Quy Chuẩn Kỹ Thuật Quốc Gia QCVN 12-1:2011/BYT

You might also like

You are on page 1of 19

QUY CHUN K THUT QUC GIA

QCVN 12-1:2011/BYT
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

Gii hn ti
a

Th thi nhim
Ch tiu kim
tra

iu kin
ngm thi

Dung dch
ngm thi

Gii hn
ti a

Acid acetic
4%

Kim loi nng


Ch

100 g/g

Cadmi

100 g/g

1 g/ml

600C trong

10 g/ml

30 pht [7]

Lng KMnO4
s dng[1]

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

iu kin ngm thi

Dung dch ngm thi

600C trong 30 pht[7]

Formaldehyd

5 g/ml

Nc

25oC trong 1 gi

m tnh

Heptan

60 C trong 30 pht

Cn kh

Gii hn ti a

Ethanol 20%

30 g/ml
[4]

Nc

600C trong 30 pht[7]

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
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

Gii hn ti a

Th thi nhim
Ch tiu kim
tra

iu kin
ngm thi

Dung dch
ngm thi

Gii hn ti a

Vinyl clorid

1g/g

150 g/ml

25 C trong
1 gi

[3]

Heptan

30 g/ml
Cresyl
phosphat

1g/g

Cc hp cht
dibutyl thic

50/g

60 C trong
30 pht

Cn kh

Ethanol 20%
[4]

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

Dung dch ngm thi

Heptan

[3]

Ethanol 20%

25 C trong 1 gi
Cn kh

60 C trong 30 pht
0

Gii hn ti a
[a]

30 g/ml

[4]

Nc[5]

[7]

60 C trong 30 pht

30 g/ml

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 vt liu
Ch tiu kim tra
Tng s cht bay
hi(styren, tuluen,
ethybenzen, npropyl benzen)

Th thi nhim
Gii hn
ti a

Ch tiu kim
tra

Dung dch
ngm thi

5mg/g

2mg/g

Gii hn
ti a
240 g/ml

Cn kh

Polylstyren trng
n(khi dng nc

iu kin
ngm thi

25 C trong
1 gi

600C trong
30 pht

[3]

Heptan

Ethanol 20%
[4]

30 g/ml

si)

Nc[5]

Styren v
Ethybenzen

60 C trong
[7]
30 pht

1mg/g

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 vt liu
Ch tiu kim
tra

Th thi nhim

Gii hn ti a

Ch tiu
kim tra

iu kin
ngm thi

Dung dch
ngm thi

Bari

100 g/g

25oC 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]


Nc[5]

60 C 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
Antimony
Germani

iu kin ngm thi

[7]

60 C trong 30 pht
o

Heptan

600C trong 30 pht


0

[7]

60 C trong 30 pht

Gii hn ti a
0,05 g/ml

Acid acetic 4%
[3]

25 C trong 1 gi
Cn kh

Dung dch ngm thi

0,1 g/ml
30 g/ml

Ethanol 20% [4]


Nc[5]
[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

iu kin ngm thi

Dung dch ngm thi

Gii hn ti a

Methyl methacrylat

60 C trong 30 pht
o

15 g/ml

Ethanol 20%
[3]

25 C trong 1 gi

Heptan

60 C trong 30 pht
Cn kh

30 g/ml
[4]

Ethanol 20%
[5]

Nc
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
Caprolactam

iu kin ngm thi


0

60 C trong 30 pht
o

Gii hn ti a

Ethanol 20%

15 g/ml

[3]

25 C trong 1 gi

Heptan

Cn kh

Dung dch ngm thi

60 C trong 30 pht

30 g/ml
[4]

Ethanol 20%
[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

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]

[5]

Cn kh

Nc
600C trong 30 pht[7]

30 g/m l
[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

Th thi nhim

Ch tiu kim
tra
Bis-phenol A
(Phenol,P-tbutylphenol)[8]

Gii hn
ti a

Ch tiu
kim tra

600C trong 30
pht

Khng qu
500g/g

Gii hn
ti a
2,5 g/ml

[3]

Heptan

Ethanol 20% [4]


[5]

Nc
600C trong 30
pht[7]

Cn kh
Amin(triethylam
in v
tributylamin)

Dung dch ngm


thi

25oC trong 1
gi

Khng qu
500g/g
Bisphenol A
(Phenol,P-tbutylphenol)

Diphenyl
carbonat

iu kin
ngm thi

Acid acetic 4%[6]

25oC trong 1
gi

Heptan

600C trong 30
pht

Ethanol 20%

30 g/ml

[3]

[4]

Nc[5]
0

60 C trong 30
pht[7]

Khng qu
1g/g

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
Acid lactic tng s

iu kin ngm thi

Dung dch ngm thi

Gii hn ti a

Nc

30 g/ml

60 C trong 30 pht
o

[3]

25 C trong 1 gi

Heptan

600C trong 30 pht

30 g/ml

Ethanol 20% [4]


[5]

Cn kh

Nc
600C trong 30 pht[7]

[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
Cn kh

iu kin ngm thi


25oC trong 1 gi

Dung dch ngm thi

Gii hn ti a

Heptan[3]

30 g/ml

600C trong 30 pht

Ethanol 20% [4]


[5]

[7]

60 C trong 30 pht

Nc

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]

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 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
tim mu

bung

250 C

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

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

2000C

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

2200C

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


S dng kh nit hoc heli. iu chnh tc dng kh cc
diethylbenzen xut hin thi im khong 11 pht

Kh mang
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,Ndimethyl 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-tertbutylphenol, 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

40oC

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

40oC

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

200 C

mu
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
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
0
cn trong 2 gi 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
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

Nhit ct

240oC.

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

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-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-tertbutylphenol, 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

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

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

You might also like