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CNG HO X HI CH NGHA VIT NAM

QCVN 12-3 : 2011/BYT







QUY CHUN K THUT QUC GIA
V V SINH AN TON I VI BAO B, DNG C BNG
KIM LOI TIP XC TRC TIP VI THC PHM

National technical regulation on safety
and hygiene for metalic containers in direct contact with foods















H NI - 2011

2










Li ni u
QCVN 12-3:2011/BYT do Ban son tho Quy chun k thut
quc gia v bao b v cc vt liu tip xc trc tip vi thc
phm bin son, Cc An ton v sinh thc phm trnh duyt
v c ban hnh theo Thng t s 34/2011/TT-BYT ngy 30
thng 8 nm 2011 ca B trng B Y t.
























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QUY CHUN K THUT QUC GIA
V V SINH AN TON I VI BAO B, DNG C BNG KIM LOI
TIP XC TRC TIP VI THC PHM

National technical regulation on safety
and hygiene for metalic containers in direct contact with foods

I. QUY NH CHUNG

1. Phm vi iu chnh
Quy chun k thut quc gia (sau y gi tt l Quy chun) ny quy nh cc
yu cu k thut v qun l v v sinh an ton i vi bao b, dng c bng kim
loi tip xc trc tip vi thc phm (sau y gi tt l bao b, dng c kim loi).
2. i tng p dng
Quy chun ny p dng i vi:
2.1. T chc, c nhn nhp khu, sn xut, bun bn v s dng cc sn phm
bao b, dng c kim loi.
2.2. C quan qun l nh nc v cc t chc c nhn c lin quan khc.
3. Gii thch t ng
3.1 Dung dich ngm thi: l dung mi dng ngm mu th.
II. YU CU K THUT
Th thi nhim
Ch tiu kim
tra
iu kin ngm thi Dung dch ngm thi Gii hn ti a
Arsen

60
0
C trong 30 pht
[5]
Nc
[3]

0,2 g/ml
60
0
C trong 30 pht
Dung dch acid citric
0.5%
[4]

Cadimi
60
0
C trong 30 pht
[5]
Nc
[3]

0,1 g/ml
60
0
C trong 30 pht
Dung dch acid citric
0.5%
[4]

Ch
60
0
C trong 30 pht
[5]
Nc
[3]

0,4 g/ml
60
0
C trong 30 pht
Dung dch acid citric
0.5%
[4]

Phenol
60
0
C trong 30 pht
[5]
Nc
5 g/ml
[8]

Formaldehyd m tnh
[8]

Cn kh
25
0
C trong 1 gi Heptan
[1] , [6]

30 g/ml
[8]
60
0
C trong 30 pht Ethanol 20%
[2]

60
0
C trong 30 pht
[5]
Nc
[3] , [7]

4
Acid acetic 4%
[4]

Epichlorohydrin 25
0
C trong 2 gi Pentan 0,5 g/ml
[8] , [9]

Vinylchlorid
Khng qu 5
0
C trong
24h
Ethanol 20% 0,05 g/ml
[8]


Ghi ch
[1]
Bao b, dng c kim loi dng cha ng cht bo, du n v thc phm cha cht bo.
[2]
Bao b, dng c kim loi dng cha ng ung c cn.
[3]
Bao b, dng c kim loi dng cha ng thc phm c pH ln hn 5.
[4]
Bao b, dng c kim loi dng cha ng thc phm c pH nh hn hoc bng 5.
[5]
Bao b, dng c kim loi s dng nhit ln hn 100
0
C iu kin ngm 95
0
C trong 30 pht.
[6]
Hm lng cn kh khng qu 90 g/ml trong trng hp mu l hp c ph bn trong mt
lp ph c nguyn liu chnh l cc loi du t nhin hoc cht bo v hm lng ca km oxyd trong
lp ph ln hn 3%.
[7]
S lng mt cht ha tan trong cloroform (gii hn n 30g/ml hoc t hn) c xc nh khi mt
mu c th c s dng tng t nh
[6]
v s lng vt qu 30g/ml.
[8]
Khng p dng i vi cc bao b, dng c kim loi khng ph 1 lp nha tng hp tip xc trc tip
vi thc phm.
[9]
Dung dch ra gii c c c 5 ln, mc d nng trong dung dch ra gii
khng qu 25g/ml.

