CNG HO X HI CH NGHA VIT NAM

QCVN 12-1 : 2011/BYT

QUY CHUN K THUT QUC GIA

V AN TON V SINH I VI BAO B, DNG C BNG NHA TNG HP
TIP XC TRC TIP VI THC PHM
National technical regulation on safety and hygiene for synthetic resin Implement,
container and packaging in direct contact with foods

H NI 2011

Li ni u
QCVN 12-1:2011/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.

QUY CHUN K THUT QUC GIA

V V SINH AN TON I VI BAO B, DNG C BNG NHA TNG HP TIP XC TRC
TIP VI THC PHM
National technical regulation on safety and hygiene for synthetic resin implement, container
and packaging 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 nha tng hp tip xc trc tip vi thc
phm (sau y gi tt l bao b, dng c nha).
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 nha.
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 dch dng ngm mu th.
II. YU CU K THUT
1. Yu cu k thut i vi bao b, dng c nha
Cc bao b, dng c nha phi t cc yu cu chung quy nh ti bng 1:
Bng 1. Yu cu chung i vi bao b, dng c nha
Th vt liu
Ch tiu kim
tra

Th thi nhim

Gii hn ti
a

Ch tiu kim
tra

iu kin
ngm thi

Kim loi nng

Ch
Cadmi

100 g/g
100 g/g

Dung dch
ngm thi

Gii hn
ti a

Acid acetic
4%

1 g/ml

60 C trong
Lng KMnO4
[1]
s dng

30 pht

10 g/ml

[7]

Nc

2. Yu cu k thut i vi bao b, dng c t nha Phenol, Melamin v Ure

Ngoi cc yu cu k thut quy nh ti khon II, mc 1, cc bao b, dng c t nha Phenol,
Melamin v Ure phi t cc yu cu quy nh ti bng 2:
Bng 2: Yu cu i vi bao b, dng c t nha Phenol, Melamin v Ure
Th thi nhim
Ch tiu kim tra
Phenol
Formaldehyd
Cn kh

iu kin ngm thi

[7]

60 C trong 30 pht
o

25 C trong 1 gi

Dung dch ngm thi

Nc
Heptan

Gii hn ti a
5 g/ml
m tnh
30 g/ml

60 C trong 30 pht
0

Ethanol 20%

[4]

Nc

[7]

60 C trong 30 pht

Acid acetic 4%

3. Yu cu k thut i vi bao b, dng c t nha Formaldehyd

Ngoi cc yu cu k thut quy nh ti khon II, mc 1, cc bao b, dng c t nha Formaldehyd
phi t cc yu cu quy nh ti bng 3:
Bng 3: Yu cu i vi bao b, dng c t nha Formaldehyd
Th thi nhim
Ch tiu kim tra

Dung dch ngm

thi

iu kin ngm thi

Gii hn ti a
m tnh

Phenol
Nc
Formaldehyd

m tnh

[7]

60 C trong 30 pht

Cn kh

30 g/ml

Acid acetic 4%

4. Yu cu k thut i vi bao b, dng c t nha Polyvinyl Clorid (PVC)

Ngoi cc yu cu k thut quy nh ti khon II, mc 1, cc bao b, dng c t nha Polyvinyl Clorid
(PVC) phi t cc yu cu quy nh ti bng 4:
Bng 4: Yu cu i vi bao b, dng c t nha Polyvinyl Clorid (PVC)
Th vt liu
Ch tiu kim
tra

Th thi nhim

Gii hn ti a

Vinyl clorid

Ch tiu kim
tra

1g/g

iu kin
ngm thi

Dung dch
ngm thi

Gii hn ti a
150 g/ml

25 C trong
1 gi

[3]

Heptan

30 g/ml
Cresyl
phosphat

1g/g

Cc hp cht
dibutyl thic

50/g

Cn kh

60 C trong
30 pht

Ethanol 20%
[4]

[5]

Nc

60 C trong
30 pht

Acid acetic
4%

5. Yu cu k thut i vi bao b, dng c t nha Polyethylen v Polypropylen (PE v PP)

Ngoi cc yu cu k thut quy nh ti khon II, mc 1, cc bao b, dng c t nha Polyethylen v
Polypropylen (PE v PP) phi t cc yu cu quy nh ti bng 5:
Bng 5: Yu cu i vi bao b, dng c t nha Polyethylen v Polypropylen (PE v PP)
Th thi nhim
Ch tiu kim tra

iu kin ngm thi

o

Heptan

Ethanol 20%

25 C trong 1 gi
Cn kh

Dung dch ngm thi

60 C trong 30 pht

[3]

Gii hn ti a
30 g/ml

[4]

[a]

30 g/ml

[5]

Nc

[7]

60 C trong 30 pht

[6]

Acid acetic 4%

6. Yu cu k thut i vi bao b, dng c t nha Polystyren (PS)

Ngoi cc yu cu k thut quy nh ti khon II, mc 1, cc bao b, dng c t nha Polystyren (PS)
phi t cc yu cu quy nh ti bng 6:
Bng 6: Yu cu i vi bao b, dng c t nha Polystyren (PS)
Th vt liu

Th thi nhim
Gii hn
ti a

Ch tiu kim tra

Tng s cht bay
hi(styren, tuluen,
ethybenzen, npropyl benzen)

Ch tiu kim
tra

iu kin
ngm thi

Dung dch
ngm thi

Gii hn
ti a

5mg/g

240 g/ml

25 C trong
1 gi

[3]

Heptan

Cn kh
Polylstyren trng
n(khi dng nc
si)

2mg/g

60 C trong
30 pht

[4]

30 g/ml

[5]

Styren v
Ethybenzen

Ethanol 20%

60 C trong
[7]
30 pht

1mg/g

Nc

Acid acetic
[6]
4%

7. Yu cu k thut i vi bao b, dng c t nha Polyvinyliden Clorid (PVDC)

Ngoi cc yu cu k thut quy nh ti khon II, mc 1, cc bao b, dng c t nha Polyvinylden
Clorid (PVDC) phi t cc yu cu quy nh ti bng 7:
Bng 7: Yu cu i vi bao b, dng c t nha Polyvinyliden Clorid (PVDC)
Th vt liu
Ch tiu kim
tra

Gii hn ti a

Th thi nhim
Ch tiu
kim tra

iu kin
ngm thi

Dung dch
ngm thi

Bari

100 g/g

25 C trong 1
gi

Vinyliden
Clorid

Khng qu 6
g/g

60 C trong 30
pht

30 g/ml

[3]

Heptan

Cn kh

Gii hn
ti a

Ethanol 20%

[4]

[5]

60 C trong 30
[7]
pht

Nc

[6]

Acid acetic 4%

8. Yu cu k thut i vi bao b, dng c t nha Polyethylen terephthalat (PET)

Ngoi cc yu cu k thut quy nh ti khon II, mc 1, cc bao b, dng c t nha Polyethylen
terephthalat (PET) phi t cc yu cu quy nh ti bng 8:
Bng 8: Yu cu i vi bao b, dng c t nha Polyethylen terephthalat (PET)
Th thi nhim
Ch tiu kim tra

iu kin ngm thi

Dung dch ngm thi

Gii hn ti a

Antimony
Germani

[7]

60 C trong 30 pht
o

0,1 g/ml

[3]

25 C trong 1 gi

Heptan

Cn kh

0,05 g/ml
Acid acetic 4%

60 C trong 30 pht

30 g/ml

Ethanol 20%

[4]

[5]

[7]

60 C trong 30 pht

Nc

[6]

