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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 thi nhim

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

Kim loi nng


600C trong
[7]
Lng KMnO4 30 pht
s dng[1]

Dung dch
ngm thi

Gii hn
ti a

Acid acetic
4%

1 g/ml
10 g/ml

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 iu kin ngm thi
Phenol
Formaldehyd

600C trong 30 pht[7]


o

25 C trong 1 gi
600C trong 30 pht

Cn kh

Dung dch ngm


thi

600C trong 30 pht[7]

Gii hn ti a
5 g/ml

Nc

m tnh

Heptan

30 g/ml

Ethanol 20% [4]


Nc
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

iu kin ngm thi

Dung dch ngm


thi

Gii hn ti a

600C trong 30 pht[7]

Phenol

m tnh
Nc

Formaldehyd

m tnh
30 g/ml

Cn kh

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

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%

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
25oC trong 1 gi

Cn kh

600C trong 30 pht


0

[7]

60 C trong 30 pht

Dung dch ngm


thi

Gii hn ti a

Heptan[3]

30 g/ml [a]

Ethanol 20% [4]

30 g/ml

Nc[5]
Acid acetic 4%[6]

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 thi nhim

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]

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 thi nhim

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]

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
Antimony
Germani

600C trong 30 pht[7]


25oC trong 1 gi

Gii hn ti a

Acid acetic 4%

0,05 g/ml
0,1 g/ml

Heptan[3]

Cn kh

Dung dch ngm


thi

60 C trong 30 pht
600C trong 30 pht[7]

Ethanol 20%

30 g/ml
[4]

Nc[5]
Acid acetic 4%[6]

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 iu kin ngm thi

Dung dch ngm


thi

Gii hn ti a

Methyl
methacrylat

600C trong 30 pht


25oC trong 1 gi

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

Acid acetic 4%[6]

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 iu kin ngm thi
Caprolactam

600C trong 30 pht


o

Ethanol 20%

15 g/ml

Heptan

60 C trong 30 pht
0

Gii hn ti a

[3]

25 C trong 1 gi
Cn kh

Dung dch ngm


thi

[7]

60 C trong 30 pht

30 g/ml

Ethanol 20%

[4]

Nc[5]
Acid acetic 4%[6]

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
25oC trong 1 gi
0

60 C trong 30 pht
Cn kh

Dung dch ngm


thi

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

Acid acetic 4%[6]

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

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]

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 iu kin ngm thi
Acid lactic tng s 600C trong 30 pht
25oC trong 1 gi

Dung dch ngm


thi

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]

Acid acetic 4%[6]

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
25oC trong 1 gi
Cn kh

60 C trong 30 pht
0

[7]

60 C trong 30 pht

Dung dch ngm


thi

Gii hn ti a

Heptan[3]

30 g/ml

Ethanol 20%
Nc[5]

[4]

Acid acetic 4%[6]

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.

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 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 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 bung 2500C


tim mu
Detector

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 acetonitril, y cht nt bnh v qua m khong 400C. 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

500C

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
Nhit ct
Nhit bung tim mu
Detector

Kh mang

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
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.
2000C
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
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
Nhit ct
Nhit bung tim mu
Detector

Kh mang

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
un nng ct t 60 oC sau tng nhit t t, c
4C mi pht cho n khi t 100C, v tip tc tng
10 oC mi pht cho n khi t 150oC
2200C
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
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 trc tip trn ngn la khong 3000C, sau nung khong
4500C 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
Nhit ct

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
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


2000C
mu
Detector ion ha ngn la hydro. Vn hnh nhit
Detector
khong 250C. 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
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-tertbutylphenol 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


S dng ct bng thp khng g di 250 mm c ng knh
Ct sc k
trong l 4,6 mm
Nhit ct
40oC
Detector
Detector quang ph ngoi. Vn hnh bc sng 217 nm
Pha ng
A = acetonitril ; B= nc ct
Gradient dung mi tuyn tnh vi t l A :B t 30 :70 n
Chng trnh dung
100 :0 trong thi gian 35 pht ; sau duy tr dung mi A
mi
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
Ct sc k
Nhit ct
Detector
Pha ng

S dng gel silica octadecylsilyl


S dng ct bng thp khng g di 250 mm c ng knh trong
l 4,6 mm
40oC
S dng Detector quang ph t ngoi. Vn hnh bc sng
217 nm
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
Nhit ct

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


c ph mt lp dimethylpolysiloxan dy 5 m
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
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

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
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

3. Xc nh phenol trong nha phenol, melamin v ure


3.1 Chun b dung dch th
Ra sch mu bng nc ct, ngm thi 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.
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
Ra sch mu bng nc ct, ngm thi mu trong dung dch ngm t l 2ml/1cm2
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 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

7.1 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.
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


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.
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
Nhit ct
Nhit bung tim mu
Detector

Kh mang

S dng ct bng thy tinh silicat di 30 m ng


knh trong 0,32 mm c ph mt lp
dimethylpolysiloxan dy 5 m
un nng ct n 120C trong 1 pht, sau tng
nhit t t, c 5C mi pht cho n khi t
170C.
2000C
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
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


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.
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
240oC.

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

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


10.1 Chun b dung dch th
Ra k mu bng nc, s dng dung dch ngm vi t l 2ml/cm2 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-tertbutylphenol 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
Ct sc k
Nhit ct
Detector
Pha ng
Chng trnh
dung mi

S dng gel silica octadecylsily


S dng ct bng thp khng g di 250 mm c ng knh trong
l 4,6 mm
40oC
S dng detector quang ph t ngoi. Vn hnh bc sng
217 nm
A = acetonitril ; B= nuc ct
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
Ra sch cc mu bng nc ct, sau ngm mu trong dung dch ngm theo t
l 2ml/cm2 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
Ct sc k
Nhit ct
Detector
Pha ng

S dng gel silica octadecylsilyl


S dng ct bng thp khng g di 250 mm c
ng knh trong l 4,6 mm
40oC
Detector quang ph t ngoi. Vn hnh bc
sng 210 nm
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

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