K bi: Cng Thng tin in t Chnh ph

Email: thongtinchinhphu@chinhphu.vn
C quan: Vn phng Chnh ph
Thi gian k: 25.12.2015 09:37:47 +07:00

CNG BO/S 1217 + 1218/Ngy 23-12-2015

47

B Y T

CNG HA X HI CH NGHA VIT NAM

c lp - T do - Hnh phc

S: 47/2015/TT-BYT

H Ni, ngy 01 thng 12 nm 2015

THNG T
Ban hnh Quy chun k thut quc gia
v cht h tr ch bin thc phm - Dung mi
Cn c Lut an ton thc phm ngy 17 thng 6 nm 2010 v Ngh nh s
38/2012/N-CP ngy 25 thng 4 nm 2012 ca Chnh ph v vic quy nh chi tit
thi hnh mt s iu ca Lut an ton thc phm;
Cn c Lut tiu chun v quy chun k thut ngy 29 thng 6 nm 2006 v
Ngh nh s 127/2007/N-CP ngy 01 thng 8 nm 2007 ca Chnh ph quy nh
chi tit thi hnh mt s iu ca Lut tiu chun v quy chun k thut;
Cn c Ngh nh s 63/2012/N-CP ngy 31 thng 8 nm 2012 ca Chnh ph
quy nh chc nng, nhim v, quyn hn v c cu t chc ca B Y t;
Theo ngh ca Cc trng Cc An ton thc phm;
B trng B Y t ban hnh Thng t ban hnh Quy chun k thut quc gia
v cht h tr ch bin thc phm - Dung mi.
iu 1. Ban hnh km theo Thng t ny:
QCVN 18-1:2015/BYT - Quy chun k thut quc gia v cht h tr ch bin
thc phm - Dung mi.
iu 2. Thng t ny c hiu lc thi hnh k t ngy 01 thng 9 nm 2016.
iu 3. Cc trng Cc An ton thc phm, th trng cc n v thuc B Y t,
n v trc thuc B Y t; gim c S Y t cc tnh, thnh ph trc thuc Trung
ng v cc c quan, t chc, c nhn c lin quan chu trch nhim thi hnh Thng
t ny./.
KT. B TRNG
TH TRNG

Nguyn Thanh Long

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CNG BO/S 1217 + 1218/Ngy 23-12-2015

CNG HA X HI CH NGHA VIT NAM

QCVN 18-1:2015/BYT

QUY CHUN K THUT QUC GIA

V CHT H TR CH BIN THC PHM - DUNG MI
National technical regulation on food processing aids - Sovents

H NI - 2015

CNG BO/S 1217 + 1218/Ngy 23-12-2015

49

Li ni u
QCVN 18-1:2015/BYT do Ban son tho quy chun k thut quc gia v Ph gia
thc phm v cht h tr ch bin bin son, Cc An ton thc phm trnh duyt,
B Khoa hc v Cng ngh thm nh v c ban hnh theo Thng t s 47/2015/
TT-BYT ngy 01 thng 12 nm 2015 ca B trng B Y t.

50

CNG BO/S 1217 + 1218/Ngy 23-12-2015

QUY CHUN K THUT QUC GIA
V CHT H TR CH BIN THC PHM - DUNG MI
National technical regulation on food processing aids - Sovents
I. QUY NH CHUNG
1. Phm vi iu chnh

Quy chun ny quy nh cc yu cu k thut, yu cu qun l i vi cc dung

mi c s dng vi mc ch lm cht h tr ch bin thc phm (sau y gi
tt l dung mi).
2. i tng p dng
Quy chun ny p dng i vi:
2.1. Cc t chc, c nhn nhp khu, sn xut, kinh doanh cc dung mi ti
Vit Nam.
2.2. Cc c quan qun l nh nc c lin quan.
3. Gii thch ch vit tt
Trong quy chun ny, cc ch vit tt di y c hiu nh sau:
3.1. M s C.A.S (Chemical Abstracts Service): M s ng k ha cht ca
Hip hi Ha cht Hoa K.
3.2. TS (test solution): Dung dch thuc th.
3.3. ADI (Acceptable daily intake): Lng n vo hng ngy chp nhn c.
3.4. INS (International numbering system): H thng m s quc t v ph gia
thc phm.
4. Ti liu vin dn
4.1. JECFA monograph 1 - Vol.4: Cc yu cu k thut i vi ph gia thc phm,
Tp 4 Cc phng php phn tch, quy trnh th nghim, dung dch th nghim
c s dng (hoc tham chiu) trong yu cu k thut i vi ph gia thc phm;
JECFA bin son; FAO ban hnh nm 2006.
4.2. TCVN 6469:2010 Ph gia thc phm - Phng php nh gi ngoi quan
v xc nh cc ch tiu vt l.
4.3. TCVN 6471:2010 Ph gia thc phm - Phng php th i vi cc cht
to hng.
4.4. TCVN 8900-1:2012 Ph gia thc phm - Xc nh cc thnh phn v c.
Phn 1: Hm lng nc (Phng php Karl Fischer).
4.5. TCVN 8900-2:2012 Ph gia thc phm - Xc nh cc thnh phn v c Phn 2: Hao ht khi lng khi sy, hm lng tro, cht khng tan trong nc v
cht khng tan trong axit.