Acid acetic 4%

9. Yu cu k thut i vi bao b, dng c t nha Polymethyl Metacrylat (PMMA)

Ngoi cc yu cu k thut quy nh ti khon II, mc 1, cc bao b, dng c t nha Polymethyl
Metacrylat (PMMA) phi t cc yu cu quy nh ti bng 9:
Bng 9: Yu cu i vi bao b, dng c t nha Polymethyl Metacrylat (PMMA)
Th thi nhim
Ch tiu kim tra
Methyl methacrylat

iu kin ngm thi

0

60 C trong 30 pht
o

Dung dch ngm thi

Gii hn ti a

Ethanol 20%

15 g/ml

[3]

25 C trong 1 gi

Heptan

60 C trong 30 pht
Cn kh

30 g/ml

Ethanol 20%

[4]

[5]

Nc
0

[7]

60 C trong 30 pht

[6]

Acid acetic 4%

10. Yu cu k thut i vi bao b, dng c t nha Nylon (PA)

Ngoi cc yu cu k thut quy nh ti khon II, mc 1, cc bao b, dng c t nha Nylon phi t
cc yu cu quy nh ti bng 10:
Bng 10: Yu cu i vi bao b, dng c t nha Nylon (PA)
Th thi nhim
Ch tiu kim tra
Caprolactam

iu kin ngm thi

0

60 C trong 30 pht

Gii hn ti a

Ethanol 20%

15 g/ml

[3]

Heptan

Ethanol 20%

25 C trong 1 gi
Cn kh

Dung dch ngm thi

60 C trong 30 pht

30 g/ml
[4]

[5]

[7]

60 C trong 30 pht

Nc

[6]

Acid acetic 4%

11. Yu cu k thut i vi bao b, dng c t nha Polymethyl Penten (PMP)

Ngoi cc yu cu k thut quy nh ti khon II, mc 1, cc bao b, dng c t nha Polymethyl
Penten (PMP) phi t cc yu cu quy nh ti bng 11:
Bng 11: Yu cu i vi bao b, dng c t nha Polymethyl Penten (PMP)
Th thi nhim
Ch tiu kim tra

iu kin ngm thi

o

Cn kh

25 C trong 1 gi
0

60 C trong 30 pht

Dung dch ngm

thi
[3]

Heptan

Ethanol 20%

Gii hn ti a
120 g/ml

[4]

30 g/m l

[5]

Nc
0

[7]

60 C trong 30 pht

[6]

Acid acetic 4%

12. Yu cu k thut i vi bao b, dng c t nha Polycarbonat (PC)

Ngoi cc yu cu k thut quy nh ti khon II, mc 1, cc bao b, dng c t nha Polycarbonat
phi t cc yu cu quy nh ti bng 12:
Bng 12: Yu cu i vi bao b, dng c t nha Polycarbonat (PC)
Th vt liu
Ch tiu kim
tra
Bis-phenol A
(Phenol,P-t[8]
butylphenol)

Th thi nhim

Gii hn
ti a

Ch tiu
kim tra

iu kin
ngm thi

Dung dch ngm

thi

Khng qu
500g/g

25 C trong 1
gi
0

Bisphenol A
(Phenol,P-tbutylphenol)

2,5 g/ml

[3]

Heptan

60 C trong 30
pht

Ethanol 20%

Gii hn
ti a

[4]

[5]

Nc
0

Diphenyl
carbonat

60 C trong 30
[7]
pht

Khng qu
500g/g

[6]

Acid acetic 4%

25 C trong 1
gi
0

Cn kh
Amin(triethylam
in v
tributylamin)

30 g/ml

[3]

Heptan

60 C trong 30
pht

Ethanol 20%

[4]

[5]

Nc
0

60 C trong 30
[7]
pht

Khng qu
1g/g

[6]

Acid acetic 4%

13. Yu cu k thut i vi bao b, dng c t nha Polylactic Acid (PLA)

Ngoi cc yu cu k thut quy nh ti khon II, mc 1, cc bao b, dng c t nha Polylactic Acid
(PLA) phi t cc yu cu quy nh ti bng 13:
Bng 13: Yu cu i vi bao b, dng c t nha Polylactic Acid (PLA)
Th thi nhim
Ch tiu kim tra
Acid lactic tng s

iu kin ngm thi

Dung dch ngm thi

Gii hn ti a

Nc

30 g/ml

Heptan

60 C trong 30 pht

[3]

25 C trong 1 gi
0

60 C trong 30 pht
Cn kh

Ethanol 20%

30 g/ml
[4]

[5]

Nc
0

[7]

60 C trong 30 pht

[6]

Acid acetic 4%

14. Yu cu k thut i vi bao b, dng c t nha Polyvinyl Alcol (PVA)

Ngoi cc yu cu k thut quy nh ti khon II, mc 1, cc bao b, dng c t nha Polyvinyl Acol
(PVA) phi t cc yu cu quy nh ti bng 14:
Bng 14: Yu cu i vi bao b, dng c t nha Polyvinyl Alcol (PVA)

Th thi nhim
Ch tiu kim tra

iu kin ngm thi

Dung dch ngm thi

Heptan

[3]

Ethanol 20%

25 C trong 1 gi
Cn kh

60 C trong 30 pht

Gii hn ti a
30 g/ml

[4]

[5]

[7]

60 C trong 30 pht

Nc

[6]

Acid acetic 4%

Ghi ch
[1]

Ngoi tr bao b, dng c c thnh phn chnh l nha Phenol, nha Melamin v nha
Ure.
[2]

p dng vi dng c nu n, b n ung.

[3]

p dng vi bao b, dng c cha ng cht bo, du n v thc phm cha cht bo.

[4]

p dng vi bao b, dng c cha ng ung c cn.

[5]

p dng vi bao b, dng c cha ng thc phm c pH ln hn 5.

[6]

p dng vi bao b, dng c cha ng thc phm c pH nh hn hoc bng 5.

[7]

p dng vi dng c s dng nhit ln hn 100 C v iu kin ngm l 95 C trong

30 pht.
[8]

Khng c trong bao b, dng c nha dnh cho tr nh.

III. PHNG PHP TH V LY MU

Phng php th v ly mu c quy nh ti cc ph lc ban hnh km theo quy chun ny
nh sau:
1. Ph lc 1: Phng php th i vi vt liu.
2. Ph lc 2: Phng php th thi nhim.
IV. YU CU QUN L
1. Cng b hp quy
1.1 Cc sn phm l bao b, dng c nha 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 nha
Vic kim tra nh nc i vi cc sn phm bao b, dng c nha 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 cc sn phm bao b, dng c nha phi cng b hp quy
ph hp vi cc quy nh k thut ti 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
nha 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.