III. PHNG PHP TH V LY MU
Phng php th v ly mu c quy nh ti ph lc hnh km theo quy
chun ny.
IV. YU CU QUN L
1. Cng b hp quy
1.1 Cc sn phm bao b, dng c kim loi nhp khu, sn xut, bun bn
v s dng trong nc phi c cng b hp quy ph hp vi cc quy nh ti
Quy chun ny.
1.2 Phng thc, trnh t, th tc cng b hp quy c thc hin theo
Quy nh v chng nhn hp chun, chng nhn hp quy v cng b hp chun,
cng b hp quy c ban hnh km theo Quyt nh s 24/2007/Q BKHCN
ngy 28 thng 09 nm 2007 ca B trng B Khoa hc v Cng ngh v cc
quy nh ca php lut.
2. Kim tra nh nc i vi bao b, dng c kim loi
Vic kim tra nh nc i vi cc sn phm bao b, dng c kim loi phi
c thc hin theo qui nh ca php lut.
V. TRCH NHIM CA T CHC, C NHN
1. T chc, c nhn nhp khu, sn xut, bun bn v s dng cc sn phm
bao b, dng c kim loi phi cng b hp quy ph hp vi cc quy nh k thut ti
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Quy chun ny, ng k bn cng b hp quy ti Cc An ton v sinh thc phm v
bo m cht lng, v sinh an ton theo ng ni dung cng b.
2. T chc c nhn ch c php nhp khu, sn xut, bun bn v s dng
cc sn phm bao b, dng c kim loi sau khi hon tt ng k bn cng b hp
quy v bo m cht lng, v sinh an ton ph hp vi cc quy nh ca php lut.

VI. T CHC THC HIN
1. Giao Cc An ton v sinh thc phm ch tr, phi hp vi cc c quan chc
nng c lin quan hng dn trin khai v t chc vic thc hin Quy chun ny.
2. Cn c vo yu cu qun l, Cc An ton v sinh thc phm c trch nhim
kin ngh B Y t sa i, b sung Quy chun ny.


























6
Ph lc
PHNG PHP TH THI NHIM

1. Chun b dung dch th:
- Ra sch mu bng nc ct, x l mu th thi nhim theo hng dn c
th sau:
i vi mu c th ng cht lng, cho dung dch ngm thi vo trong lng
mu.
i vi mu khng th cha ng cht lng, ngm mu ngp trong dung dch
ngm thi theo t l 2 ml/cm2 din tch b mt mu th.
- S dng dung dch ngm thi v iu kin ngm thi theo hng dn ti mc II.
Quy nh k thut.
2. Xc nh hm lng ch v cadmi
2.1 Chun b dung dch chun
2.1.1 Cadmi
- Dung dch cadmi chun gc:
Cn 100 mg cadmi, ha tan trong 50 ml acid nitric 10%, c trn bp cch thy. Sau
thm acid nitric 0,1 mol/l ha tan v nh mc n 100 ml. Dung dch
chun cadmi gc ny c nng 1 mg/ml.
- Dung dch cadmi chun lm vic:
Ly chnh xc 2 ml dung dch cadmi chun gc, v thm dung dch lm dung dch
ngm thi, nh mc n 100 ml. Nng dung dch cadmi chun lm vic 0,1
g/ml.
2.1.2 Ch
- Dung dch chun ch gc:
Ha tan 159,8 mg ch (II) nitrat trong 10 ml acid nitric 10%, v thm nc ct nh
mc n 100 ml. Dung dch chun ch gc ny c nng 1 mg/ml.
- Dung dch chun ch lm vic:
Ly chnh xc 8 ml dung dch ch chun gc, thm dung dch lm dung dch ngm
thi v nh mc n 100 ml. Dung dch ch chun lm vic c nng 0,4
g/ml.
2.2 Tin hnh
Xc nh ch v cadmi trong dung dch th bng phng php quang ph hp th
nguyn t hoc quang ph pht x plasma.

