng cao, ra i nhiu phng php
xc nh hm lng nitrat, nitrit trong mu thc phm. Tuy nhin phng php trc
quang l phng php c ng dng rng ri trong vic kim sot cht lng thc
phm ni chung, thc phm ch bin ni ring v phng php ny c th nh lng
nhanh chng vi chnh xc cao.
V vy, trong bn kha lun ny chng ti nghin cu qui trnh xc nh
nitrat, nitrit trong cc mu thc phm ch bin bng phng php trc quang da trn
c s phn ng to hp cht diazo ca axit sunfanilic v -naphthylamin.
Ni dung ca phng php nghin cu gm:
-
ii
DANH MC CC T VIT TT
CAC
Commission)
FAO
Organization)
WHO : T chc Y t th gii (World Health Organization)
TCVN : Tiu chun Vit Nam ( Viet Nam Standards)
HPLC : Sc k lng hiu nng cao (High Performance
Liquid
LOQ
SA
NA
Rev
: thu hi (Recovery)
RSD
iii
MC LC
Trang
Li cm n ................................................................................................................... i
Tm tt ........................................................................................................................ ii
Danh mc cc t vit tt ............................................................................................. iii
Mc lc ...................................................................................................................... iv
Danh mc cc bng..................................................................................................... vi
Danh mc cc hnh .................................................................................................... vii
M U .................................................................................................................... 1
Chng 1. TNG QUAN ........................................................................................... 2
1.1. Ph gia thc phm ............................................................................................ 2
1.1.1. Vai tr ca ph gia thc phm ................................................................ 3
1.1.2. nh hng ca ph gia thc phm n sc kho con ngi ................... 3
1.2. nh hng nitrat, nitrit ln sc khe con ngi ................................................ 4
1.3. Tnh cht ca nitrat, nitrit .................................................................................. 5
1.3.1. Tnh cht ca nitrat ................................................................................. 5
1.3.2. Tnh cht ca nitrit .................................................................................. 6
1.4. Cc phng php phn tch nitrat, nitrit ............................................................ 7
1.4.1. Cc phng php phn tch nitrat ............................................................ 7
1.4.2. Phng php phn tch nitrit .................................................................... 9
1.4.3. Cc phng php xc nh ng thi nitrat, nitrit .................................. 10
1.5. Cc phng php x l mu thc phm ......................................................... 11
1.5.1. K thut v c ha t .......................................................................... 11
1.5.2. K thut v c ha kh .......................................................................... 12
1.5.3. K thut v c ha kh t kt hp ....................................................... 12
1.6. C s ca phng php trc quang ................................................................. 13
1.6.1. nh lut Bouguer Lambert Beer ..................................................... 13
1.6.2. Phn tch nh lng.............................................................................. 14
iv
39
DANH MC CC BNG
Trang
Bng 2.1. Cc ha cht s dng................................................................................. 22
Bng 3.1. S ph thuc hp th quang ca dung dch cc hp cht mu diazo vo
nng axit sunfanilic ............................................................................. 24
Bng 3.2. S ph thuc hp th quang ca dung dch cc hp cht mu diazo vo
nng -naphthylamin ........................................................................... 26
Bng 3.3. S ph thuc hp th quang ca dung dch hp cht mu diazo theo pH ...... 27
Bng 3.4. S thay i hp th quang pH khc nhau vi ct kh Cd-Cu ............. 29
Bng 3.5. S thay i hp th quang pH khc nhau vi hn hp huyn ph km