PH LC 1
PHNG PHP TH I VI VT LIU NHA
1. Xc nh Ch v Cadmi trong vt liu nha
1.1 Chun b dung dch th
Cn 1,0 g mu (chnh xc n mg) cho vo a bay hi bng bch kim, thch anh hoc thy tinh chu
nhit, thm 2ml acid sulfuric, gia nhit t t cho n khi ht khi trng bay ra t acid sulfuric v phn
ln mu b than ha. Sau , cho a vo nung trong l in ti 450C qu trnh than ha xy ra
hon ton, lp li qu trnh thm acid sulfuric v nung i vi cn trn a, ngui. Thm vo cn
5ml acid hydrocloric (12), trn u, v cho bay hi trn b cch thy. Sau khi ngui, thm 20 ml
acid nitric 0,1 mol/l, ha tan, lc v loi b phn khng tan, thu phn dch lc lm dung dch th.
1.2 Chun b dung dch chun
1.2.1

Cadmi

- Dung dch chun Cadmi 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 chun Cadmi lm vic: Ly chnh xc 1 ml dung dch chun cadmi gc, thm acid nitric
0,1 mol/l n 200 ml. Dung dch chun lm vic ny c nng 5 g/ml.
1.2.2

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 1 ml dung dch chun ch gc, thm acid nitric 0,1 mol/l
nh mc n 200 ml. Dung dch chun lm vic ny c nng 5 g/ml.
1.3 Tin hnh
Dng quang ph hp th nguyn t hoc quang ph pht x plasma xc nh cadmi v ch trong
dung dch th.
2. Xc nh cc hp cht dibutyl thic
2.1 Chun b dung dch th
Cn 0,5g mu ( c ct hoc nghin nh) cho vo bnh thy tinh c mi. Thm 20ml hn hp
aceton v hexan t l 3:7 v mt git acid hydrochloric, y cht np bnh v qua m khong
0
40 C, thnh thong lc trn u. Sau khi lm ngui, lc ly dch, thu dch lc v dch ra, c n
0
khong 1ml trn my c quay chn khng nhit khng qu 40 C. Sau , dng hexan chuyn
vo bnh nh mc 25ml, thm hexan n 25 ml. Ly tm hn hp trong khong 10 pht vi tc
2500 vng/pht v s dng lp trn lm dung dch th. Thm aceton v 2-3 git acid hydrocloric vo
100ml dibutyl thic diclorid v ha tan, sau thm aceton n va 100ml. Ly 1ml dung dch ny,
thm hexan v 2-3 git acid hydrocloric n va 1000ml, dung dch chun dibutyl thic c nng
1 g/ml.
2.2 Tin hnh
Ly 2ml mi loi dung dich th v dung dch chun dibutyltin, thm 5 ml dung dch m acid aceticnatri acetat v 1 ml thuc th natri tetraethylborate, sau ng nt ngay lp tc v lc mnh trong
20 pht. yn hn hp trong khong 1 gi nhit phng, v loi b lp hexan. Dng 1l dung
dch ny, chy sc k kh v khi ph theo hng dn di y.
Ct sc k

S dng ct bng thy tinh silicat di 30 m ng knh trong 0,25 mm

c ph mt lp dy 0,25 m dimethylpolysiloxan cha
diphenylpolysiloxan 5%

Nhit ct

Lm nng ct n 45C trong 4 pht, sau tng tc gia nhit

15C/pht cho n khi t 300C ,duy tr nhit ny trong 10 pht.

Nhit
tim mu
Detector

bung

250 C
Dng Detector khi ph ci t s khi l 263

Kh mang

S dng kh Heli.iu chnh tc dng kh dibutyltin xut hin thi

im khong 13 pht.

3. Xc nh Tricresyl phosphat trong nha PVC

3.1 Chun b dung dch th
Cn 0,5g mu ( c ct hoc nghin nh) v cho vo bnh thy tinh c nt mi. Thm 15ml
0
acetonitril, y cht nt bnh v qua m khong 40 C. Sau , lc ly dch, thu dch lc v dch
ra, thm acetonitril n 25 ml v s dng dch ny l dch chit acetonitril.
Ly ct mini nhi sn silica gel c octadecyl silyl ha, luyn ct bng 5ml acetonitril v 5ml hn
hp acetonitril : nc (1 :1)
Ly 5ml dch chit acetonitril v 5ml nc trn u v np vo u ct luyn trn.
Ra gii bng hn hp acetonitril:nc t l 2:1 v thu ly 10ml dch ra gii l dung dch th.
3.2 Chun b dung dch chun
Cn chnh xc 100 mg tricresyl phosphat, thm acetonitril ha tan v nh mc n 100 ml. Ly 1
ml dung dch vi 60 ml acetonitril, sau thm nc v nh mc n 100 ml. Dung dch chun
tricresyl phosphate c nng 10 g/ ml.
3.3 Tin hnh
Ly 20 l mi loi, dung dch th v dung dch chun tricresyl phosphat. Chy sc k lng theo iu
kin di y.
Ct sc k

Ct thp khng g di 250mm c ng knh 4,6 mm

Nhit ct

50 C

Detector

Detector quang ph t ngoi, hot ng bc sng 264 nm.

Pha ng

Dng hn hp acetonitril v nc trn vi t l 2:1. iu chnh tc dng

chy tricresyl phosphat xut hin thi im khong 9 pht.

4. Xc nh Vinyl clorid trong nha PVC

4.1 Chun b dung dch th
Cn 0,5g mu c (ct mng) v cho vo bnh thy tinh dung tch 20ml c np kn. Sau , thm
2,5ml N,N-dimethyl acetamid v y np ngay, lc u c dung dch th. Tuy nhin, i vi cc
mu khng d dng ha tan th sau khi y np, cn lc k trn u nhit phng, qua m
v s dng lm dung dch th.
4.2 Dung dch vinyl clorid chun
Ly khong 190 ml Ethanol vo bnh nh mc 200 ml, y bnh bng nt cao su silicon v cn trng
lng. Lm lnh bnh nh mc bng methanol bng kh v tim vo 200 mg vinyl clorua 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 vinyl clorid chun 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.
4.3 Tin hnh
Rt 50 l dung dch chun vinyl clorua vo bnh thy tinh c nt y c 2,5 ml N, N
dimethylacetamide, 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 iu kin di y.
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 divinylbenzen styren

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 C

Detector

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 cc

vinyl chloride xut hin thi im khong 5 pht

5. Xc nh cc cht bay hi trong nha PS

5.1 Chun b dung dch th
Cn chnh xc khong 0,5g mu, cho vo bnh nh mc 20ml v thm mt lng thch hp
tetrahydrofuran. Sau khi ha tan ht mu, thm 1ml dung dch th diethylbenzen v thm
tetrahydrofuran nh mc cho 20 ml.
5.2 Chun b dung dch chun
Cho 90 ml dung dch tetrahydrofuran vo bnh nh mc 100 ml. Cn chnh xc 50 mg mi loi cc
cht sau : styren, toluen, ethylbenzen, isopropyl benzen, v propyl benzen. Sau thm
tetrahydrofuran nh mc n 100 ml. Ly 1 ml, 2 ml, 3 ml, 4 ml, v 5 ml dung dch trn ln lt
cho vo cc bnh nh mc 20 ml ring bit v thm vo mi bnh 1 ml dung dch th diethylbenzen,
sau thm dung dch tetrahydrofuran nh mc n 20 ml.
5.3 Dung dch th diethylbenzen
Cho tetrahydrofuran vo 1 ml diethylbenzen, nh mc n 100 ml. Ly 10 ml dung dch ny v
thm tetrahydrofuran tip tc nh mc n 100 ml.
5.4 Xy dng ng chun
Ly 1 l mi dung dch chun, chy sc k kh theo hng dn m t di y. S dng sc k
thu c tnh cc t l din tch pic ca styren, toluen, Ethylbenzen, isopropyl benzen v propyl
benzen vi din tch pic ca diethylbenzen, sau v ng chun.
Ct sc k