CNG BO/S 1217 + 1218/Ngy 23-12-2015

51

4.6. TCVN 8900-6:2012 Ph gia thc phm - Xc nh cc thnh phn v c Phn 6: nh lng antimon, bari, cadimi, crom, ng, ch v km bng o ph hp
th nguyn t ngn la.
4.7. TCVN 8900-7:2012 Ph gia thc phm - Xc nh cc thnh phn v c - Phn
7: nh lng antimony, bari, cadimi, crom, ng, ch v km bng o ph pht x
nguyn t plasma cm ng cao tn (ICP-AES).
4.8. TCVN 8900-8:2012 Ph gia thc phm - Xc nh cc thnh phn v c Phn 8: nh lng ch v cadimi bng o ph hp th nguyn t dng l graphit.
II. YU CU K THUT, PHNG PHP TH, LY MU V GHI NHN
1. Cc yu cu k thut v phng php th
Yu cu k thut v phng php th i vi cc dung mi c quy nh ti
cc ph lc ban hnh km theo Quy chun ny nh sau:
1.1.

Ph lc 1:

Yu cu k thut v phng php th i vi Aceton

1.2.

Ph lc 2:

Yu cu k thut v phng php th i vi Isoamyl acetat

1.3.

Ph lc 3:

Yu cu k thut v phng php th i vi Butan-1,3-diol

1.4.

Ph lc 4:

Yu cu k thut v phng php th i vi Butan-1-ol

1.5.

Ph lc 5:

Yu cu k thut v phng php th i vi Cyclohexan

1.6.

Ph lc 6:

Yu cu k thut v phng php th i vi Diethyl ether

1.7.

Ph lc 7:

Yu cu k thut v phng php th i vi Ethyl acetat

1.8.

Ph lc 8:

Yu cu k thut v phng php th i vi Ether du ha

1.9.

Ph lc 9:

Yu cu k thut v phng php th i vi Toluen

1.10. Ph lc 10:

Yu cu k thut v phng php th i vi Benzyl alcohol

1.11. Ph lc 11:

Yu cu k thut v phng php th i vi Butan-2-ol

1.12. Ph lc 12:

Yu cu k thut v phng php th i vi Dicloromethan

1.13. Ph lc 13:

Yu cu k thut v phng php th i vi cc Hexan

Cc phng php th c hng dn trong Quy chun ny khng bt buc

phi p dng, c th s dng cc phng php th khc nhng phi c chnh
xc tng ng.
2. Quy nh ly mu
Vic ly mu c thc hin theo hng dn ti Thng t s 26/2012/TT-BKHCN
ngy 12 thng 12 nm 2012 ca B trng B Khoa hc v Cng ngh Quy nh
vic kim tra nh nc v cht lng hng ha lu thng trn th trng v cc
quy nh khc ca php lut c lin quan.

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CNG BO/S 1217 + 1218/Ngy 23-12-2015

3. Yu cu v ghi nhn

Vic ghi nhn cc dung mi theo ng quy nh ti Ngh nh s 89/2006/N-CP

ngy 30 thng 8 nm 2006 ca Chnh ph v nhn hng ha, Thng t lin tch s
34/2014/TTLT-BYT-BNNPTNT-BCT ngy 27 thng 10 nm 2014 ca B trng
B Y t, B trng B Nng nghip v Pht trin nng thn, B trng B Cng
thng hng dn ghi nhn hng ha i vi thc phm, ph gia thc phm v cht
h tr ch bin thc phm bao gi sn v cc quy nh ca php lut c lin quan.
III. YU CU QUN L
1. Cng b hp quy
1.1. Cc dung mi phi c cng b 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 iu 6,
iu 7 Ngh nh s 38/2012/N-CP ngy 25 thng 4 nm 2012 ca Chnh ph quy
nh chi tit thi hnh mt s iu ca Lut an ton thc phm v iu 4, iu 5,
iu 7, iu 9 Thng t s 19/2012/TT-BYT ngy 09 thng 11 nm 2012 ca B trng
B Y t hng dn vic cng b hp quy v cng b ph hp quy nh an ton thc
phm v cc quy nh khc ca php lut c lin quan.
2. Thanh tra, kim tra v x l vi phm php lut
C quan nh nc c thm quyn thc hin vic thanh tra, kim tra v x l vi
phm php lut i vi t chc, c nhn nhp khu, sn xut, kinh doanh dung mi
vi phm cc quy nh v k thut v qun l quy nh ti Quy chun ny v cc quy
nh php lut khc c lin quan.
IV. TRCH NHIM CA T CHC, C NHN
1. T chc, c nhn nhp khu, sn xut, kinh doanh dung mi phi cng b hp
quy theo cc yu cu ca Quy chun ny.
2. T chc, c nhn ch c php nhp khu, sn xut, kinh doanh dung mi
sau khi c Cc An ton thc phm cp Giy tip nhn bn cng b hp quy
v p ng cc quy nh php lut hin hnh khc c lin quan.
V. T CHC THC HIN
1. Giao Cc An ton 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 thc phm c trch nhim kin ngh
B trng B Y t sa i, b sung Quy chun ny.
3. Trng hp hng dn ca quc t v phng php th v cc quy nh ca
php lut vin dn trong Quy chun ny c sa i, b sung hoc thay th th p
dng theo vn bn mi.

CNG BO/S 1217 + 1218/Ngy 23-12-2015

53

Ph lc 1
YU CU K THUT V PHNG PHP TH I VI ACETON
1. Tn khc, ch s

Dimethylketone; propanone.

2. nh ngha
Tn ha hc

Propan-2-one

M s C.A.S

67-64-1

Cng thc ha hc

C3H6O

Cng thc cu to

CH3COCH3

Khi lng phn t

58,08

3. Cm quan

Cht lng trong, khng mu, d bay hi, rt d chy,

c mi c trng, khng cha cn v cc cht l lng

4. Chc nng

Dung mi chit, cht to hng

5. Yu cu k thut
5.1. nh tnh
tan

C th trn ln vi nc v ethanol bt k t l no

Trng lng ring

d2020: 0,790 - 0,793

Ch s khc x

n20D: 1,358 - 1,360

5.2. tinh khit

Khong nhit chng ct

55,5oC - 57,0oC

Cn khng bay hi

Khng c qu 0,001% (kl/kl)

acid

Khng c qu 0,002% (kl/kl) (tnh theo acid acetic)

Phenol

Khng c qu 0,001% (kl/kl)

Cc cht d oxi ha

t yu cu trong phn phng php th

5.3. Hm lng C3H6O

Khng thp hn 99,5% (kl/kl).