+ dung dch CdSO4 ................................................................................... 30
Bng 3.6. S ph thuc hp th quang ca dung dch mu diazo vo nng nitrit
v phng trnh ng chun xc nh nitrit ............................................ 30
Bng 3.7. S ph thuc hp th quang ca dung dch mu diazo vo nng nitrat
v phng trnh ng chun xc nh nitrat ............................................ 32
Bng 3.8. Gii hn pht hin v gii hn nh lng ca nitrit, nitrat ........................ 33
Bng 3.9. S thay i hp th quang khi c nh nng nitrit ............................ 33
Bng 3.10. nh hng ca phng php x l mu n hp th quang ................ 35
Bng 3.11. Gi tr hp th quang tnh s mt mt nitrit qua qu trnh x l mu ... 36
Bng 3.12. Kt qu hm lng nitrat, nitrit trong Xc xch b ViSan ........................ 39
vi
DANH MC CC HNH
Trang
Hnh 1.1. Dng ng chun trong phn tch trc quang ........................................... 14
Hnh 1.2. Dng ng thm chun ............................................................................ 15
Hnh 2.1. Ph hp th ca hp cht mu diazo .......................................................... 21
Hnh 3.1. S ph thuc hp th quang ca dung dch hp cht mu diazo vo nng
SA ........................................................................................................ 25
Hnh 3.2. S ph thuc hp th quang ca dung dch hp cht mu diazo vo nng
NA ....................................................................................................... 26
Hnh 3.3. S ph thuc hp th quang ca dung dch mu diazo theo pH ............. 27
Hnh 3.4. S ph thuc hp th quang ca dung dch mu diazo theo thi gian .... 28
Hnh 3.5. S ph thuc hp th quang ca dung dch mu diazo vo nng nitrit
.................................................................................................................. 31
Hnh 3.6. S ph thuc hp th quang ca dung dch mu diazo vo nng nitrat
.................................................................................................................. 32
Hnh 3.7. S qui trnh phn tch nitrat, nitrit trong mu thc phm ch bin ......... 37
vii
M U
Trong cuc sng hin i, thc phm ch bin l nhng sn phm i lin vi
i sng hng ngy ca mi gia nh v n tit kim thi gian v tin bc cho thc n
ba n gia nh. Nhng iu ng lo ngi nht l cht lng ca thc phm ch bin
(hm lng cht bo qun, ph gia thc phm) m ngi sn xut a vo vi mc
ch gi gn v ko di thi gian s dng ca cc loi thc phm. Mt trong s l
nitrit, nitrat (mui dim) l mt dng mui c xp vo nhm cht bo qun c chc
nng n nh mu, ngn chn s pht trin ca vi sinh vt gy c.Tuy nhin nu dng
cc mui ny ch bin, bo qun khng ng qui nh th s l mi e da cho sc
khe con ngi. V th, vic xc nh hm lng nitrat, nitrit trong thc phm ch bin
l rt cn thit nhm m bo s an ton cho ngi tiu dng.
Trong bn kha lun ny chng ti nghin cu qui trnh xc nh nitrat, nitrit
trong cc mu thc phm ch bin da trn c s phn ng to hp cht diazo ca
nitrit vi axit sunfanilic v -napthylamin. Phng php ny c mt s u im nh
nhy ca phng php cao, t b nh hng ca cc cht cn tr, c th thc hin
cc phng th nghim trang b n gin.
Hin nay c nhiu nghin cu xc nh nitrat, nitrit tuy nhin cha c nhiu
nghin cu xc nh nitrat, nitrit trn thc phm ch bin mt cch y . V vy,
mc tiu ca chng ti l nghin cu xc nh nitrat, nitrit trong cc mu thc phm
ch bin bng phng php trc quang.V vi bt k phng php no th vic nghin
cu kho st cc iu kin thch hp phng php cho kt qu chnh xc nht vn
l nhim v quan trng nht.
Chng 1
TNG QUAN
1.1. Ph gia thc phm [4]
Theo FAO: Ph gia l cht khng dinh dng c thm vo cc sn phm vi
cc nh khc nhau. Thng thng cc cht ny c hm lng thp dng ci thin
tnh cht cm quan, cu trc, mi v cng nh bo qun sn phm.
Theo WHO: Ph gia l mt cht khc hn l thc phm hin din trong thc
phm l kt qu ca mt s mt: sn xut, ch bin, bao gi, tn tr...Cc cht ny
khng bao gm s nhim bn.
Theo y ban Tiu chun ha thc phm quc t (Codex Alimentarius
Commisson - CAC): Ph gia l mt cht c hay khng c gi tr dinh dng, khng
c tiu th thng thng nh mt thc phm v cng khng c s dng nh mt
thnh phn ca thc phm. Vic b sung chng vo thc phm gii quyt mc ch
cng ngh trong sn xut, ch bin, bao gi, bo qun, vn chuyn thc phm, nhm
ci thin cu kt hoc c tnh k thut ca thc phm . Ph gia thc phm khng
bao gm cc cht nhim hoc cc cht c b sung vo thc phm nhm duy tr hay
ci thin thnh phn dinh dng ca thc phm.