S dng ct bng thy tinh silicat di 30 m ng knh 0,5 mm

c ph mt lp dy 0,5 m polyethylen glycol

Nhit ct

un nng ct t 60 C sau tng nhit t t, c 4C mi

o
pht cho n khi t 100C, v tip tc tng 10 C mi pht cho
o
n khi t 150 C

Nhit bung tim mu

220 C

Detector

Detector ion ha bng ngn la hydro. Vn hnh nhit

khong 220C. 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 cc

diethylbenzen xut hin thi im khong 11 pht

5.5 Tin hnh

Dng 1 ml dung dch th, chy sc k kh theo hng dn m t nh trn. S dng sc k thu
c tnh cc t l din tch pic ca cc cht vi din tch pic ca diethylbenzen. Tip theo, s
dng cc ng chun tng ng xc nh nng styren, toluen, ethylbenzen, isopropyl benzen
v propyl benzen, sau s dng cc phng trnh sau y xc nh hm lng ca tng cht.
Hm lng (g/g) = Nng cht trong dung dch mu th (g/ml) 20 (ml) / khi lng mu th (g)
6. Xc nh bari trong nha PVDC
6.1 Chun b dung dch th
Cn 0,5g mu, cho vo chn nung bng platin, thch anh hoc thy tinh chu nhit; v c ha t t
0
0
trc tip trn ngn la khong 300 C, sau nung khong 450 C chuyn thnh tro. Thm
50ml dung dch acid nitric 0,1 mol/l vo cn v ha tan.
6.2 chun b dung dich bari chun
- Dung dch Bari chun gc: Ha tan 190,3 mg bari nitrat trong acid nitric 0,1 mol/l nh mc n
100 ml. Nng ca bari trong dung dch chun gc l 1 mg/ml.
- Dung dch Bari chun lm vic: Ly 1 ml dung dch bari chun gc v thm acid nitric 0,1 mol/l nh
mc n 1.000 ml. Nng ca bari trong dung dch chun lm vic l 1 g/ml.

6.3 Tin hnh

Phn tch Bari trong dung dch th bng quang ph hp th nguyn t hoc quang ph pht x
plasma
7. Xc nh vinyliden chloride trong nha PVDC
7.1 Chun b dung dch th
Ct nh mu, cn 0,5g v cho vo bnh thy tinh 20ml c np y. Sau , thm 2,5ml N,N-dimethyl
acetamide v ng np ngay.
7.2 Dung dch chun
Cho khong 98 ml dung dch N,N-dimethyl acetamid vo bnh nh mc 100 ml c nt cao su silicon.
Tim 250 ml vinyliden clorid vo bnh. Sau tim N,N-dimethyl acetamid qua nt cao su silicon nh
mc n 100 ml. Tip tc ly 1 ml dung dch ny v thm N, N-dimethyl acetamid nh mc n
50 ml. Nng ca Vinyliden Clorid trong dung dch chun lm vic l 60 g/ml. Dung dch vinyliden
Clorid chun lm vic c nng l 60 g/ml.
7.3 Tin hnh
Rt 50 l dung dch vinyliden clorua chun vo mt chai thy tinh c nt y cha 2,5 ml dung dch
N,N-dimethylacetamide, 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 iu kin di y.
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 divinylbenzen styren

Nhit ct

Lm nng ct n 80 C trong 1 pht, tng nhit vi tc gia

nhit 10C/pht cho n khi t 250C, duy tr trong 10 pht.

Nhit bung tim

mu

200 C

Detector

Detector ion ha 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 vinyliden

clorid xut hin thi im khong 9 pht

8. Xc nh bisphenol A trong nha PC

8.1 Chun b dung dch th
Ly 1.0 g mu, cho vo bnh nn 200ml v thm 20 ml dicloromethan. Sau khi mu ha tan hon
ton, thm 100 ml aceton bng dng c nh git, va thm va lc k, ly tm hn hp trong 10 pht
vi tc 3000 vng/pht, c lp trn n khong 2ml bng my c quay chn khng. Sau , thm
10ml acetonitril v thm nc n 20ml. Ly 1ml dch ny v lc qua mng lc vi ng knh l lc
khng ln hn 0,5 m.
8.2 Chun b dung dch chun
Cn chnh xc 10 mg mi loi cc cht sau : bisphenol A, phenol, v p-tert-butylphenol vo mt bnh
nh mc 100 ml, sau thm methanol nh mc n 100 ml. Ly 1 ml, 2 ml, 3 ml, 4 ml, v 5 ml
dung dch trn ln lt cho vo cc bnh nh mc 20 ml ring bit v thm nc n 20 ml. y
l nhng dung dch chun (5 g / ml, 10 g / ml, 15 g / ml, 20 g / ml, v 25 g / ml).
8.3 V ng chun
S dng 20 l cc dung dch chun, chy sc k lng theo iu kin di y. S dng sc k thu
c tnh ton chiu cao v din tch cc pic ca bisphenol A, phenol, v p-tert-butylphenol, sau
v ng chun cho tng cht.
Cht nhi

S dng gel silica octadecylsilyl

Ct sc k

S dng ct bng thp khng g di 250 mm c ng knh trong l 4,6

mm

Nhit ct

40 C

Detector

Detector quang ph ngoi. Vn hnh bc sng 217 nm

Pha ng

A = acetonitril ; B= nc ct

Chng
mi

trnh

dung

Gradient dung mi tuyn tnh vi t l A :B t 30 :70 n 100 :0 trong

thi gian 35 pht ; sau duy tr dung mi A thm 10 pht na

8.4 Tin hnh

S dng 20 l dung dch mu, chy sc k lng theo iu kin trn, dng ng chun xc nh
nng ca bisphenol A, phenol, v p-tert-butylphenol trong dung dch mu th, sau s dng
phng trnh i y tnh hm lng cc cht.
Hm lng (g/g) = Nng cc cht trong dung dch mu th (g/ml) 20 (ml) / khi lng mu th
(g)
9. Xc nh diphenyl carbonat trong nha PC
9.1 Chun b dung dich th
Ly 1,0 g mu, cho vo bnh nn 200ml v thm 20 ml diclometan. Sau khi mu ha tan hon ton,
thm 100 ml aceton bng dng c nh git, va thm va lc k, ly tm hn hp trong 10 pht vi tc
3000 vng/pht, c lp trn n khong 2ml bng my c quay chn khng. Sau , thm 10ml
acetonitril v thm nc n 20ml. Ly 1ml dch ny v lc qua mng lc vi ng knh l lc khng
ln hn 0,5 m.
9.2 Chun b dung dch chun
Cn chnh xc 10 mg diphenyl carbonat cho vo bnh nh mc 100 ml, v thm methanol n 100
ml. Ly 1 ml, 2 ml, 3 ml, 4 ml, v 5 ml dung dch trn ln lt cho vo cc bnh nh mc 20 ml ring
bit v thm nc n 20 ml.
9.3 Xy dng ng chun
S dng 20 l cc dung dch chun, chy sc k lng theo iu kin di y. S dng sc k thu
c tnh ton chiu cao v din tch pic ca diphenyl carbonat, sau v ng chun.
Cht nhi

S dng gel silica octadecylsilyl

Ct sc k

S dng ct bng thp khng g di 250 mm c ng knh trong l 4,6 mm

Nhit ct

40 C

Detector

S dng Detector quang ph t ngoi. Vn hnh bc sng 217 nm

Pha ng

A = acetonitril ; B= nc ct

Chng trnh
dung mi

Sau khi tin hnh gradien nng theot l A: B t (3:07) n (100:0) trong 35
pht, cho dng chy acetonitrile trong 10 pht.

