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Coeus - VN - g1.BAO BÌ NH A T NG H P
Coeus - VN - g1.BAO BÌ NH A T NG H P
Coeus - VN - g1.BAO BÌ NH A T NG H P
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.
Th vt liu
Ch tiu
kim tra
Ch
Cadmi
Gii hn
ti a
100 g/g
100 g/g
Ch tiu kim
tra
iu kin
ngm thi
Dung dch
ngm thi
Gii hn
ti a
Acid acetic
4%
1 g/ml
10 g/ml
Nc
25 C trong 1 gi
600C trong 30 pht
Cn kh
Gii hn ti a
5 g/ml
Nc
m tnh
Heptan
30 g/ml
Gii hn ti a
Phenol
m tnh
Nc
Formaldehyd
m tnh
30 g/ml
Cn kh
Acid acetic 4%
Gii hn ti a
Th thi nhim
Ch tiu
kim tra
Vinyl clorid
25oC trong
1 gi
1g/g
Cresyl
phosphat
1g/g
Cc hp
50/g
iu kin
ngm thi
Dung dch
ngm thi
Gii hn ti a
150 g/ml
[3]
Heptan
30 g/ml
Cn kh
600C trong
30 pht
Ethanol 20%
[4]
cht dibutyl
thic
Nc[5]
600C trong
30 pht
Acid acetic
4%
iu kin ngm
thi
25oC trong 1 gi
Cn kh
[7]
60 C trong 30 pht
Gii hn ti a
Heptan[3]
30 g/ml [a]
30 g/ml
Nc[5]
Acid acetic 4%[6]
Th vt liu
Ch tiu kim tra
Tng s cht
bay hi(styren,
tuluen,
ethybenzen, npropyl benzen)
Gii hn
ti a
Ch tiu
kim tra
iu kin
ngm thi
Dung dch
ngm thi
Gii hn
ti a
240 g/ml
5mg/g
25oC trong
1 gi
Heptan[3]
Ethanol 20%
Cn kh
Polylstyren
trng n(khi
dng nc si)
2mg/g
600C trong
30 pht
Styren v
Ethybenzen
1mg/g
600C trong
30 pht[7]
30 g/ml
[4]
Nc[5]
Acid acetic
4%[6]
Th vt liu
Ch tiu
kim tra
Gii hn ti
a
Ch tiu
kim tra
iu kin
ngm thi
Dung dch
ngm thi
Gii hn
ti a
Heptan[3]
30 g/ml
Bari
100 g/g
25oC trong 1
gi
Vinyliden
Clorid
Khng qu 6
g/g
600C trong
30 pht
Cn kh
Ethanol 20%
[4]
Nc[5]
600C trong
30 pht[7]
Acid acetic
4%
[6]
Gii hn ti a
Acid acetic 4%
0,05 g/ml
0,1 g/ml
Heptan[3]
Cn kh
60 C trong 30 pht
600C trong 30 pht[7]
Ethanol 20%
30 g/ml
[4]
Nc[5]
Acid acetic 4%[6]
Gii hn ti a
Methyl
methacrylat
15 g/ml
Ethanol 20%
Heptan[3]
60 C trong 30 pht
Cn kh
30 g/ml
Ethanol 20%
[4]
Nc[5]
0
[7]
60 C trong 30 pht
Ethanol 20%
15 g/ml
Heptan
60 C trong 30 pht
0
Gii hn ti a
[3]
25 C trong 1 gi
Cn kh
[7]
60 C trong 30 pht
30 g/ml
Ethanol 20%
[4]
Nc[5]
Acid acetic 4%[6]
60 C trong 30 pht
Cn kh
Gii hn ti a
Heptan[3]
120 g/ml
Ethanol 20%
[4]
Nc[5]
0
30 g/m l
[7]
60 C trong 30 pht
Th thi nhim
Ch tiu kim
tra
Gii hn
ti a
Bis-phenol A
(Phenol,P-tbutylphenol)[8]
Khng qu
500g/g
Diphenyl
carbonat
Khng qu
500g/g
Ch tiu
kim tra
iu kin
ngm thi
Dung dch
ngm thi
Gii hn ti
a
25oC trong 1
gi
Heptan[3]
2,5 g/ml
600C trong 30
Ethanol 20% [4]
Bisphenol A pht
(Phenol,P-tNc[5]
butylphenol)
600C trong 30
Acid acetic 4%
pht[7]
[6]
25oC trong 1
gi
Cn kh
Amin(triethyla
min v
tributylamin)
30 g/ml
600C trong 30
Ethanol 20% [4]
pht
Nc[5]
600C trong 30
pht[7]
Khng qu
1g/g
Heptan[3]
Acid acetic
4%[6]
30 g/ml
Nc
Heptan[3]
60 C trong 30 pht
Cn kh
Ethanol 20%
Gii hn ti a
30 g/ml
[4]
Nc[5]
600C trong 30 pht[7]
60 C trong 30 pht
0
[7]
60 C trong 30 pht
Gii hn ti a
Heptan[3]
30 g/ml
Ethanol 20%
Nc[5]
[4]
Ghi ch
[1]
Ngoi tr bao b, dng c c thnh phn chnh l nha Phenol, nha Melamin v nha
Ure.
[2]
Dng c nu n, b n ung.
[3]
Bao b, dng c nha cha ng cht bo, du n v thc phm cha cht bo.
[4]
Bao b, dng c nha cha ng ung c cn.
[5]
Bao b, dng c nha cha ng thc phm c pH ln hn 5.
[6]
Bao b, dng c nha cha ng thc phm c pH nh hn hoc bng 5.
[7]
0
0
Bao b, dng c nha 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.
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 400C, thnh thong lc trn u. Sau khi lm
ngui, lc ly dch, thu dch lc v dch ra, c n khong 1ml trn my c quay
chn khng nhit khng qu 400C. 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 acetic-natri 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 ct
Kh mang
Nhit ct
500C
Detector
Pha ng
Kh mang
Ct sc k
Nhit ct
Nhit bung tim mu
Detector
Kh mang
Chng trnh
dung mi
Nhit bung
2000C
tim mu
Detector nhit ion ngn la kim hoc mt detector nitphosphor nhy cao. Vn hnh nhit gn 250C. iu
Detector
chnh lu lng ca khng kh v hydro sao cho nhy
pht hin ti a
S dng kh heli. iu chnh tc dng kh triethylamin
Kh mang
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
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
Ra sch mu bng nc ct, ngm trong dung dch ngm thi theo t l 2ml /1cm2
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
- Ra sch mu bng nc ct, ngm thi mu trong dung dch theo t l 2ml/1cm2
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
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 mt chn bch kim, thch anh, hoc cc thy
tinh chu nhit ( gia nhit ti 1050C 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 1050C, 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
Ra sch mu bng nc ct, ngm trong dung dch ngm theo t l 2ml /1cm2
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
Kh mang
9. Caprolactam
Nhit ct
Nhit bung tim
2400C
mu
Detector ion ha bng ngn la hydro. Vn hnh nhit
Detector
khong 240C. iu chnh lu lng ca khng kh v
hydro sao cho nhy pht hin ti a
S dng kh nit hoc heli. iu chnh tc dng kh
Kh mang
caprolactam xut hin thi im khong 5 pht
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
Ct sc k
Nhit ct
Detector
Pha ng
Chng trnh
dung mi