Theo TCVN: Ph gia thc phm l nhng cht khng c coi l thc phm
hay mt thnh phn ch yu ca thc phm, c hoc khng c gi tr dinh dng, m
bo an ton cho sc khe, c ch ng cho vo thc phm vi mt lng nh nhm
duy tr cht lng, hnh dng, mi v, kim hoc axt ca thc phm, p ng v
yu cu cng ngh trong ch bin, ng gi, vn chuyn v bo qun thc phm.
Nh vy, ph gia thc phm khng phi l thc phm m n c b sung mt
cch ch , trc tip hoc gin tip vo thc phm, ci thin tnh cht hoc c tnh k
thut ca thc phm . Ph gia thc phm tn ti trong thc phm nh mt thnh
phn ca thc phm vi mt gii hn ti a cho php c quy nh.
2 NaNO3 =
2 NaNO2
O2
Nitrat ca nhng kim loi t Magie n ng, khi un nng b phn hy thnh
oxyt, nit dioxyt v oxy.
V d:
2 Pb(NO3)2 =
2 PbO
4 NO2
+ O2
Hg(NO3)2
Hg +
5
2 NO2 +
O2
Cch phn hy khc nhau ca mui nitrat kim loi l do bn khc nhau ca
mui nitrit v oxyt ca ca cc kim loi quyt nh. Chng hn nh NaNO2 v PbO
bn, trong khi Pb(NO2)2, Hg(NO2)2 v HgO khng bn.
Do d mt oxi, cc mui nitrat khan khi un nng l cht oxi ha mnh.
Ion NO3- trong mi trng axit c kh nng oxi ha nh axit nitric, trong mi
trng trung tnh hu nh khng c kh nng oxy ha, nhng trong mi trng kim
c th b Al, Zn kh n NH3.
V d: NaNO3 + 4 Zn + 7 NaOH + 6 H2O = 4 Na2[Zn(OH)4] + NH3
1.3.2. Tnh cht ca nitrit [6]
1.3.2.1. Tnh cht vt l
Nitrit l mui ca axit nitr. Hu ht mui nitrit d tan trong nc, mui t tan
l AgNO2. Cng nh mui nitrat, a s mui nitrit khng c mu.
1.3.2.2. Tnh cht ha hc
Nitrit ca kim loi kim bn vi nhit, chng khng phn hu khi nng chy
m ch phn hu trn 500oC. Nitrit ca cc kim loi khc km bn hn, b phn hu
khi un nng, chng hn nh AgNO2 phn hu 140oC, Hg(NO2)2 75oC.
Trong mi trng axit, mui nitrit c tnh oxy ha v tnh kh nh axit nitr.
Mui nitrit oxy ha c axit HI n I2, dung dch SO2 n H2SO4, ion Fe2+ n
Fe3+ ... cn bn thn n chuyn thnh NO.
V d:
2 HI +
2 NO2- + 2 H+
2 NO + I2
2 H2 O
OH
COONa
+
NO3-
COONa
H+
O3N
(p-nitrosalixylat)
+ NH3 = C6H2(NO2)2ONH4
HO3S
HO3S
N N
2H2O
diazonium
axit sunfanilic
NH2
HO3S
NH2
N N+
HO3S
N=N
(diazonium)
Cht mu
diazo
-naphthylamin
9
+ H+
10
11
b. X l mu trong l vi sng:
Trong cc h l n gin:
H bnh mu h;
H bnh mu ng kn (c p sut cao);
Trong cc h nhiu bnh v t ng hon ton:
H bnh mu h c khng ch nhit ;
H bnh mu ng kn (c p sut cao) c khng ch nhit v p sut;
X l trong l vi sng h kn (c p sut) th ch cn 50 - 60 pht.