9.4 Tin hnh

Dng 20 l dung dch th, chy sc k lng theo iu kin trn. S dng sc k tnh chiu
cao v din tch cc pc. Tip theo dng ng chun xc nh nng ca diphenyl carbonat
trong dung dch th, sau s dng phng trnh di y tnh hm lng cc cht ny:
Hm lng (g/g) = Nng trong dung dch mu th (g/ml) 20 (ml) / khi lng mu th (g)
10. Xc nh cc Amin trong nha PC
10.1 Chun b dung dch th
Ly 1,0 g mu, cho vo bnh nn 200ml v thm 20 ml dicloromethan. Sau khi mu ha tan hon
ton, thm 100 ml aceton bng dng c nh git, va thm va lc k, ly tm hn hp trong 10 pht
vi tc 3000 vng/pht, c lp trn n khong 2ml bng my c quay chn khng. S dng dch
ny lm dung dch th (ch p dng vi triethylamin v tributylamin)
10.2 Chun b dung dch chun
Cn chnh xc cc cht triethylamin v tributylamin 10 mg mi loi. Cho vo bnh nh mc 100 ml,
sau thm dichloroethan nh mc n 100 ml. Tip theo, ly ra 4 ml dung dch ny vo bnh
nh mc 100 ml, v thm dichloroethan n 100 ml. Ly 1 ml, 2 ml, 3 ml, 4 ml, v 5 ml dung dch
trn ln lt cho vo cc bnh nh mc 20 ml ring bit v thm nc nh mc n 20 ml. y l
nhng dung dch chun (0,2 g/ml, 0,4 /g ml, 0,6 /g ml, 0,8 g/ml, v 1,0 g/ml).

10.3 Xy dng ng chun

S dng 1l cc dung dch chun, chy sc k kh theo iu kin di y. S dng sc k thu
uc tnh chiu cao v din tch cc pic ca triethylamin v tributylamin, sau v ng chun
cho tng cht.
Ct sc k

S dng ct thy tinh silicat di 30 m ng knh 0,32 mm c ph mt

lp dimethylpolysiloxan dy 5 m

Nhit ct

un nng ct n 150 C trong 5 pht, sau tng nhit t t, c

20C mi pht cho n khi t 250C.gi nhit ny trong 5 pht

Nhit bung tim

mu

200 C

Detector

Detector nhit ion ngn la kim hoc mt detector nit-phosphor

nhy cao. Vn hnh nhit gn 250C. iu chnh lu lng ca
khng kh v hydro sao cho nhy pht hin ti a

Kh mang

S dng kh heli. iu chnh tc dng kh triethylamin xut hin

thi im khong 3 n 4 pht

10.4 Tin hnh

Dng 1 ml dung dch th, thc hin sc k kh theo iu kin trn. S dng sc k thu uc
tnh ton chiu cao v din tch ca mi pic. Tip theo, s dng cc ng chun tng ng xc
nh nng triethylamin v tributylamin, sau s dng cc phng trnh sau y xc nh hm
lng ca tng cht:
Hm lng (g/g) = Nng cht trong dung dch mu th (g / ml) 20 (ml) / khi lng mu th
(g)

PH LC 2
PHNG PHP TH THI NHIM
1. Xc nh hm lng kim loi nng trong nha
10.1 Chun b dung dch th
2

Ra sch mu bng nc ct, ngm trong dung dch ngm thi theo t l 2ml /1cm mu
- S dng dung dch ngm v iu kin ngm : Theo hng dn trong phn quy nh k thut.
10.2 Chun b dung dch chun 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 1 ml dung dch chun ch gc, thm acid nitric 0,1 mol/l
nh mc n 100 ml. Dung dch chun lm vic ny c nng 10 g/ml.
10.3 Tin hnh:
ng th: Cho 20ml dung dch th vo ng Nessler, thm nc ct n 50ml.
ng so snh: Tin hnh ng thi vi 1 ng Nessler khc, cho 2ml dung dch chun ch, thm 20ml
dung dch acid acetic 4%, thm nc ct n 50ml.
Nh vo mi ng 2 git thuc th Natri sulfid, yn trong 5 pht, sau quan st c 2 ng trn nn
trng. Dung dch trong ng th khng uc thm mu hn dung dch trong ng so snh.
2. Xc nh lng KmnO4 tiu tn trong nha
2.1 Chun b dung dch th
2

- Ra sch mu bng nc ct, ngm thi mu trong dung dch theo t l 2ml/1cm mu.
- S dng dung dch ngm v iu kin ngm : Theo hng dn trong phn quy nh k thut.
2.2 Tin hnh
Cho 100 ml nc, 5 ml acid sulfuric (1 3), v 5ml dung dch KMnO4 0,002 mol/l. un si khong 5
pht, sau loi b dung dch v ra bnh bng nc. Cho vo bnh tam gic 100 ml dung dch

th, 5 ml acid sulfuric (1 3), v 10ml dung dch KMnO4 0,002 mol/l v un si trong 5 pht. Ngay
sau khi ngng lm nng, thm 10 ml dung dch natri oxalat 0,005 mol/l lm mt mu dung dch.
Chun vi dung dch KMnO4 0,002 mol/l cho n khi c mu pht bn. Tin hnh vi mu trng
v tnh lng kali permanganat tiu th bng cch s dng cng thc sau.
Lng KMnO4 tiu th (g/ml) = [(a b)x0,316xfx 1,000]/100
Trong
a = lng (ml) dung dch KMnO4 0,002 mol/l dng tin hnh vi mu th
b = lng (ml) dung dch KMnO4 0,002 mol/l dng tin hnh vi mu trng
f = h s hiu chnh ca dung dch KMnO4 0,002 mol/l
3. Xc nh phenol trong nha phenol, melamin v ure
3.1 Chun b dung dch th
2

Ra sch mu bng nc ct, ngm thi trong dung dch ngm theo t l 2ml/1cm mu
- S dng dung dch ngm v iu kin ngm : Theo hng dn trong phn quy nh k thut.
3.2 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 1ml dung dch chun trung gian vo bnh nh mc 20ml v
thm nuc n vch. Dung dch chun lm vic c nng 5 g/ml.
3.3 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
3.4 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 kali 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.
4. Xc nh formaldehyd trong nha
4.1 Chun b dung dch th
2

Ra sch mu bng nc ct, ngm thi mu trong dung dch ngm t l 2ml/1cm mu
S dng dung dch ngm v iu kin ngm : Theo hng dn trong phn quy nh k thut.
4.2 Tin hnh
Cho vo ng o c chia vch 200 ml mt lng 10 ml dung dch mu th 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 trong cch thy si 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 trong cch thy si 10 pht.
Quan st cc ng nghim trn nn trng, dung dch mu th phi khng ti mu hn dung dch so
snh.
5. Xc nh cn kh
5.1 Chun b dung dch th:

Ra sch cc mu bng nc ct, sau ngm mu trong dung dch ngm thi theo t l 2ml/cm2
mu.
S dng dung dch ngm v iu kin ngm : Theo hng dn trong phn quy nh k thut.
5.2 Tin hnh:
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
0
mt chn bch kim, thch anh, hoc cc thy tinh chu nhit ( gia nhit ti 105 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
0
105 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
6. Xc nh Antimon
6.1 Chun b dung dch th
2

Ra sch mu bng nc ct, ngm trong dung dch ngm theo t l 2ml /1cm mu
S dng dung dch ngm v iu kin ngm : Theo hng dn trong phn quy nh k thut.
6.2 Chun b dung dch chun gc Antimon
Cn chnh xc 1,874 g triclorua antimon v ha tan trong mt t acid hydrochloric (1 2), sau
thm acid clohydric (1 10) nh mc n 1.000 ml. Dung dch chun Antimon c nng 1
mg/ml.
Chun b dung dch Antimon chun lm vic : Ly 1 ml dung dch antimon chun gc, thm acid axetic
4% nh mc n 100 ml, ly 1 ml dung dch ny v thm acid axetic 4% nh mc n 200 ml.
Dung dch Antimon chun lm vic c nng 0,05 g/ml.
6.3 Tin hnh
Thc hin php phn tch antimon bng phng php quang ph hp th nguyn t hoc quang ph
pht x plasma vi dung dch th v dung dch Antimon chun lm vic, so snh kt qu vi nhau.
7. Xc nh Germani
7.1 Chun b dung dch th
2

