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coeus.vn a18.CHẤT-GIỮ-MÀU
coeus.vn a18.CHẤT-GIỮ-MÀU
H NI - 2010
Li ni u
QCVN 4-5:2010/BYT do Ban son tho quy chun k thut
quc gia v Ph gia thc phm v cht h tr ch bin
bin son, Cc An ton v sinh thc phm trnh duyt v
c ban hnh theo Thng t s 22/2010/TT-BYT
ngy 20 thng 5 nm 2010 ca B trng B Y t.
1.1.
Ph lc 1:
1.2.
Ph lc 2:
1.3.
Ph lc 3:
1.4.
Ph lc 4:
Ph lc 1
YU CU K THUT V PHNG PHP TH I VI KALI NITRIT
1. Tn khc, ch s
Potassium nitrite
INS 249
ADI= 0 - 0,06 mg/kg th trng (Khng c s dng
trong thc phm cho tr nh di 3 thng tui).
2. nh ngha
Tn ha hc
Kali nitrit
M s C.A.S.
7758-09-0
Cng thc ha hc
KNO2
85,10
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Kali
Nitrit
Ch
6. Phng php th
6.1 tinh khit
Ch
6.2. nh lng
Cn khong 1,0 g (chnh xc n mg) mu th c
lm kh trn silicagen trong 4 gi, ho tan v nh mc
bng nc ct n vch trong bnh nh mc dung tch
100 ml. Dng pipet ht 10,0 ml dung dch ny v cho vo
hn hp gm 50,0 ml dung dch kali permanganat 0,1 N;
100 ml nc ct v 5 ml acid sulfuric, gi u ca pipet
di b mt ca hn hp dung dch. un nh dung dch
n 40 oC, yn trong 5 pht, sau thm 25 ml acid
oxalic 0,1 N. un hn hp n khong 80 oC v chun
bng dung dch kali permanganat 0,1 N.
% KNO2 =
(25 + X)
W
x 4,256
Trong :
X = Th tch kali permanganat 0,1 N dng chun
(ml)
W = Khi lng mu th (g)
Ph lc 2
YU CU K THUT V PHNG PHP TH I VI NATRI NITRIT
1. Tn khc, ch s
Sodium nitrite
INS 250
ADI= 0 - 0,06 mg/kg th trng (Khng nn s dng Natri
nitrit cho tr em di 3 thng tui)
2. nh ngha
Tn ha hc
Natri nitrit
M s C.A.S.
7632-00-0
Cng thc ha hc
NaNO2
69,00
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Natri
Nitrit
Ch
6. Phng php th
6.1 tinh khit
Ch
6.2. nh lng
(25 + X)
W
x 3,450
Trong :
X = Th tch kali permanganat 0,1N dng chun
(ml)
W = Khi lng mu th (g)
Ph lc 3
YU CU K THUT V PHNG PHP TH I VI NATRI NITRAT
1. Tn khc, ch s
2. nh ngha
Tn ha hc
Natri nitrat
M s C.A.S.
7631-99-4
Cng thc ha hc
NaNO3
85,00
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Natri
Nitrat
Nitrit
Ch
6. Phng php th
6.1. Th tinh khit
Ch
Nitrit
Nguyn l:
Xc nh bng phng php quang ph s dng phn
ng gia nitrit, suphanilamid v N-(1-naphthyl)-ethylendiamin dihydroclorid to nn phc mu hng. o
hp th quang ca dung dch ti bc sng 540 nm.
Thuc th:
- Dung dch sulfanilamid: Ha tan 2 g sulfanilamid vo
1000ml dung dch acid hydrocloric long (TS).
- Thuc th kt hp: Ho tan 0,2 g N-(1-naphthyl)ethylen-diamin dihydroclorid trong nc ct v pha
long n 100 ml. Bo qun trnh nh sng trong l
thy tinh mu nu v gi trong t lnh.
- Chun nitrit: Ha tan 0,750 g natri nitrit ( c lm
kh trc trong 4 gi trn silicagel) trong nc ct
v pha long n 1000 ml (500 g nitrit/ml). Ly 10 ml
dung dch gc ny pha long n 100 ml vi nc ct
(50 g nitrit/ml). Cui cng ly 10 ml dung dch ny,
pha long bng nc ct n 1000 ml, thu c chun
lm vic (0,5 g nitrit/ml).
Tin hnh:
Dng ng chun
Ln lt ly vo cc bnh nh mc dung tch 100 ml 0;
5 ml; 10 ml; 20 ml; 50 ml dung dch chun lm vic v
pha long bng nc ct n 80 ml (ng vi 0; 2,5; 5;
10; 25 g nitrit). Thm vo mi bnh 10 ml dung dch
sulfanilamid, lc u. yn trong 3 pht v thm 1 ml
thuc th kt hp ln lt vo cc bnh, pha long n
vch bng nc ct, lc u v yn trong 15 pht.
o hp th quang ca cc dung dch chun so vi
nc ct bc sng 540 nm, s dng cuvt 10 mm.
Dng ng chun biu th s ph thuc ca hp
th quang so vi lng nitrit trong dung dch (ng
chun phi l ng thng).