6. Phng php th
6.1. Th nh tnh
tan

TCVN 6469:2010

Trng lng ring

TCVN 6469:2010

Ch s khc x

TCVN 6469:2010

6.2. Th tinh khit

Khong nhit chng ct

TCVN 6469:2010

Cn khng bay hi

TCVN 8900-2:2012

acid

Ht 100 ml nc ct va un si ngui (trung tnh

vi dung dch th phenolphatalein) v vi ht chng

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CNG BO/S 1217 + 1218/Ngy 23-12-2015

tro trong bnh cu 500 ml bng thy tinh boro-silicat
v un si trong 5 pht loi carbon dioxid. ngui
t t v thm 100 ml mu. un si nh thm 5 pht.
y bnh bng np c ni vi ng cha xt. Khi ngui,
m np v thm 0,5 ml dung dch th phenolphthalein
v kim tra tnh kim. Nu khng kim chun bng
dung dch natri hydroxyd s dng micro buret.
Tnh acid theo acid acetic (%, kl/kl) theo cng thc
% acid =

6xT
dx1000

Trong :
T = th tch (ml) ca dung dch natri hydroxyd 0,1 N s dng
d = trng lng ring ca mu
Phenol

Ly 3ml mu th vo chn nung v cho bay hi n

kh 60oC, thm 3 git dung dch Natri nitrit (0,1g
Natri nitrit ha tan trong 5 ml acid sulphuric) yn
trong 2 - 3 pht. Thm t t 3 ml Natri hydroxyd 2 N,
khng c xut hin mu.

Cc cht d oxi ha

Lc 30 ml mu vi 0,1 ml dung dch kali permanganat 3%

mi pha trong nc; yn 20oC trong 15 pht khng
c xut hin mu

6.3. Th nh lng

Cn chnh xc khong 1 g mu vo bnh c cha 20 ml

nc v thm nc n 1000 ml. Ht 10 ml dung dch vo
bnh thy tinh c np, thm 25 ml natri hydroxyd 0,1N
v n nh trong 5 pht. Thm 25 ml iod 0,1 N, y
np v n nh ch ti v lnh trong 10 pht,
thm 30 ml acid sulfuric 1 N. Chun iod d bng
natri thiosulfat s dng ch th h tinh bt. Thc hin
mu trng tng t nh mu th v tnh kt qu
hiu chnh theo mu trng. Mi ml iod 0,1 N tng ng
vi 0,9675 mg C3H6O.

CNG BO/S 1217 + 1218/Ngy 23-12-2015

55

Ph lc 2
YU CU K THUT V PHNG PHP TH I VI ISOAMYL ACETAT
1. Tn khc, ch s

Amyl acetate, isoamyl ethanoate

2. nh ngha

Hn hp cc ester ca acid acetic vi cc pentanol

Tn ha hc

3-methylbutyl ethanoat (cht chnh)

M s C.A.S

123-92-2

Cng thc ha hc

C7H14O2

Cng thc cu to

Khi lng phn t

130,19

3. Cm quan

Cht lng trong, khng mu, c mi qu c trng

4. Chc nng

Dung mi mang, cht to hng (xem phn Cht to hng

theo JECFA s 139)

5. Yu cu k thut
5.1. nh tnh
tan

Tan t trong nc, khng tan trong glycerol, thc t khng

tan trong propylen glycerol.
Tan trong ethanol, diethyl ether, ethyl acetat, hu ht cc
du khong v du hn hp.

Trng lng ring

d2525: 0,868 - 0,878

Ch s khc x

n20D: 1,400 - 1,404

5.2. tinh khit

Ch s acid

Khng c qu 1

Cn khng bay hi

Khng c qu 7 mg/100 ml

Khong nhit chng ct Khng thp hn 99% (tt/tt) c ct nhit t 135oC

n 143oC
Ch

Khng c qu 2,0 mg/kg

5.3. Hm lng C7H14O2

Khng thp hn 95,0% C7H14O2

6. Phng php th
6.1. Th nh tnh
tan

TCVN 6469:2010

Trng lng ring

TCVN 6469:2010

Ch s khc x

TCVN 6469:2010

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CNG BO/S 1217 + 1218/Ngy 23-12-2015

6.2. Th tinh khit

Ch s acid

TCVN 6471:2010

Cn khng bay hi

TCVN 8900-2:2012

Khong nhit chng ct TCVN 6469:2010

Ch

TCVN 8900-6:2012
TCVN 8900-7:2012
TCVN 8900-8:2012

6.3. Th nh lng

Cn chnh xc khong 0,8 g mu v thc hin theo

hng dn ti JECFA monograph 1-Vol. 4. Phn Xc
nh Este, s dng h s (e) trong cng thc tnh kt
qu bng 65,10.

CNG BO/S 1217 + 1218/Ngy 23-12-2015

57

Ph lc 3
YU CU K THUT V PHNG PHP TH I VI BUTAN-1,3-DIOL
1. Tn khc, ch s

1,3-butylene glycol, -butylene glycol

2. nh ngha
Tn ha hc

Butan-1,3-diol

M s C.A.S

107-88-0

Cng thc ha hc

C4H10O2

Cng thc cu to

Khi lng phn t

90,12

3. Cm quan

Cht lng nht, trong, khng mu, khng mi, ht m

4. Chc nng

Dung mi mang

5. Yu cu k thut
5.1. nh tnh
tan

Trn ln vi nc, aceton v ete.