1.5.2. K thut v c ha kh
Nung x l s b mu c ph gia v cht bo v l qu trnh x l mu s b
nh tc dng ca nhit thch hp, c thm tng tc h tr ca cht ph gia, thng
l cc cht chy, axit c ph v cu trc dng tinh th ban u ca mu phn tch,
chuyn n sang mt dng cc hp cht khc d ha tan tip bng axit. Khi c cht
chy, nhit nung thng thp hn khi khng c cht chy, thi gian ngn hn, song
li trit hn, m li khng mt cht phn tch. Nht l cc mu c cu trc bn, chu
nhit hay mu hu c th tc dng cu cht bo v l rt quan trng.
V d: Tro ho mu sa xc nh cc kim loi (Na, K, Ca, Mg, Cd, Co, Cr,
Cu, Fe, Mn, Ni, Pb, Zn), dng cht ph gia l 8 mL H2SO4 45% v 2 g KNO3. Ly 5 g
mu vo chn nung thch anh, thm cht ph gia, trn u, sy kh cn thn cho mu
kh v thnh than en, sau em nung 3 gi u nhit 440-4500C, ri sau
550-5300C, n khi ht than en, c tro mu trng. Sau ha tan tro thu c
trong 15 mL dung dch HCl 18%, un nh cho mu tan ht ri nh mc thanh 25 mL
bng dung dch HCl 2%.
1.5.3. K thut v c ha kh t kt hp
V l x l kh t kt hp l k tip nhau, trc tin x l t s b, sau
mi nung, nn tnh cht v din bin ca n cng tng t nh trong hai kiu
cp trn, ch c khc l sau khi x l mu khng phi ui lng axit d qu nhiu
12
: nng ca cu t (mol/L)
(1.1)
14
Cx
Cx + C1
Cx + C2
...
Cx + Cn
Ax
Ax+1
Ax+2
...
Ax+n
15
Chng 2
NI DUNG V PHNG PHP NGHIN CU
b. Chn pH kh thch hp
Thc hin phn ng kh vi hn hp huyn ph km + dung dch CdSO4
chn cc pH khc nhau chn pH thch hp.
2.1.2. nh gi tin cy ca phng php
2.1.2.1. Xc nh gii hn pht hin, gii hn nh lng
- Gii hn pht hin (LOD): L nng nh nht ca cht phn tch to ra c mt
tn hiu o c th phn bit mt cch tin cy vi tn hiu o ca mu trng (hay tn
hiu nn). Gii hn pht hin c xc nh theo qui tc 3.
y = yB + 3B hay y = yB + 3SB
Trong :
(2.1)
y: tn hiu ng vi LOD
yB: tn hiu ng vi mu trng (blank)
B (hay SB): lch chun ca tn hiu mu trng
(y
Yi ) 2
n2
(2.2)
y = yB + 3SB = a + 3Sy/C
(2.3)
17
2.1.2.2. nh gi lp li
Tin hnh th nghim 4 - 5 ln trn mi mu thc phm ch bin bng phng
php thm chun xc nh lp li thng qua gi tr lch chun tng i
(RSD). Theo cc cng thc sau:
n
S2 =
Phng sai:
xi2
xi)2
(
i=1
n
i= 1
(2.5)
n-1
S
100 (%)
x
(2.6)
(2.7)
Re v(%)
C x a Cx
.100
Ca
(2.8)
18
S a2
1
S b2
(2.9)
S2
xa xb
S
na .nb
na nb
(2.10)
(2.11)
Trong :
n: S th nghim
xi: Gi tr trung bnh ca xi
Si 2: Phng sai ca dy kt qu i
2.1.3. Kho st phng php x l mu thc phm
Tin hnh chit nitrat, nitrit trong mu thc phm ch bin bng hai phng
php khc nhau l: ngm nhit khong t 50 - 60oC, rung siu m tm ra
phng php no chit nitrat, nitrit l hiu qu cao nht.
2.1.4. Xc nh m trong mu thc phm ch bin
ng vi mi loi thc phm ch bin, xc nh m ca chng bng cch sy
kh cc thy tinh n khi lng khng i c m1 (g), sau thm mt lng mu
vo em cn c cc v mu c m2 (g), sy kh mu nhit t 100 - 105oC n
khi lng khng i c m3 (g). m c xc nh theo cng thc sau:
m2 - m3
X = m - m .1 0 0 %
2
1
19
(2.12)
2.1.5. p dng quy trnh x l mu phn tch nitrat, nitrit trong mu thc phm
ch bin
T cc iu kin kho st c trn, tin hnh h thng li thnh mt quy
trnh phn tch hon chnh xc nh hm lng nitrat v nitrit trong mu thc phm
ch bin.