Tin hnh th
Cn khong 1 g mu (chnh xc n mg). Ha tan v
nh mc n 100 ml bng nc ct. Dng pipet ht
20ml dung dch, cho vo bnh nh mc 100 ml v pha
long bng nc ct n khong 80 ml. Thm 10 ml
dung dch sulfanilamid, lc u. yn trong 3 pht v
thm 1 ml thuc th kt hp, pha long n vch bng
nc ct, lc u v yn trong 15 pht. o hp
th quang ca dung dch chun so vi nc ct
bc sng 540 nm, s dng cuvt 10 mm. Da vo
ng chun v hp th quang ca dch th o
c, tnh lng nitrit c trong dch th.
Tnh kt qu
Hm lng nitrit =
Trong :
A x 5 (mg/kg)
W
Ph lc 4
YU CU K THUT V PHNG PHP TH I VI KALI NITRAT
1. Tn khc, ch s
INS 252
ADI = 0 - 3,7 mg/kg th trng (Khng s dng nitrat cho
tr em di 3 thng tui).
2. nh ngha
Tn ha hc
Kali nitrat
M s C.A.S.
7757-79-1
Cng thc ha hc
KNO3
101,11
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Kali
Nitrat
Nitrit
Ch
6. Phng php th
6.1. tinh khit
Nitrit
Nguyn l:
Xc nh bng phng php o quang s dng phn
ng gia nitrit, suphanilamid v N-(1-naphthyl)-ethylendiamin dihydroclorid trong nc to phc mu hng, o
hp th quang ca dung dch ti bc sng 540 nm.
Thuc th:
- Dung dch sulfanilamid: Ha tan 2 g sulfanilamid vo
dung dch acid hydrocloric long (TS) v nh mc n
1000 ml.
- Thuc th kt hp: Ho tan 0,2 g N-(1-naphthyl)ethylen-diamin dihydroclorid trong nc ct v nh mc
n 100 ml. Bo qun trnh nh sng trong l thy tinh
mu v gi trong t lnh.
- Chun nitrit: Ha tan 0,750 g Natri nitrit ( c lm
khan trc trong 4 gi trn silicagen) trong nc ct
v pha long n 1000 ml (500 g nitrit/ml). Ly 10 ml
dung dch gc pha long ra 100 ml vi nc ct (50 g
nitrit/ml). Cui cng ly 10 ml dung dch ny bng nc
ct n 1000 ml thu c chun lm vic (0,5 g
nitrit/ml).
Tin hnh:
Dng ng chun
Ln lt ly vo cc bnh nh mc dung tch 100 ml 0; 5
ml; 10 ml; 20 ml; 50 ml dung dch chun lm vic v pha
long vi 80 ml nc ct. Thm vo mi bnh 10 ml dung
dch sulfanilamid, lc u. yn trong 3 pht v thm 1
ml thuc th kt hp ln lt vo cc bnh, pha long
n vch th tch bng nc ct, lc u v yn trong
15 pht. o hp th quang ca cc dung dch chun
so vi nc ct bc sng 540 nm, s dng cuvt c
chiu dy 10 mm. Xy dng ng chun biu th s
ph thuc ca hp th quang so vi lng nitrit trong
dung dch (ng chun phi l ng tuyn tnh).
Tin hnh th
Cn khong 1 g mu (chnh xc n mg). Ha tan v
nh mc n 100 ml bng nc ct. Dng pipet ht 20
ml dung dch, cho vo bnh nh mc 100 ml v pha
long vi khong 80 ml nc ct. Thm vo 10 ml dung
dch sulfanilamid, lc u. yn trong 3 pht v thm
1ml thuc th kt hp, pha long n vch th tch bng
nc ct, lc u v yn trong 15 pht. o hp th
quang ca dung dch chun so vi nc ct bc
sng 540 nm, s dng cuvt c chiu dy 10 mm. Da
vo ng chun v hp th quang ca dch th o
c tnh lng nitrit c trong dch th.
Tnh kt qu
Hm lng nitrit =
Ax5
Trong :
A = Lng nitrit trong dch th ( g)
W = Khi lng mu th (g)
(mg/kg)
Ch
6.2. nh lng
Cn khong 0,4 g (chnh xc n mg) mu th c
sy kh ti 105 oC trong 4 gi, ho tan vo 300 ml nc
ct trong mt bnh cu dung tch 500 ml. Thm 3 g bt
hp kim Devada v 15 ml dg dch natri hydroxyd (nng
2/5). Lp bnh cu vi sinh hn v b phn chng
phun tro. yn khong 2 gi. Cho 50 ml dung dch
acid sulfuric 0,1N vo bnh hng dch ct, tin hnh ct
v thu ly khong 250 ml dch ct.Chun lng acid
sulfuric d bng dung dch natri hydroxyd 0,1N s dng
ch th l 3 git dung dch thuc th methyl/ xanh
methylen (TS). Tin hnh lm mu trng theo cch
lm i vi mu th v hiu chun kt qu, nu cn.
Mi ml dung dch acid sulfuric 0,1N tng ng vi
10,11 mg KNO3.