Tan trong du hn hp, etanol v ete

Trng lng ring

1,004 - 1,006

5.2. tinh khit

Khong nhit chng ct

200oC - 215oC

Nc

Khng c qu 0,5% (kl/kl)

Ch

Khng c qu 2,0 mg/kg

5.3. Hm lng C4H10O2

Khng thp hn 99,0% (kl/kl)

6. Phng php th
6.1. Th nh tnh
tan

TCVN 6469:2010

Trng lng ring

TCVN 6469:2010

6.2. Th tinh khit

Khong nhit chng ct

TCVN 6469:2010

Nc

TCVN 8900-1:2012

Ch

TCVN 8900-6:2012
TCVN 8900-7:2012
TCVN 8900-8:2012

6.3. Th nh lng

Thc hin theo hng dn ti JECFA monograph 1-Vol. 4,

s dng 0,2 g mu

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Ph lc 4
YU CU K THUT V PHNG PHP TH I VI BUTAN-1-OL

1. Tn khc, ch s

Butyl alcohol, n-butyl alcohol, 1-hydroxybutane, n-butanol,

n-propyl carbinol, NBA

2. nh ngha
Tn ha hc

1-butanol, butan-1-ol

M s C.A.S

76-36-3

Cng thc ha hc

C4H10O

Cng thc cu to
Khi lng phn t

74,12

3. Cm quan

Cht lng hi nht, trong, khng mu, c mi c trng

4. Chc nng

Dung mi chit, cht to hng

5. Yu cu k thut
5.1. nh tnh
tan

Tan trong nc, trn ln vi ethanol v ether.

Trng lng ring

0,810 - 0,812

5.2. tinh khit

Khong nhit chng ct 116oC - 118oC
Cn khng bay hi

Khng c qu 2 mg/100 ml

Nc

Khng c qu 0,1%

acid

Khng c qu 0,003% (kl/kl) (theo acid acetic)

Aldehyd v keton

Khng c qu 0,2% (kl/kl)

Cc alcol, ete v tp cht Khng c qu 0,5%; v khng c qu 0,1% i vi

bay hi khc
tng tp cht.
Ch

Khng c qu 2 mg/kg

5.3. Hm lng C4H10O

Khng thp hn 99,5%

6. Phng php th
6.1. Th nh tnh
tan

TCVN 6469:2010

Trng lng ring

TCVN 6469:2010

6.2. Th tinh khit

Khong nhit chng ct TCVN 6469:2010
Cn khng bay hi

TCVN 8900-2:2012

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59

Nc

TCVN 8900-1:2012

acid

Nh vi git phenolphthalein TS vo 60 g dung dch

mu, tin hnh chun bng KOH 0,1 N n khi xut
hin mu hng bn trong t nht 15 giy. Khng c
qu 0,3 ml KOH.

Aldehyd v keton

- JECFA monograph 1-Vol. 4 phn xc nh aldehyd v keton;

- Dng 10 g mu v 36,06 l h s chuyn i (e) trong
tnh ton

Cc alcol, ete v tp cht JECFA monograph 1 - Vol.4

bay hi khc
Ch

TCVN 8900-6:2012
TCVN 8900-7:2012
TCVN 8900-8:2012

6.3. Th nh lng

Thc hin bng sc k kh theo hng dn ti JECFA

monograph 1-Vol. 4 phn Phng php chung vi cc
iu kin nh sau:
Ct di 1,8 m; ng knh trong 6 mm bng thp khng g,
nhi vi P.E.G 400 10% trn nn Chromosorb W (60/80 mesh)
hoc tng ng.
Kh mang: Heli, tc 45 ml/pht
- Detector: Loi ion ha ngn la
- Nhit injector: 150oC
- Nhit ct: 90oC
- Nhit detector: 150oC
Tim 1 n 5 ml mu, trn sc thu c xc nh tng
thnh phn bng phng php chun ha din tch.

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CNG BO/S 1217 + 1218/Ngy 23-12-2015

Ph lc 5
YU CU K THUT V PHNG PHP TH I VI CYCLOHEXAN

1. Tn khc, ch s

Hexahydrobenzene

2. nh ngha
Tn ha hc

Cyclohexan

M s C.A.S

110-82-7

Cng thc ha hc

C6H12

Cng thc cu to
Khi lng phn t

84,16

3. Cm quan

Cht lng trong, khng mu, d chy, c mi c trng

4. Chc nng

Dung mi chit

5. Yu cu k thut
5.1. nh tnh
tan

Khng tan trong nc, trn ln c vi ethanol v ether

Trng lng ring

0,776 - 0,780

5.2. tinh khit

Khong nhit chng ct

80oC - 82oC

Cn khng bay hi

Khng c qu 1 mg/100 ml

Lu hunh

Khng c qu 10 mg/kg

Benzen

Khng c qu 0,1% (tt/tt)

Hydrocarbon thm a vng

hp th trn 1 cm chiu di ng quang khng c

vt qu cc gi tr trong bng sau
Bc sng (nm)

hp th

280 - 289

0,15

290 - 299

0,12

300 - 359

0,08

360 - 400

0,02

Ch

Khng c qu 2 mg/kg

5.3. Hm lng C6H12

Khng thp hn 99,5% (kl/kl)

6. Phng php th
6.1. Th nh tnh
tan

TCVN 6469:2010

Trng lng ring

TCVN 6469:2010

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61

6.2. Th tinh khit

Khong nhit chng ct

TCVN 6469:2010

Cn khng bay hi

TCVN 8900-2:2012

Lu hunh

JECFA monograph 1 - Vol.4

Benzen

JECFA monograph 1 - Vol.4 (Phn xc nh hydrocacbon

thm)

Hydrocarbon thm a vng

JECFA monograph 1 - Vol.4

Ch

TCVN 8900-6:2012
TCVN 8900-7:2012
TCVN 8900-8:2012

6.3. Th nh lng

Thc hin theo hng dn ti JECFA monograph 1-Vol.4

phn Phng php sc k kh xc nh hydrocarbon
thm a vng v tnh hm lng bng phng php
phn trm din tch (phng php chun ha din tch).