3. Xc nh Arsen
3.1 Chun b dung dch chun gc:
- Chun b dung dch chun gc:
Nghin mn arsen trioxyd, sy kh trong 4 gi 105C, cn 0,10g, thm 5ml dung
dch NaOH (1 5) v ha tan. Trung ha dung dch ny bng acid sulfuric (1
20), thm 10 ml acid sulfuric d (1 20), thm nc va un si v ngui, nh
mc n 1.000 ml. Nng dung dch chun lm vic l 0,1 g /ml.
-Chun b dung dch chun lm vic :
Ly 10 ml dung dch arsen chun gc, thm 10 ml acid sulfuric (1 20), thm
nc va un si v ngui, nh mc n 1.000 ml. Nng dung dch
chun lm vic l 0.1 g /ml.
7

Ch chun b dung dch chun lm vic ngay trc khi s dng v lu tr trong mt
bnh kn.
3.2 Dung dch hp th arsen ha tan 0,5 g bc N,N diethyldithylocarbamat n
va 100ml bo qun dung dch ny trong l thy tinh mu nt nhm ch mt
3.3 Bnh phn ng


A. Bnh phn ng (dung tch n vai ca n khong 70ml)
B. ng dn hi
C. ng thy tinh (ung knh trong 5,6 mm); ung knh trong ca u chui ca
phn cm vo ng hp th l 1mm.
D. ng hp th (ung knh trong 10mm)
E. Mt l nh trn ng B
F. Bng thy tinh ( khong 0,2 g)
G. Vch chia 5ml trn ng hp th
H v J nt thy tinh
L. Vch chia 40ml trn bnh A

3.4 Tin hnh
- Php th uc tin hnh trn thit b uc m t nh trn, cho mt t bng thy
tinh vo ng dm hi B n cao khong 30ml. sau khi lm m nuf bng hn
hp ng th tch ca thuc th ch acetat v nuc, ndng mt lc ht nh rloi
b git cht lng tha. napws ng n hi thangwr ng qua tm ca nt tcao su H
vo bnh phn ng A sao cho l nh E va pha dui ca nt cao su. np cht
nt cao su J vo ming ng B. np ng thy tinh C thng ng qua nt J. Np ng
dn hi C qua nt cao su J.
- Rt dung dch th vo bnh phn ng v thm mt git thuc th bromophenol
blue, sau trung ha bng dung dch amoniac hoc thuc th amoniac. Nu dung
dch ngm thi l nc th c th b qua bc trung ha. Thm vo dung dch ny
5 ml acid clohydric (1/2) v 5 ml kali iodid. i 2-3 pht, thm 5 ml thic(II) clorid v
10 pht nhit phng. Thm nc n 40ml, thm 2 g km (loi dng
th arsen) v ngay lp tc ng nt cao su ni ng thot kh v ng thy tinh. a
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mi hp ca ng thy tinh gn chm y ng hp th, trong ng hp th cha
sn 5 ml dung dch hp th arsen.
Tip theo, t bnh phn ng trong nc ngp n vai bnh 25C v li trong 1
gi. Tho ng hp th v nu cn thit, thm pyridin n 5 ml. Dung dch hp
th ca dung dch th khng c xut hin m mu hn so vi cc mu dung
dch hp th ca dung dch chun.
xc nh mu chun, thc hin cc bc tng t vi dung dich chun nh i
vi dung dch th. t cng mt lng dung dch thi nhim nh vi dung dch th
v 2,0 ml dung dch arsen chun vo bnh phn ng. Mu sc biu hin bi dung
dch hp th l mu chun.