Ra sch mu bng nc ct, ngm trong dung dch ngm theo t l 2ml/1cm mu.
- S dng dung dch ngm v iu kin ngm: Theo hng dn trong phn quy nh k thut.
7.2 Chun b dung dch chun
- Cn chnh xc 144 mg germani dioxyd cho vo mt chn nung bch kim, thm 1g Natri carbonat v
trn u. Gia nhit lm tan chy hn hp, sau lm lnh v thm nc ha tan. Trung ha dung
dch bng acid hydrochloric, thm 1 ml acid hydrochloric na v sau thm nc nh mc n
100 ml. Nng germani trong dung dch ny l 1 mg/ ml.
- Ly 1ml dung dch chun germani cho vo bnh nh mc 100ml thm dung dch acid acetic 4% cho
n vch. Ly 1ml dung dch ny pha long bng dung dch ac ace tic 4% n 100ml trong bnh nh
mc. Dung dch germani chun lm vic c nng 1 g/ml.
7.3 Tin hnh
Dng quang ph hp th nguyn t hoc quang ph pht x plasma xc nh Germani trong dung
dch th
8. Xc nh methyl methacrylat

8.1 Chun b dung dch th

2

Ra sch mu bng nc ct, ngm trong dung dch ngm thi theo t l 2ml /1cm mu
- S dng dung dch ngm v iu kin ngm : Theo hng dn trong phn quy nh k thut.
8.2 Dung dch chun c nng methyl methacrylat l 15 g/ml.
8.3 Tin hnh
S dng 1l dung dch th v 1l dung dch chun methyl methacrylat, chy sc k kh theo hng
dn m t di y.
Ct sc k

S dng ct bng thy tinh silicat di 30 m ng knh trong

0,32 mm c ph mt lp dimethylpolysiloxan dy 5 m

Nhit ct

un nng ct n 120C trong 1 pht, sau tng nhit t

t, c 5C mi pht cho n khi t 170C.

Nhit bung tim mu

200 C

Detector

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

methyl methacrylat xut hin thi im khong 4 n 5 pht

9. Caprolactam
9.1 Chun b dung dch th
2

Ra sch mu bng nc ct, ngm trong dung dch ngm thi theo t l 2ml /1cm mu
- S dng dung dch ngm v iu kin ngm : Theo hng dn trong phn quy nh k thut.
9.2 Chun b dung dch chun
Cn 1,5 g caprolactam v ha tan trong ethanol 20% nh mc n 1.000 ml. Tip tc ly 1 ml
dung dch ny v thm ethanol 20% nh mc n 100 ml. Dung dch chun c nng
caprolactam l 15 g/ml.
9.3 Tin hnh
S dng 1l dung dch th v 1l dung dch chun caprolactam, chy sc k kh theo hng dn m
t di y, sau so snh thi gian lu trong sc k ca dung dch th v thi gian lu ca
caprolactam trong sc k ca dung dch caprolactam chun.
Ct sc k

S dng ct bng thy tinh silicat di 30 m ng knh 0,32 mm

c ph mt lp dimethylpolysiloxan dy 5 m

Nhit ct

240 C.

Nhit bung tim mu

240 C

Detector

Detector ion ha bng ngn la hydro. Vn hnh nhit khong

240C. 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

caprolactam xut hin thi im khong 5 pht

o
0

10. Bisphenol A ( phenol v p-tert-butylphenol)

10.1 Chun b dung dch th
2

Ra k mu bng nc, s dng dung dch ngm vi t l 2ml/cm din tch b mt mu.
- S dng dung dch ngm v iu kin ngm : Theo hng dn trong phn quy nh k thut.
Chuyn 25 ml dch ny vo phu chit, thm 10 ml acetonitril, lc k trn u trong 5 pht, cho
n nh v chuyn lp acetonitril vo bnh nh mc 25ml. Thm 10ml acetonitril vo lp heptan, thc
hin qu trnh chit nh trn v ly lp acetonitril vo bnh nh mc trn. Sau , b sung acetonitril
n 25 ml.
10.2 Chun b dung dch chun

- Cn chnh xc 10 mg mi loi cc cht sau : bisphenol A, phenol, v p-tert-butylphenol vo mt bnh

nh mc 100 ml, sau thm methanol n 100 ml. Ly 1 ml, 2 ml, 3 ml, 4 ml, v 5 ml dung dch
trn ln lt cho vo cc bnh nh mc 20 ml ring bit v thm nc nh mc n 20 ml. y l
nhng dung dch chun (5 g / ml, 10 g / ml, 15 g / ml, 20 g / ml, v 25 g / ml).
- Chun b dung dch chun lm vic: ly 2 ml ca cc dung dch chun gc trn vo bnh nh mc
20 ml thm nc nh mc n 20 ml. Nng ca tng dung dch ny (0,5 g / ml, 1,0 g / ml,
1,5 g / ml, 2,0 g / ml, v 2,5 g / ml) .
10.3 V ng chun
S dng 100 l cc dung dch chun lm vic, chy sc k lng theo iu kin di y. S dng sc
k thu uc tnh chiu cao v din tch pc ca bisphenol A, phenol, v p-tert-butylphenol, sau
v ng chun cho tng cht.
Ct np

S dng gel silica octadecylsily

Ct sc k

S dng ct bng thp khng g di 250 mm c ng knh trong l 4,6 mm

Nhit ct

40 C

Detector

S dng detector quang ph t ngoi. Vn hnh bc sng 217 nm

Pha ng

A = acetonitril ; B= nuc ct

Chng trnh
dung mi

gradien dung mi tuyn tnh vi t l A:B t (30:70) n (100:0) trong thi gian
35 pht, sau duy tr dng dung mi A thm 10 pht na.

10.4 Tin hnh

S dng 20 l dung dch th, chy sc k lng theo iu kin trn. S dng sc k thu uc
tnh chiu cao v din tch cc pc. Tip theo dng ng chun xc nh nng ca bisphenol
A, phenol, v p-tert-butylphenol trong dung dch mu th, sau s dng cng thc di y tnh
hm lng cc cht:
Hm lng (g/g) = Nng cht trong dung dch mu th (g/ml) 20 (ml) / khi lng mu (g)
11. Tng Acid lactic
11.1 Chun b dung dch th
2

Ra sch cc mu bng nc ct, sau ngm mu trong dung dch ngm theo t l 2ml/cm mu.
- S dng dung dch ngm v iu kin ngm : Theo hng dn trong phn quy nh k thut.
11.2 Dung dch chun c nng acid lactic l 30 g/ml
11.3 Tin hnh
Ly 1 ml dung dch th v 1 ml dung dch acid lactic chun vo ct, thm vo mi ct 100 l natri
hydroxyd 0,2 mol/l, yn 60C trong 15 pht, thnh thong lc u. Sau lm ngui ct, thm
vo mi ct 100 l acid phosphoric 0,2 mol/l. S dng 100 l mi dung dch, chy sc k lng theo
iu kin di y.
Cht nhi ct

S dng gel silica octadecylsilyl

Ct sc k

S dng ct bng thp khng g di 250 mm c ng knh

trong l 4,6 mm

Nhit ct

40 C

Detector

Detector quang ph t ngoi. Vn hnh bc sng 210 nm

Pha ng

S dng dung dch acid phosphoric, acetonitril v nc vi t l

0,1:1:99. iu chnh tc dng chy acid lactic xut hin
thi im khong 5 pht

CNG HO X HI CH NGHA VIT NAM

QCVN 12-2 : 2011/BYT

QUY CHUN K THUT QUC GIA

V V SINH AN TON I VI BAO B, DNG C BNG CAO SU TIP XC
TRC TIP VI THC PHM
National technical regulation on safety and hygiene for ruber implements, container and
packaging in direct contact with foods

H NI - 2011

Li ni u
QCVN 12-2:2011/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.