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Ph lc 6
YU CU K THUT V PHNG PHP TH I VI DIETHYL ETHER

1. Tn khc, ch s

Ether, ethyl ether

2. nh ngha

Diethyl ether thng c cha cc cht n nh nh pyrogallol

hoc BHT. Cc nh sn xut cn ghi r trn nhn cc cht
n nh c s dng v lng thm vo. Hm lng
ph bin l t 3 n 7 mg/l.

Tn ha hc

Diethyl ether; diethyl oxyd; 1,1-oxybisetan.

M s C.A.S

60-29-7

Cng thc ha hc

C4H10O

Cng thc cu to

Khi lng phn t

74,12

3. Cm quan

Cht lng linh ng, trong, khng mu, rt d bay hi v

d chy, c mi c trng

4. Chc nng

Dung mi chit

5. Yu cu k thut
5.1. nh tnh
tan

Khng tan trong nc, trn ln c vi ethanol

Trng lng ring

0,714 - 0,716

5.2. tinh khit

Khong nhit chng ct 34oC - 35oC
Cn khng bay hi

Khng c qu 2 mg/100 ml

Nc

Khng c qu 0,2%

acid

t yu cu trong phn phng php th

Aldehyd v keton

t yu cu trong phn phng php th

Peroxyd

t yu cu trong phn phng php th

Ch

Khng c qu 2 mg/kg

6. Phng php th

Phi th peroxyd trc khi tin hnh th cc ch tiu khc.

Cnh bo nguy him khi trng ct hoc ha hi Diethyl
ether m khng kim tra peroxyd.

6.1. Th nh tnh
tan

TCVN 6469:2010

Trng lng ring

TCVN 6469:2010

CNG BO/S 1217 + 1218/Ngy 23-12-2015

63

6.2. Th tinh khit

Khong nhit chng ct TCVN 6469:2010
Cn khng bay hi

TCVN 8900-2:2012

Nc

TCVN 8900-1:2012

acid

Ly 20 ml ethanol 95% vo ng ong chia vch c np

dung tch 50 ml, thm 0,5 ml dung dch th phenolphthalein
v va natri hydroxyd 0,02 N to thnh mu hng
bn sau khi lc mnh trong 30 giy. Thm 0,3 ml natri
hydroxyd 0,02 N na v 25 ml mu, y np ng ong,
trn v lc mnh trong 30 giy. Mu hng khng bin mt.

Aldehyd v keton

Ly 2 ml thuc th dung dch th Nesslers vo ng

nghim c np dung tch 12 ml v ng knh khong
1,5 cm; thm mu th n y ng. y np, lc mnh
trong 10 giy v n nh ch ti trong 5 pht. Nu
khng c mu v vn c to thnh, mu c xem l
t yu cu. Nu c mu hoc vn c v mu th t
yu cu php th peroxid th thc hin ct mu bng ct
ct phn on v lp li php th. Khng c c mu
hoc vn c to thnh.

Peroxyd

Mu ca iod t do to thnh di tc dng ca cc

peroxyd hu c vi kali iod c so vi mu ca dung
dch chun iod. Ly 8 ml dung dch kali iod 10% vo ng
nghim c np dung tch 12 ml v ng knh khong
1,5 cm. Thm mu th n y ngp ng, y np sao
cho khng c bt kh to thnh, lc mnh v yn
ch ti trong 30 pht. Nu c mu vng c to thnh
th khng c m hn mu ca 0,5 ml dung dch iod
0,001 N pha long vi 8 ml dung dch kali iod.

Ch

TCVN 8900-6:2012
TCVN 8900-7:2012
TCVN 8900-8:2012

64

CNG BO/S 1217 + 1218/Ngy 23-12-2015

Ph lc 7
YU CU K THUT V PHNG PHP TH I VI ETHYL ACETAT

1. Tn khc, ch s

Acetic acid ethyl ester, ethyl ethanoate

2. nh ngha
Tn ha hc

Ethyl acetat

M s C.A.S

141-78-6

Cng thc ha hc

C4H8O2

Cng thc cu to

Khi lng phn t

88,11

3. Cm quan

Cht lng trong sut, khng mu, c mi qu

4. Chc nng

Dung mi mang, cht to hng

5. Yu cu k thut
5.1. nh tnh
Ch s khc x

n20D: 1,371 - 1,376

Trng lng ring

d2525: 0,894 - 0,901

Ch s acid

Khng c ln hn 5,0

im si

77oC

5.2. Hm lng C4H8O2

Khng thp hn 99,0%

6. Phng php th
6.1. Th nh tnh
Ch s khc x

TCVN 6469:2010

Trng lng ring

TCVN 6469:2010

Ch s acid

TCVN 6471:2010

im si

TCVN 6469:2010

6.2. Th nh lng

Cn chnh xc 1,5 g mu vo l c np c cn tr
b; chuyn vo bnh thch hp v thm 50,0 ml natri
hydroxyd 0,5 N; un hi lu trn b cch thy trong 1 gi.
ngui, thm dung dch th phenolphthalein v chun
lng natri hydroxyd d bng acid hydrochloric 0,5 N.
Thc hin phn tch mu trng v hiu chnh kt qu theo
mu trng. Mi ml dung dch natri hydroxyd 0,5 N tng
ng vi 44,06 mg C4H8O2.