4. Xc nh hm lng Phenol
4.1 Chun b dung dch phenol chun
- Dung dch chun phenol gc: Cn chnh xc 1,0 g phenol, ha tan trong 100 ml
nc.
- Dung dch chun trung gian: Ly chnh xc 1 ml dung dch chun gc vo bnh
nh mc v thm nc ct n 100 ml.
- Dung dch chun lm vic: Ly chnh xc 1 ml dung dch chun trung gian thm
nc ct n 20 ml. Dung dch chun lm vic c nng 5 g/ml.
4.2 Chun b dung dch m acid boric:
Chun b 2 dung dch
Dung dch s 1: Ho tan 4,0 g NaOH trong nc, thm nc nh mc n
100 ml.
Dung dch s 2: Ha tan 6,2 g acid boric trong nc, thm nc nh mc n
100 ml.
Ly mi dung dch mt lng bng nhau ri lc u
4.3 Tin hnh:
Ly chnh xc 20 ml dung dch th, thm 3 ml dung dch m acid boric v trn u,
sau thm 5 ml dung dch antipyrin 4-amin v 2,5 ml dung dch fericyanid v nc
100 ml. Trn u v yn trong 10 pht nhit phng.
Tin hnh tng t vi 20 ml dung dch chun lm vic thay cho 20 ml dung dch
th. o hp th quang ca 2 hn hp bc sng 510 nm ; hp th quang
ca mu th khng c ln hn hp th quang ca mu chun.

5. Formaldehyd
5.1 Tin hnh
Cho vo ng ong c chia vch 200 ml mt lng 10 ml dung dch mu vi 1 ml
acid phosphoric 20%, sau thm 5-10 ml nc v tin hnh ct ko hi nc vi
ng sinh hn ngp trong nc. Khi chng ct c khong 190 ml th ngng v
thm nc nh mc 200 ml. Ly 5 ml dung dch ny cho vo ng nghim c
ng knh 15 mm v thm 5 ml thuc th acetylaceton. Khuy u v gia nhit
cch thy trn b nc si trong 10 pht.
- Dung dch so snh: Mt ng nghim c ng knh 15 mm khc, cho vo 5 ml
nc v 5 ml thuc th acetylaceton. Khuy u v gia nhit cch thy trn b
nc si trong 10 pht. Quan st cc ng nghim trn nn trng dung dch mu th
pho khng ti mu hn dung dch so snh.
6. Cn kh
6.1 Tin hnh:
9
- Ly 200-300 ml dung dch th (nu s dng heptan l dung dch ngm thi, th
chuyn 200-300 ml dung dch th vo mt bnh hnh qu l, c chn khng n cn
mt vi ml, chuyn phn dch c vo mt chn bch kim, thch anh, hoc cc thy
tinh chu nhit ( gia nhit ti 105
0
C v cn b) sau trng bnh ct hai ln, mi
ln vi khong 5 ml heptan v gp dch ra vo dch c c. Cho bay hi trn b
cch thy n khi bc hi ht dung dch v cn li cn cng. Sy kh cn trong 2
gi 105
0
C, ngui trong bnh ht m, cn chn v cn xc nh khi lng cn
(s chnh lch khi lng chn v cn vi khi lng b).
- Tin hnh ng thi mu trng, trong thay th tch dung dch th bng th tch
nc ct tng ng.
- S dng cng thc sau tnh lng cn:
Cn kh (g/ml) = [(a-b) x1.000] / th tch dung dch th (ml)
Trong :
a (mg) = s chnh lch khi lng gia chn c cn v b trong th nghim vi
dung dch th.
b (mg) = s chnh lch khi lng gia chn c cn v b trong th nghim vi
mu trng
Ngoi ra, nu dng nc lm dung dch ngm thi m lng cn kh ln hn 30
g/ml th kt qu phi theo phng php th sau y:
- Thm 30 ml cloroform vo phn cn kh thu c, gia nhit, lc v sau cn
cht lng thu c sau lc trong mt chn thch anh, bch kim, hoc thy tinh chu
nhit bit khi lng. Hn na, ra cn kh va lc hai ln, s dng 10 ml
chloroform mi ln, gia nhit, lc, a cht lng c lc vo b bay hi cch thy.
Sau khi lm ngui, cn chn v cn xc nh khi lng cn (s chnh lch khi
lng chn v cn vi khi lng b). Tin hnh ng thi mu trng, trong thay
th tch dung dch th bng th tch nc ct tng ng.
- S dng cng thc sau tnh lng cht tan trong chloroform
Lng cht tan trong chloroform (g/ml) = [(a-b) x1,000] / th tch dung dch th
ban u(ml)
b (mg) = mu trng
7. Epiclorohydrin
7.1 Chun b dung dch epichlorohydrin chun
- Ha tan 100 mg epichlorohydrin trong pentan, thm pentan nh mc n 100
ml, ly 1 ml dung dch ny v thm pentan nh mc n 100 ml. Sau ly 5 ml
dung dch ny v thm pentan nh mc n 100 ml. Dung dch epichlorohydrin
chun c nng 0,5 g/ml.
7.2 Tin hnh
- Ly 5 l mi loi, dung dch mu v dung dch chun epichlorohydrin. Chy sc k
kh theo hng dn c m t di y.