QUY CHUN K THUT QUC GIA

V V SINH AN TON I VI BAO B, DNG C BNG CAO SU TIP XC TRC TIP VI
THC PHM
National technical regulation on safety and hygiene for Ruber Implements, Container and
Packaging 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 cao su tip xc trc tip vi thc phm
(sau y gi tt l bao b, dng c cao su).
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 cao su.
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 dch dng ngm mu th.
II. YU CU K THUT
1. Yu cu k thut i vi bao b, dng c cao su (khng dnh cho tr nh)
Cc bao b, dng c cao su phi t cc yu cu chung quy nh ti bng 1:
Bng 1. Yu cu chung i vi bao b, dng c cao su (khng dnh cho tr nh)
Th vt liu
Ch tiu kim
tra

Gii hn ti
a

Cadmi

100g/g

Ch

100g/g

Th thi nhim
Ch tiu kim
tra

iu kin
ngm thi

Dung dch
ngm thi

Phenol

5 g/ml
Nc

Formaldehyd
Km
2Mercaptoimidazolin (Cao
su cha Clor)

Gii hn ti
a

Kim loi nng

m tnh
0

60 C trong
[5]
30 pht

Acid acetic 4%

15 g/ml
1 g/ml

m tnh

Nc

[3] , [6]

Acid acetic
[4]
4%

Cn kh
0

60 C trong
30 pht

Ethanol 20%
[1] [2]

2. Yu cu k thut i vi bao b, dng c cao su (dnh cho tr nh)

Cc bao b, dng c cao su phi t cc yu cu chung quy nh ti bng 2:
Bng 2. Yu cu chung i vi bao b, dng c cao su (dnh cho tr nh)

60 g/ml

Th vt liu
Ch tiu kim
tra
Cadmi

Gii hn ti
a

Th thi nhim
Ch tiu kim
tra

iu kin
ngm thi

Dung dch
ngm thi

Gii hn ti
a

10g/g
Phenol

5 g/ml
Nc

Formaldehyd
Ch

10g/g

Km

m tnh

40 C trong
24 gi

1 g/ml

Kim loi nng

Acid acetic 4%

1 g/ml

Cn kh

Nc

40 g/ml

Ghi ch
[1]

p dng vi bao b, dng c cha ng cht bo, du n v thc phm cha cht bo.

[2]

p dng vi bao b, dng c cha ng ung c cn.

[3]

p dng vi bao b, dng c cha ng thc phm c pH ln hn 5.

[4]

p dng vi bao b, dng c cha ng thc phm c pH nh hn hoc bng 5.

[5]

p dng vi dng c s dng nhit ln hn 100 C iu kin ngm l 95 C trong 30 pht.

[6]

Gii hn i vi cc dng c.

III. PHNG PHP TH V LY MU

Phng php th v ly mu c quy nh ti cc ph lc ban hnh km theo Quy chun ny
nh sau:
1. Ph lc 1: Phng php th vt liu.
2. Ph lc 2: Phng php th thi nhim.
IV. YU CU QUN L
1. Cng b hp quy
1.1 Cc sn phm l bao b, dng c cao su 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 cao su
Vic kim tra nh nc i vi cc sn phm bao b, dng c cao su 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 cao su
phi cng b hp quy ph hp vi cc quy nh k thut ti 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 cao su 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.

PH LC 1
PHNG PHP TH VT LIU
1. Xc nh Ch v Cadmi
1.1 Chun b dung dch th:
Cn 1,0 g (chnh xc n mg) mu cho vo chn bay hi bng bch kim, thch anh hoc thy tinh
chu nhit, thm 2ml acid sulfuric, gia nhit t t cho n khi ht khi trng bay ra t acid sulfuric v
phn ln mu b than ha. Sau , cho chn vo nung trong l in ti 450C qu trnh than
ha xy ra hon ton, c th lp li qu trnh thm acid sulfuric v nung i vi cn trn chn,
ngui. Thm vo cn 5ml acid hydrocloric (1/2), trn u, v cho bay hi trn b cch thy. Sau khi
ngui, thm 20 ml acid nitric 0,1 mol/l, ha tan, lc v loi b phn khng tan, thu phn dch lc lm
dung dch th.
1.2 Chun b dung dch chun:
1.2.1 Cadmi
+ Dung dch chun Cadmi 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 chun Cadmi lm vic (loi khng dnh cho tr nh)
Ly chnh xc 1 ml dung dch chun cadmi gc, thm acid nitric 0,1 mol/l n 200 ml. Dung dch
chun lm vic ny c nng 5 g/ml.
+ Dung dch chun Cadmi lm vic (loi khng dnh cho tr nh)
Ly chnh xc 1 ml dung dch chun cadmi gc, thm acid nitric 0,1 mol/l n 200 ml. Tip tc ly
10 ml dung dch trn, thm acid nitric 0,1 mol/l nh mc n 100 ml. Dung dch chun lm vic ny
c nng cadmi 0.5 g/ml.
1.2.2 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 (loi khng dnh cho tr nh)
Ly chnh xc 1 ml dung dch chun ch gc, thm acid nitric 0,1 mol/l nh mc n 200 ml. Dung
dch chun lm vic ny c nng 5 g/ml.
+ Dung dch chun ch lm vic (loi khng khng dnh cho tr nh)
Ly chnh xc 1 ml dung dch chun ch gc, thm acid nitric 0,1 mol/l n 200 ml. Tip tc ly 10
ml dung dch trn, thm acid nitric 0,1 mol/l nh mc n 100 ml. Dung dch chun lm vic ny c
nng ch 0.5 g/ml.
1.3 Tin hnh
Dng quang ph hp th nguyn t hoc quang ph pht x plasma xc nh cadmi v ch trong
dung dch th.
2. Xc nh 2-mecaptoimidazolin
2.1 Chun b dung dch th
Ly 1,0 g mu cho vo ng giy lc hnh tr, v s dng h thng chit Soxhlet chit trong 8 gi
vi khong 45ml methanol. C c dch chit n khong 1 ml v s dng 10 l lm dung dch
th.
2.2 Chun b dung dch chun
Ly 200 mg mercaptoimidazolin-2 v ha tan trong methanol nh mc n 100 ml. Tip tc ly 1
ml dung dch ny v thm methanol nh mc n 100 ml. Dung dch chun c nng 2mercaptoimidazoline l 20 g/ml.

2.3 Chun b dung dch 2,6-dicloroquinon clorimid trong ethanol : Ha tan 100 mg 2,6-dichloroquinon
clorimid trong ethanol nh mc n 10 ml.
2.4 Tin hnh
- Tin hnh chy sc k lp mng i vi dung dch th v dung dch chun 2-mercaptoimidazolin, s
dng dung dch chun lm dung dch i chiu.
Dng hn hp ethyl acetat, benzen t l 5:1 ; hn hp ethyl acetat, methanol, dung dch amoniac v
nc t l 30:2:1:1 lm dung mi khai trin. Bn mng s dng silica gel lm cht hp ph v c
o
lm kh trong 1 gi 120 C.
Khi lp dung mi khai trin chy c khong 10cm th ngng trin khai v cho kh t nhin. Sau
o
, phun dung dch 2,6-dicloroquinon clorimid trong ethanol, sy kh 10 pht 120 C v quan st.