CNG BO/S 1217 + 1218/Ngy 23-12-2015

65

Ph lc 8
YU CU K THUT V PHNG PHP TH I VI ETHER DU HA
1. Tn khc, ch s

Petroleum spirits, petroleum ether

2. nh ngha

Phn du nh c si t 25oC n 105oC. Hn hp

hydrocarbon loi paraffinic (normal v iso) vi loi
cycloparaffinic.
ADI 0-5 mg/kg th trng

3. Cm quan

Cht lng linh hot, trong, khng mu, d chy, c mi du

c trng

4. Chc nng

Dung mi chit

5. Yu cu k thut
5.1. nh tnh
tan

Khng tan trong nc, tan trong ethanol

5.2. tinh khit

Cn khng bay hi

Khng c qu 2 mg/100 ml

Lu hunh

Khng c qu 10 mg/kg

Benzen

Khng c qu 0,05% (tt/tt)

Hydrocarbon thm

Khng c qu 0,3% (tt/tt) (gm c benzen)

Hydrocarbon thm a vng Mu phi p ng cc yu cu sau v gii hn hp th

Bc sng (nm) hp th cc i/1cm (chiu di quang)
280-289

0,15

290-299

0,12

300-359

0,08

360-400

0,02

Ch s brom

Khng c qu 200

Ch

Khng c qu 2 mg/kg

6. Phng php th
6.1. Th nh tnh
tan

TCVN 6469:2010

5.2. Th tinh khit

Cn khng bay hi

TCVN 8900-2:2012

Lu hunh

JECFA monograph 1-Vol.4

Benzen

JECFA monograph 1-Vol.4 phn xc nh hydrocarbon thm

Hydrocarbon thm

JECFA monograph 1-Vol.4 phn xc nh hydrocarbon thm

Hydrocarbon thm a vng JECFA monograph 1-Vol.4

66
Ch s brom

CNG BO/S 1217 + 1218/Ngy 23-12-2015

Nguyn tc
Chun mt lng mu bit ha tan trong dung
mi ph hp bng dung dch chun bromat-bromid. Xc
nh im kt thc bng my chun in th, s c
mt ca brom d to nn s thay i dn in ca
my. Ch s brom l s mg brom phn ng vi 100 g
mu di cc iu kin th ny.
Thit b, dng c
- My chun in th t ng: Bt k thit b t xc
nh im un no cng c th s dng nu p ng
dng in th ti in cc duy tr xp x 0,8V qua hai
in cc platin v c nhy tng ng s thay i
in th xp x 50 mV ti cc in cc ny cn xc
nh im kt thc.
- Bnh chun : Bnh thy tinh c bc kn, dung tch
khong 150 ml c th duy tr nhit t 1oC - 5oC. Hai
in cc platin khng t xa nhau qu 5 mm, cn t
sao cho u nm di lp cht lng. Cn khuy bng
my khuy in t hoc c hc tc nhanh nhng
khng qu mnh gy ra bt kh pha di in cc.
- Buret: Dung tch 10 ml v 50 ml
- Bnh s iod: C np y, dung tch 500 ml
Thuc th
Dung dch bromide-bromat 0,05 N: Ha tan 5,1 g kali bromide
v 1,4 g kali bromat trong nc v pha long n 1,000 ml.
Hiu chun n 4 ch s c ngha nh sau: Ly 50 ml
acid acetic v 1 ml dung dch th acid hydrochloric vo bnh
s iod 500 ml. Ngm bnh trong nc khong 10 pht,
v va lc va thm 40 - 50 ml dung dch bromide-bromat
t buret 50 ml (c n 0,01 ml) vi tc sao cho tng
thi gian thm khong t 90-120 giy. y ngay np
bnh, lc v t vo b nc , thm 5 ml dung dch
kali iod 15% vo ming bnh. Sau 5 pht, ly bnh ra khi
b nc v dung dch kali iod 15% chy vo bnh
bng cch m np bnh t t. Lc mnh, thm 100 ml
nc ra np, ming bnh v thnh bnh; chun
bng dung dch natri thiosulfat 0,05 N. Khi gn n im
kt thc, cho thm tinh bt v chun chm n khi
mu xanh bin mt.
Tnh ton nng ng lng ca dung dch bromidebromat nh sau:
N1 =

A 2N2
A1

CNG BO/S 1217 + 1218/Ngy 23-12-2015

Ch

67

Trong :
N1 = nng ng lng ca dung dch bromide-bromat
A1 = th tch (ml) dung dch bromide-bromat
N2 = nng ng lng ca dung dch Na2S2O3
A2 = th tch (ml) dung dch Na2S2O3 cn chun
dung dch bromide-bromat.
- Dung mi chun : chun b 1000 ml dung mi chun
bng cch trn cc cht sau: acid acetic bng (714 ml),
carbon tetrachloride (134 ml), methanol (134 ml), v acid
sulfuric (18 ml ca dung dch 1+5)
Tin hnh
Bt my chun v n nh th theo hng dn
ca nh sn xut. Lm lnh bnh chun v 0oC - 5oC
bng cch thi mt cht lm lnh vo bnh chun
c bc kn. Thm 110 ml dung mi chun v t 8 g
n 10 g mu. Bt my khuy v iu chnh tc
khuy nhanh nhng khng qu nhanh dn n to thnh
bt kh trong dung dch. Lm lnh mu v 0oC - 5oC v
duy tr nhit ny trong qu trnh chun . Thm dung
dch bromide-bromat tng lng nh t buret 10 ml n
khi c tn hiu sp n im kt thc (mt thn hoc
my o th). Tip tc thm 0,1 ml thuc th ngay khi
detector cho thy t c im kt thc n nh (im
kt thc ko di trong 30 giy). Lp li php xc nh nhng
khng cho thm mu; khng c mt qu 0,1 ml dung
dch bromid-bromat.
Tnh kt qu
Tnh ch s brom theo cng thc
(T T ) xNx 7990
Ch s brom = 1 2
W
Trong
T1 = s ml dung dch bromide-bromat cn chun
mu th
T2 = s ml dung dch bromide-bromat cn chun
mu trng
N = nng ng lng ca dung dch bromide-bromat
W = khi lng mu (g)
TCVN 8900-6:2012
TCVN 8900-7:2012
TCVN 8900-8:2012