2.1.6. Th p dng qui trnh phn tch trn cc i tng thc t
2.2. Phng php nghin cu
2.2.1. Cc phng php nghin cu
2.2.1.1. C s l thuyt ca phng php [9], [15]
Phng php xc nh nitrit da trn c s phn ng ca nitrit vi hn hp
thuc th axit sunfanilic v -naphthylamin to thnh hp cht diazo mu . o
hp th quang ca dung dch bc sng = 540 nm, phn ng nh sau:
NH 2 +
HO3S
NO2-
2H +
HO3S
(axit sunfanilic)
N N
2H 2O
(diazonium)
NH2
NH2
HO3S
N N+
HO3S
N=N
+ H
(diazonium)
Cht
mu diazo
-naphthylamin
20
(2.13)
: nng cu t (mol/L)
2.2.2.2. Ha cht
Cc ha cht s dng c lit k bng 2.1
Bng 2.1. Cc ha cht s dng
Tn ha cht
Xut x
Tn ha cht
Xut x
KNO2
Trung Quc
Km acetat
Trung Quc
KNO3
Trung Quc
HCl m c
Trung Quc
Axit sunfanilic
CH3COOH m c
Trung Quc
-naphthylamin
Trung Quc
Chlorofom
Trung Quc
EDTA
Trung Quc
CdSO4
Trung Quc
NaOH
Trung Quc
Zn
Trung Quc
Natri borat
Trung Quc
Trung Quc
K4[Fe(CN)6]
Trung Quc
22
Chng 3
KT QU V THO LUN
3.1. Kho st cc yu t nh hng tm iu kin thch hp cho phng php
3.1.1. iu kin xc nh nitrit
3.1.1.1. Nng v t l nng -naphthylamin v axit sunfanilic
a. nh hng nng axit sunfanilic n hp th quang ca dung dch hp cht
mu diazo
Ht 5 mL dung dch KNO2 10 mg/L, 3 mL dung dch HCl 0,16 M, sau thm
vo mi bnh mt th tch khc nhau ca dung dch SA c nng bng 2,5.10-3 M, ri
1,0 mL dung dch NA 2,5.10-2 M cho tt c cc bnh nh bng 3.1. nh mc n 50
mL c nng SA thay i trong khong t 0,5.10-4 10,5.10-4 M. Lc cn thn,
o hp th quang ca dung dch sau 15 pht bc sng = 540 nm. Kt qu ch
ra bng 3.1 v hnh 3.1.
Bng 3.1. S ph thuc hp th quang ca dung dch cc hp cht mu diazo
vo nng axit sunfanilic
CSA.10-4 (M)
CSA.10-4 (M)
0,5
0,323
7,5
0,374
1,5
0,373
8,5
0,367
2,5
0,383
9,5
0,363
3,5
0,382
10,5
0,356
4,5
0,382
6,5
0,378
24
0.39
0.38
0.37
0.36
0.35
0.34
0.33
0.32
0
10
12
-4
C SA.10 (M)
25
CNA.10-4 (M)
0,5
0,205
7,5
0,370
1,5
0,334
8,5
0,369
2,5
0,374
9,5
0,376
3,5
0,373
10,5
0,375
4,5
0,369
6,5
0,367
0.38
0.36
0.34
0.32
0.30
0.28
0.26
0.24
0.22
0.20
0
10
12
-4
CNA.10 (M)
= 1.
1,14
1,50
1,67
1,78
1,82
1,95
2,00
2,03
2,07
0,136
0,256
0,280
0,312
0,337
0,351
0,361
0,372
0,370
0.40
0.35
0.30
0.25
0.20
0.15
0.10
1.0
1.2
1.4
1.6
1.8
2.0
2.2
pH
27
0 .3 0
0 .2 8
0 .2 6
0 .2 4
0 .2 2
0
5 00
10 0 0
1 5 00
2 00 0
T hoi g ia n (s)
Hnh 3.4. S ph thuc hp th quang ca dung dch mu diazo theo thi gian
T hnh 3.4 cho thy: Thi gian bn mu ca hp cht diazo t 15 pht tr ln.