PH LC 2
PHNG PHP TH THI NHIM
1. Xc nh kim loi nng
1.1 Chun b dung dch th:
Ra sch mu bng nc ct, s dng dung dch ngm v iu kin theo hng dn phn quy nh
2
k thut theo t l 2ml /1cm mu (loi khng dnh cho tr nh) v t l 20ml/g (loi dnh cho tr nh)
1.2 Chun b dung dch chun 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 (loi khng dnh cho tr nh)
Ly chnh xc 1 ml dung dch chun ch gc, thm nc nh mc n 100 ml. Dung dch chun
lm vic ny c nng 10 g/ml.
+ Dung dch chun ch lm vic (loi dnh cho tr nh)
Ly chnh xc 1 ml dung dch chun ch gc, thm acid nitric 0,1 mol/l nh mc n 100 ml. Dung
dch chun lm vic ny c nng 0.5 g/ml.
1.3 Tin hnh
ng th: Cho 20ml dung dch th vo ng Nessler, thm nc ct n 50ml.
ng so snh: Tin hnh ng thi vi mu th, cho 2ml dung dch chun ch, thm 20ml dung dch
acid acetic 4%, thm nc ct n 50ml.
Nh vo mi ng 2 git thuc th Natri sulfid, yn trong 5 pht, sau quan st c 2 ng trn nn
trng.
Nu sau khi cho natri sulfid vo dung dch m xut hin mu trng c th phi cho thm dung dch
amoniac vo dung dch th a pH dung dch ln 7 hoc cao hn, sau thm dung dch kali
xyanid ri tin hnh phn ng trn dung dch ny.
2. Xc nh Phenol
2.1 Chun b dung dch th
2

Ra sch mu bng nc ct, ngm thi trong dung dch ngm theo t l 2ml/1cm mu (loi khng
dnh cho tr nh), v t l 20ml/g mu (loi dnh cho tr nh), s dng dung dch ngm v iu kin
ngm theo hng dn phn quy nh k thut
2.2 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.

2.3 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
2.4 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 kali fericyanid v nc n 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 dung dch th
khng c vt qu hp th quang ca dung dch chun lm vic.
3. Xc nh Formaldehyd
3.1 Chun b dung dch th
2

Ra sch mu bng nc ct, ngm thi trong dung dch ngm theo t l 2ml/1cm mu (loi khng
dnh cho tr nh), v t l 20ml/g mu (loi dnh cho tr nh), s dng dung dch ngm v iu kin
ngm theo hng dn phn quy nh k thut
3.2 Tin hnh
Cho vo ng o c chia vch 200 ml mt lng 10 ml dung dch mu vi 1 ml acid photphoric 20%,
sau thm 5-10 ml nc v tin hnh ko ct 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 trong cch thy 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 trong cch thy si trong 10 pht. Quan st cc ng nghim
trn nn trng, mu th khng c thm mu hn mu so snh.
4. Xc nh km
4.1 Chun b dung dch th:
Ra sch mu bng nc ct, ngm thi trong dung dch ngm theo t l 2ml/1cm2 mu (loi khng
dnh cho tr nh), hoc t l 20ml/g mu (loi dnh cho tr nh), s dng dung dch ngm v iu
kin ngm theo hng dn phn quy nh k thut.
a) Ly 1 ml dung dch ny v thm acid acetic 4% nh mc n 15 ml (loi khng dnh cho tr
nh)
b) Ly 20ml dung dch mu nh 5 git acid acetic (loi dnh cho tr nh)
4.2 Chun b dung dch chun
Cn 1,0 g km, ha tan trong acid hydrochloric nng 6 mol/l, cho bay hi v ha cn trn b cch
thy. Thm acid hydrochloric 1 mol/l vo cn nh mc n 1.000 ml. Dung dch chun gc c nng
km 1mg/ml.
- Chun b dung dch chun lm vic:
Ly 1 ml dung dch km chun gc, thm nc v nh mc n 50 ml. Ly 1 ml dung dch ny v
thm nc nh mc n 20 ml. Nng km ca dung dch chun lm vic l 1 g/ml.
4.3 Tin hnh:
Phn tch km bng phng php quang ph hp th nguyn t hoc quang ph pht x plasma
trong dung dch ny, kt qu cn so snh vi chun tng ng.
5. Cn kh
5.1 Chun b dung dch th:

Ra sch cc mu bng nc ct, ngm thi trong dung dch ngm theo t l 2ml/1cm mu (loi
khng dnh cho tr nh), v t l 20ml/g mu (loi dnh cho tr nh), s dng dung dch ngm v
iu kin ngm theo hng dn phn quy nh k thut.
5.2 Tin hnh:
Ly 200-300 ml dung dch th cho bay hi trn b cch thy n khi bc hi ht dung dch v cn li
o
cn cng. Sy kh cn trong 2 gi 105 C, ngui trong bnh ht m, cn chn v cn xc nh
khi lng cn (s chnh lch trng lng chn v cn vi trng 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 hm lng cn:
Cn kh (g/ml) = [(a-b) x1,000] / th tch dung dch th
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 nc ct.

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

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.

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 dch dng ngm mu th.
II. YU CU K THUT
Th thi nhim
Ch tiu kim
tra

iu kin ngm thi

0

[5]

60 C trong 30 pht
Arsen

60 C trong 30 pht
0

[5]

60 C trong 30 pht
Cadimi

60 C trong 30 pht
0

[5]

60 C trong 30 pht
Ch
Phenol
Formaldehyd

60 C trong 30 pht
0

[5]

60 C trong 30 pht
0

Vinylchlorid

Dung dch acid citric

[4]
0.5%

[5]

25 C trong 2 gi
0

0,2 g/ml

[3]

Nc

Dung dch acid citric

[4]
0.5%

0,1 g/ml

[3]

Nc

Dung dch acid citric

[4]
0.5%
Nc

Ethanol 20%

0,4 g/ml
5 g/ml

[8]

m tnh

[8]

[2]

30 g/ml

[3] , [7]

60 C trong 30 pht
Epichlorohydrin

[3]

Nc

Heptan

60 C trong 30 pht
0

Gii hn ti a

[1] , [6]

25 C trong 1 gi
Cn kh

Dung dch ngm thi

Khng qu 5 C trong 24h

Nc

Acid acetic 4%
Pentan
Ethanol 20%

[8]

[4]

0,5 g/ml

[8] , [9]

0,05 g/ml

[8]

Ghi ch
[1]

Mu dng cha ng cht bo, du n v thc phm cha cht bo.

[2]

Mu dng cha ng ung c cn.

[3]

Mu dng cha ng thc phm c pH ln hn 5.

[4]

Mu dng cha ng thc phm c pH nh hn hoc bng 5.

[5]

i vi dng c s dng nhit ln hn 100 C iu kin ngm 95 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
[6]
mu c th c s dng tng t nh 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 cc sn phm bao b, dng c kim loi phi cng b hp
quy ph hp vi cc quy nh k thut ti 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.

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.
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 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
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:
- 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
0
mt chn bch kim, thch anh, hoc cc thy tinh chu nhit ( gia nhit ti 105 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
0
105 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 C

Thit b o

S dng detector ion ha ngn la hydro. Vn hnh nhit

0
khong 220 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

200 C

Detector

S dng detector ion ha bng ngn la hydro. Vn hnh

o
nhit khong 250 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 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