68

CNG BO/S 1217 + 1218/Ngy 23-12-2015

Ph lc 9
YU CU K THUT V PHNG PHP TH I VI TOLUEN

1. Tn khc, ch s

Toluol, phenylmethane

2. nh ngha
Tn ha hc

Toluen, methylbenzene

M s C.A.S

108-88-3

Cng thc ha hc

C7H8

Cng thc cu to

Khi lng phn t

92,13

3. Cm quan

Cht lng trong, khng mu, c mi c trng

4. Chc nng

Dung mi chit

5. Yu cu k thut
5.1. nh tnh
tan

Rt t trn ln vi nc; trn ln c vi ethanol

Trng lng ring

0,864 - 0,870

5.2. tinh khit

Khong nhit chng ct T 110,6oC n 111,6oC
Mu

Khng m hn mu chun s 20

Cn khng bay hi

Khng c qu 5 mg/100 ml

Cc cht lu hunh

t yu cu trong phn phng php th

Cc hp cht khng c Khng c qu 0,2% (tt/tt)

vng thm
Benzen

Khng c qu 0,5% (tt/tt)

Ch

Khng c qu 2 mg/kg

5.3. Hm lng C7H8

Khng thp hn 99,0%

6. Phng php th
6.1. Th nh tnh
tan

TCVN 6469:2010

Trng lng ring

TCVN 6469:2010

6.2. Th tinh khit

Khong nhit chng ct TCVN 6469:2010

CNG BO/S 1217 + 1218/Ngy 23-12-2015

69

Mu

JECFA monograph 1-Vol.4

Cn khng bay hi

TCVN 8900-2:2012

Cc cht lu hunh

Phi m tnh vi hydro sulfua v sulfua dioxyd xc nh

bi php th sau
Thuc th
- Dung dch ch acetat (bo ha)
- Dung dch kali iodat (10 g KIO3/100 ml)
- Giy tinh bt: Nhng ming giy lc vo dung dch h
tinh bt v kh
Tin hnh
Thc hin nh tnh hydro sulfua (H2S) v sulfua dioxid
(SO2) ti thi im thc hin php th chng ct. t
ming giy lc lm m bng dung dch ch acetat v
ming giy tinh bt lm m bng dung dch kali iod
trn bnh ngng t. Cc ming giy lc c t pha
trn bnh hng sao cho git ngng t chy gia hai
ming m khng chm vo chng. Sau khi kt thc php
th, nu giy ch acetat mt mu th c H2S nhng
khng c SO2. Nu giy ch acetat khng mt mu nhng
giy tinh bt iod c mu xanh th c SO2 nhng khng c
H2S. Nu c hai loi giy u khng i mu th khng
c H2S v SO2.

Cc hp cht khng c Xc nh theo hng dn ti JECFA monograph 1-Vol.4

vng thm
phn xc nh hydrocarbon thm v tnh cc cht khng
c vng thm bng phng php phn trm din tch
(chun ha din tch)
Benzen

Xc nh theo hng dn ti JECFA monograph 1-Vol.4

phn xc nh hydrocarbon thm

Ch

TCVN 8900-6:2012
TCVN 8900-7:2012
TCVN 8900-8:2012

6.3. Th nh lng

JECFA monograph 1-Vol.4

70

CNG BO/S 1217 + 1218/Ngy 23-12-2015

Ph lc 10
YU CU K THUT V PHNG PHP TH I VI BENZYL ALCOL

1. Tn khc, ch s

Phenylcarbinol; Phenylmethyl alcohol; Benzenemethanol;

Anpha-hydroxytoluene
INS 1519

2. nh ngha
Tn ha hc

Benzyl alcol, Phenylmethanol

M s C.A.S

100-51-6

Cng thc ha hc

C7H8O

Cng thc cu to

Khi lng phn t

108,14

3. Cm quan

Cht lng trong, khng mu, c mi thm nh c trng

4. Chc nng

Cht to hng, cht mang

5. Yu cu k thut
5.1. nh tnh
tan

Tan trong nc, cn v ete

Ch s khc x

n20D: 1,538-1,541

Trng lng ring

d2525: 1,042-1,047

Hp th hng ngoi

t yu cu m t trong phn phng php th

5.2. tinh khit

Khong chng ct

Khng thp hn 95% (tt/tt) ct trong khong nhit t 202oC

n 208oC

Ch

Khng c qu 2 mg/kg

Ch s acid

Khng c qu 0,5

Aldehyd

Khng c qu 0,2% (tt/tt) (tnh theo benzaldehyd)

Peroxyd

t yu cu m t trong phn phng php th

Cc hp cht hu c t yu cu m t trong phn phng php th

clor ha
5.2. Hm lng C7H8O

Khng thp hn 98,0%

CNG BO/S 1217 + 1218/Ngy 23-12-2015

71

6. Phng php th
6.1. Th nh tnh
tan

TCVN 6469:2010
TCVN 6471:2010

Ch s khc x

TCVN 6469:2010

Trng lng ring

TCVN 6469:2010

Hp th hng ngoi

Ph hng ngoi ca mu th phi ph hp vi ph hng

ngoi chun

6.2. Th tinh khit

Khong chng ct

TCVN 6469:2010

Ch

TCVN 8900-6:2012
TCVN 8900-7:2012
TCVN 8900-8:2012

Ch s acid

TCVN 6471:2010

Aldehyd

Ly 2 ml mu vo bnh nh mc 100 ml, nh mc n

vch bng nc ct. Lc u cho tan. Chun b ng thi
mu i chng bng cch thay 2 ml dung dch mu bng 2 ml
dung dch Benzaldehyd 0,2% (mi pha).
Ly vo 2 ng nghim:
ng i chng: 2 ml dung dch mu i chng,
ng th: 2 ml dung dch mu th,
Thm vo c 2 ng 3 ml nc ct v 0,5 ml dung dch
Dinitrophenylhydrazyl bo ha trong acid Hydrochloric
long, y np ng nghim, lc u v yn trong 10 pht;
sau thm 5 ml ethanol 95% v 2 ml dung dch KOH 10%
v lc u n ng nht.
Mu nu (nu c) trong ng th khng c m hn
mu trong ng chng.