Ct sc k S dng ct bng thy tinh silicat di 30 m ng
knh trong 0,53 mm c ph mt lp dy 1 m
polyethelyne
Nhit ct un nng ct n 80 C trong 1 pht, sau tng
nhit t t, c 10C mi pht cho n khi t
250C, duy tr trong 10 pht.
Nhit bung tim mu
200
0
C
10
Thit b o S dng detector ion ha ngn la hydro. Vn hnh
nhit khong 220
0
C. iu chnh lu lng ca
khng kh v hydro sao cho nhy pht hin ti a

Kh mang S dng kh nit hoc heli. iu chnh tc dng
kh epichlorohydrin xut hin trong khong 7 pht

8. Vinyl chlorid
8.1 Chun b dung dch vinyl chlorid chun
- Ly khong 190 ml ethanol vo bnh nh mc 200 ml, y bnh bng nt cao su
silicon v cn khi lng. Lm lnh bnh nh mc bng methanol bng kh v tim
vo 200 mg vinyl clorid c ho lng. Tim ethanol c lm lnh bng
methanol bng kh vo bnh, nh mc n 200 ml. Tip tc lm lnh bnh bng
methanol bng kh. Ly 1 ml dung dch trn, v thm ethanol c lm lnh bng
methanol bng kh, nh mc n 100 ml v bo qun trong methanol bng kh.
Dung dch thu c c nng 10 g/ ml. Ethanol (99,5) dng trong th nghim
khng c cha nhng cht c nh hng n cc cht dng trong php th.
8.2 Tin hnh
- Rt 50 l dung dch chun vinyl clorua vo bnh thy tinh c nt y c 2,5 ml
N, N dimethylacetamid, v y np ngay. Lm tng t vi mu th. Sau , un
nng bnh cha dung dch mu v bnh cha dung dch chun trong 1 gi, duy tr
nhit 90C, thnh thong lc u bnh. Tip theo, ly 0,5 ml hi trong mi bnh,
chy sc k kh theo hng dn c m t di y, sau so snh thi gian lu
ca pc trong sc k ca dung dch th v dung dch chun Vinyl chlorid.

Ct sc k S dng ct bng thy tinh silicat di 25 m ng
knh 0,25 mm c ph mt lp dy 3 m nha xp
divinylbenzene styrene
Nhit ct un nng ct n 80 C trong 1 pht, sau tng
nhit t t, c 10C mi pht cho n khi t
250C, duy tr trong 10 pht.
Nhit bung tim dch
th
2000C
Detector S dng detector ion ha bng ngn la hydro. Vn
hnh nhit khong 250C. iu chnh lu lng
ca khng kh v hydro sao cho nhy pht hin
ti a
Kh mang S dng kh nit hoc heli. iu chnh tc dng
kh vinyl chlorid xut hin trong khong 5 pht

Din tch pc vinyl clorid ca mu th khng c ln hn din tch pc vinyl clorid
ca dung dch chun