3.1.2. iu kin kh t nitrat qua nitrit
3.1.2.1. Chn phng php kh
3.1.2.1.1. Kh bng ct kh Cd-Cu [9]
a. Chun b ct kh Cd-Cu
Chun b hn hp Cd Cu: cn khong 25 g cadmi (Cd) kim loi dng ht,
ra Cd bng HCl 6 M cho n khi b mt Cd c mu trng bc. Gn ly Cd v ra
sch bng nc ct. Thm 100 mL dung dch CuSO4 2% v khuy cho n khi mt
mu xanh ca CuSO4. Gn ly Cd v lp li vic x l vi CuSO4 2% cho n khi bt
u xut hin kt ta keo nu (Cu kim loi). Ra cn thn bng nc ct loi ht kt
ta keo nu ny. Hn hp Cd Cu thu c c mu en.
Nhi ct: dng mt buret loi tt c dung tch 25 mL, nhi mt lp bng thy
tinh mng vo y ct, ng kha buret ri thm nc ct vo y. Nhi hn hp Cd
Cu ln ct. Ph ln trn b mt ct mt lp bng thy tinh mng.
28
A(Ct Cd-Cu)
9,34
0,193
0,197
0,189
10,0
0,201
0,210
0,207
9,34
0,212
0,214
0,217
10,0
0,223
0,227
0,224
0,1
0,5
0,9
1,3
1,7
2,1
0,036
0,188
0,327
0,463
0,586
0,691
ng chun
Y = 0,013 + 0,334 .X
0.9984
0,013
b (mg/L)
0,334
Sa
0,010
Sb (mg/L)
0,008
Sy/x
0,016
30
0.7
0.6
0.5
0.4
0.3
0.2
0.1
0.0
0.0
0.5
1.0
1.5
2.0
2.5
31
0,5
1,5
2,5
0,045
0,087
0,134
0,171
0,189
0,247
ng chun
Y = 0,005 + 0,080 .X
0,9955
0,005
b (mg/L)
0,080
Sa
0,006
Sb (mg/L)
0,003
Sy/x
0,009
0.25
0.20
0.15
0.10
0.05
0.5
1.0
1.5
2 .0
2 .5
3 .0
NO3
(m g NO /L)
3
32
Xc nh gii hn
Nitrit (mg/L)
Nitrat (mg/L)
0,144
0,338
0,432
1,014
Cnitrat
(mg KNO2/L)
(mg KNO3/L)
1,5
0,00
0,386
1,5
0,15
0,386
1,5
0,30
0,386
1,5
0,45
0,386
1,5
0,60
0,388
1,5
0,75
0,386
1,5
0,90
0,390
1,5
1,05
0,388
1,5
1,20
0,387
1,5
1,35
0,388
Stt
33
Cnitrit
Cnitrat
(mg KNO2/L)
(mg KNO3/L)
1,5
0,00
0,552
1,5
3,00
0,555
1,5
4,50
0,554
1,5
6,00
0,555
1,5
7,50
0,555
1,5
9,00
0,561
1,5
10,5
0,556
1,5
12,0
0,558
1,5
13,5
0,577
1,5
15,0
0,557
Stt
Ngm chit
Rung siu m
Khng qua kh
Qua kh
Khng qua kh
Qua kh
Atb1
0,012
0,069
0,012
0,120
Atb2
0,016
0,151
0,016
0,146
Atb3
0,021
0,178
0,026
0,171
Atb
0,016
0,133
0,018
0,146
S2
0,000025
0,0032
0,0001
0,0007
TN1
A x = 0,149
C (mg/L)
C x = 0,017 0,002
Rev (%)
TN2
Ax a = 0,288
Cx a = 0,189 0,001
17,2
(Ca ~ 1 mg/L)
36
3.6. p quy trnh x l mu phn tch nitrat, nitrit trong mu thc phm ch
bin
Thi mng
Cn mmu = 30 g, thm 100 mL nc ct, thm 8 mL Natri
borat bo ha, thm 0,5 g than hot tnh
Ngm chit 50-60 0C, 15 pht
ngui n nhit phng
Thm 5 mL K4[Fe(CN)6] 0,4 M
Thm 5 mL Zn(CH3COOH)2
Thm 8 mL Natri borat bo ha
nh mc V0 = 250 mL
lng 30 pht
Lc ly dch lc
Xc nh nitrit
