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AOAC Official Method 980.17


PHU GIA TRONG THIT BO ~ PHUONG PHAP QUANG PHO
Preservatives in Beef Spectrophotometric Method

1 Phm vi p dng
Tiu chun ny duoc p dung d xc dinh hm luong cc cht phu gia: benzoate,
sorbate v sulphit trong thit b.
2 Nguyn tc
Chit cc cht phu gia c trong thit bng nuoc ct.
2.1 Phn tch sulphit
Sulphit c trong dung dich chit phan ung voi thuc thu p-rosanilin trong HCl v
HCHO tao phuc mu hng tm v duoc dinh luong bng phuong php so mu o buoc
sng 560 nm.
Phan ung xay ra nhu sau:
2 NaCl + HgCl
2
= 2Na
+
+ [HgCl
4
]
2-

SO
2
+ [HgCl
4
]
2-
+ H
2
O = [HgCl
2
SO
3
]
2-
+ 2H
+
+ 2Cl
-

[HgCl
2
SO
3
]
2-
+ HCHO + 2H
+
= HO-CH
2
-SO
3
H + HgCl
2
HO-CH
2
-SO
3
H + C
19
H
18
N
3
Cl

+ HCl = axit Pararosanilin Metylsulfonic
(Pararosanilin) (mu do tm)
2.2 Phn tch benzoate, sorbate
Chit sorbate, benzoate c trong dung dich chit mu d duoc axt ha bng diethyl
ete. Lop dietyl ete sau khi chit duoc do o :
- Buoc sng 225 nm d phn tch benzoate
- Buoc sng 250 nm d phn tch sorbate
3 Thit b|, dng c, ha cht, dung d|ch
a. Thit b, dng c
- My quang ph phn tu UV-VIS (190 -1100 nm)
- Cn phn tch, d chnh xc 0,1 mg.
trang 2/4
- Pipt bu, pipet vach cc loai
- Bnh dinh muc dung tch 50mL, 100mL, ...
- Dung cu thuy tinh thng dung: erlen, becher, phu loc, ...
b. Ha cht
Ho cht phai l loai tinh khit duoc su dung d phn tch, gom:
- p-rosanilin.
- Thuy ngn clorua (HgCl
2
)
- NaCl
- Formaldehyde (HCHO)
- Axit clohydric dm dc
- Dietyl ete
c. Cht chun:
- Natrisulphit
- Kali sorbate
- Natri benzoate
d. Dung dch th v dung dch chun
- Thuc thu p-rosanilin: chuyn 100mg p-rosanilin vo bnh dinh muc 1000 mL,
thm vo bnh dinh muc 200 mL nuoc ct v 160 mL HCl (1:1). dinh muc dn
vach bng nuoc ct.
- Dung dich HCl (1:1): cho tu tu 100 mL HCl dm dc vo 100 mL nuoc ct
- Dung dich [HgCl
4
]
2-
: ha tan 4,7 g NaCl v 10,9 g HgCl
2
trong 1900 mL H
2
O,
dinh muc 2000 mL bng nuoc ct.
- Dung dich chun Natri sulphite 1000mg/L: ha tan 100 mg cht chun Na
2
SO
3

trong 100mL H
2
O.
- Dung dich formaldehyde 15 mg/100 mL: pha long 2 ml HCHO thnh 100 mL
bng H
2
O. Rt 2 ml dung dich ny pha long thnh 100 mL bng H
2
O.
4 Xy dng dy chun
4.1 Dy chun sulphit
- Dung dich chun Natri sulphite 1000mg/L: ha tan 100 mg cht chun Na
2
SO
3

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trong 100mL H
2
O.
- Chun bi cc bnh dinh muc c nt dy, dung tch 50 mL. Dnh s thu tu cho mi
bnh. Cho ln luot vo mi bnh ln luot cc cht theo bang sau:
Dung dich 0 1 2 3 4 5
Dung dich chun 1000 mg/L 0 0.5 1 1.5 2 3
Dinh muc dn vach 50 ml bng H
2
O ct. Lc du
Nng d Natri sulphit tuong ung, mg/L 0 10 20 30 40 50
Ly chnh xc 1 mL mi dung dich trn cho vo cc ng nghim ring bit
Dung dich [HgCl
4
]
2-
5 mL
Dung dich p-rosanilin 2.5 mL
Dung dich HCHO 1 mL
D yn 30 pht ri do o buoc sng 560 nm.
4.2 Dy chun sorbate v benzoate
Dung dich 0 1 2 3 4 5
Dung dich chun 1000 mg/L 0 0,5 1 1.5 2 3
Nng d chun tuong ung, mg/L 0 5 10 15 20 30
Dinh muc dn vach 50 mL bng H
2
O
Rt chnh xc 5 mL mi dung dich trn cho vo cc bnh dinh muc 50 mL khc
+ 0,5 mL HCl (1:1). Dinh muc dn vach bng dietyl ete, lc manh 1 pht. Rt ly
lop dung dich pha trn do.

5. Phn tch mu
- Cn khoang 10g mu d duoc dng nht vo ng ly tm 50 mL. Thm khoang 40
mL nuoc vo ng, lc du 2 pht. D yn 10 pht. Ly tm ly phn trong. Dinh
muc dung dich thu duoc thnh 50 mL.
- Phn tch Natri sulphit: Rt 1 mL dung dich trn cho vo ng nghim 10 mL,
thm tip 5 mL dung dich [HgCl
4
]
2-
, 2.5 mL dung dich thuc thu v 1mL dung
dich HCHO, d yn 30 pht ri do tai buoc sng 560 nm.
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- Phn tch sorbat, benzoat: Rt 5mL dung dich mu thu duoc o trn cho vo bnh
dinh muc 50 ml. t hnh tuong tu nhu chun.
6 Tnh kt qua
- Dng phn mm Excel dung duong chun biu thi mi quan h giua d hp thu
(Abs) v nng d cc chun cua cht phn tch
- Tnh ton h s tuong quan hi quy tuyn tnh (R
2
)
- Tnh nng d cht phn tch trong dung dich thng qua duong chun xy dung o
buoc trn.
- Nu mu c gi tri do duoc cao hon cc tri s cua cc dung dich chun, phai pha
long mu bng dung dich Blank.
- Hm luong cht phn tch c trong mu duoc tnh theo cng thuc sau:
f
m
V C
kg mg X
dm

=
0
) / (
Trong d:
- C
0
: nng d cht phn tch tnh tu duong chun, mg/L
- V
dm
: th tch dinh muc mu, mL
- m: khi luong mu phn tch, g
- f: h s pha long (nu c)

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