+ V1 = 10 mL mu
+ Thm chun bng KNO2 10 mg/L (*)
+ 0,2 mL HCl 0,16 M
+ 1 mL EDTA 0,013 M
+ 5 mL axit sunfanilic 0,0025 M
+ 0,5 mL -napthylamin 0,025 M
+ V3 = 10 mL mu
+Thm chun bng KNO3 50 mg/L (**)
+ iu chnh pH = 8,5 10
Kh bng: 1 mL CdSO4 0,114 M
1 mL huyn ph km trong ng ly
tm 15 mL (V4)
nh mc 50 mL (V2)
Hnh 3.7. S qui trnh phn tch nitrat, nitrit trong mu thc phm ch bin
37
Trong :
(*) : Thm chun vi th tch l 0; 0,5; 5 mL dung dch KNO2 (10 mg/L)
(**): Thm chun vi th tch l 0; 0,5; 1,5 mL dung dch KNO3 (50 mg/L)
3.7. Xc nh nitrit, nitrat trong mu tht
T kt qu kho st cc iu kin thch hp cho phng php xc nh nitrit,
nitrat c p dng phn tch trn mt s mu thc phm ch bin tht. C th l
mu Xc xch b ViSan.
Quy trnh x l mu tin hnh theo quy trnh c trnh by trong mc 3.7.
Phng php nh lng l phng php thm chun.
Kt qu hm lng nitrit, nitrat trong mu c xc nh theo cc cng thc sau:
Hm lng nitrit (mg NO2-/kg) c xc nh theo cng thc:
mnitrit (1kg )
a V2 V0 1000
. .
.
( mg / kg )
b V1 1000 mmu
a V6 V4 V0 1000
. . .
.
( mg / kg )
b V5 V3 1000 mmu
38
Xc xch
b ViSan
(NSX:
10/3/2012)
a
im
Siu
th
Thun
Thnh
Mart
lp li (%)
m
(%)
Nitrit
Nitrat
0,7
0,011
0,71
10,04
(n=3)
(n=3)
(n=3)
Nitrit
Nitrat
RSD = 11,76
RSD = 50
RSDH = 3,69
RSDH = 2,65
(n=3)
(n=3)
So snh kt qu hm lng nitrat bng 3.12 vi tiu chun Vit Nam [8] cho
thy hm lng nitrat trong mu Xc xch b thp hn ngng cho php. Vy mu
Xc xch b trn c hm lng nitrat cho php s dng.
39
Chng 4
KT LUN V KIN NGH
4.1. Kt lun
1. kho st c v la chn c iu kin thch hp cho phn ng to
mu ca hp cht diazo gia nitrit, -naphthylamin, axit sunfanilic. Cc iu kin nh
sau:
C -naphthylamin
: 2,5.10-4 M
C axit sunfanilic
: 2,5.10-4 M
pH
: 1,95 2,03
40
Trn T Hiu, T Vng Nghi, Nguyn Vn Ri, Nguyn Xun Trung (2003),
Ha hc phn tch phn 2, Nxb i hc Quc gia H Ni, tr. 5 - 27.
[2].
[3].
[4].
Nguyn Ch Linh (2007), Bi ging Ph gia trong ch bin thc phm, Trng
Cao ng cng ng Kin Giang, Rch Gi.
[5].
[6].
Hong Nhm (2001), Ha hc v c, tp hai, Nxb Gio dc, tr. 188 189.
[7].
Kim Oanh (2001), Nitrat v sc khe con ngi , Vin la ng bng sng
Cu Long, tr1.
[8].
[9].
Quy trnh phn tch cc thng s cht lng nc v trm tch, nh gi cht
lng nc v trm tch m ph Tam Giang Cu Hai, D n IMOLA
(2006).
41
http://songthan.info/chi-phan-mem-download/430332/vai-tro-cua-phu-gia-thucpham-download.htmL
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