72

CNG BO/S 1217 + 1218/Ngy 23-12-2015

Peroxyd

Thi CO2 ( ui kh) vo bnh cu dung tch 100 ml gn

vi sinh hn kh. Thm 1 ml mu th, 2 ml chloroform, 0,1 g
Kali iodid v 20 ml hn hp dung dch chloroform v acid
acetic bng (t l 1:2 tt/tt). Lp sinh hn vo bnh cu, un
nh cho n khi bt u si trong 30 giy, gi nhit
dung dch tip tc si trong chnh xc 30 giy k t lc xut
hin hi trong sinh hn. Ngng un v lm mt ngay trong
nc , sau thm qua sinh hn 40 ml nc ct loi CO2.
Chun Iod t do bng dung dch Natri thiosulphat 0,005 N.
Ghi th tch Natri thiosulphat s dng l Vm. Tin hnh
tng t i vi mu trng (khng c mu th), ghi th tch
Natri thiosulphat s dng l Vt.
Mc chnh lch Vm - Vt khng c qu 1 (tng ng
vi 40 mg peroxyd/lt, tnh dng ng lng oxy).

Cc hp cht hu c Th theo JECFA monograph 1-Vol.4

clor ha
6.3. Th nh lng

Cn khong 1 g mu (chnh xc n mg), tin hnh theo

hng dn trong chuyn lun Hydroxyl value ti JECFA
monograph 1-Vol.4. Hm lng benzyl alcohol tnh theo
cng thc:
(B +
% w/w =

S) X N X 10.814

Trong :
A l th tch dung dch KOH chun acid t do (ml);
B l th tch dung dch KOH chun mu trng thuc
th (ml);
C l khi lng mu xc nh acid t do;
S l th tch dung dch KOH chun mu acetyl ha;
W l khi lng mu c s dng acetyl ha;
N l nng ng lng dung dch KOH trong ethanol.

CNG BO/S 1217 + 1218/Ngy 23-12-2015

73

Ph lc 11
YU CU K THUT V PHNG PHP TH I VI BUTAN-2-OL
1. Tn khc, ch s

Secondary butyl alcohol, 2-hydroxybutane

2. nh ngha
Tn ha hc

2-Butanol, butan-2-ol

M s C.A.S

78-92-2

Cng thc ha hc

C4H10O

Cng thc cu to

Khi lng phn t

74,12

3. Cm quan

Cht lng trong, hi nht, khng mu, d bt la, c mi thm

c trng.

4. Chc nng

Dung mi chit, cht to hng

5. Yu cu k thut
5.1. nh tnh
tan

D tan trong nc; c th trn ln vi ethanol v ether

Trng lng ring

0,806 - 0,809

5.2. tinh khit

Khong chng ct

t 98,5oC n 100,5oC

Cn khng bay hi

Khng c qu 2 mg/100 ml

Nc

Khng c qu 0,2% kl/kl

acid

Khng c qu 0,003% kl/kl (tnh theo acid acetic)

Andehyd v keton

Khng c qu 0,3% kl/kl (tnh theo butanal)

Ch

Khng c qu 2,0 mg/kg

6. Phng php th
6.1. Th nh tnh
tan

TCVN 6469:2010

Trng lng ring

TCVN 6469:2010

5.2. tinh khit

Khong chng ct

TCVN 6469:2010

Cn khng bay hi

TCVN 8900-2:2012

Nc

TCVN 8900-1:2012

74

CNG BO/S 1217 + 1218/Ngy 23-12-2015

acid

Ly 60 g mu, nh vi git dung dch th phenolphthalein

v chun bng KOH 0,1N cho ti khi xut hin mu
hng bn trong 15 giy. Lng KOH khng c qu 0,3 ml.

Andehyd v keton

- Th theo hng dn ti JECFA monograph 1-Vol.4.

- Dng 10 g mu vi h s tng ng l 36,06.

Ch

TCVN 8900-6:2012
TCVN 8900-7:2012
TCVN 8900-8:2012

CNG BO/S 1217 + 1218/Ngy 23-12-2015

75

Ph lc 12
YU CU K THUT V PHNG PHP TH I VI DICLOROMETHAN
1. Tn khc, ch s
2. nh ngha

Methylene chloride, Methylene dichloride

Dicloromethan (DCM) l sn phm ca qu trnh clo ha
methan, trong qu trnh ny c th cho cc sn phm clo
ha methan khc. n nh qu trnh tng hp, c th
s dng propylen oxid, cyclohexan, v/hoc 2-methyl-2-buten.
tinh khit ph thuc vo lng C2 v hydrocacbon
mch di hn ln trong methan v qu trnh clo ha. Do
c th c lng nh cc hp cht clo ha khc. Dicloro methan
thng thng s c thu hi t cc qu trnh chit v c
nhiu loi vi cht lng khc nhau. Dicloromethan bn
trong iu kin kh nhng s b thy phn nu c nc.

Tn ha hc

Dicloromethan

M s C.A.S

75-09-2

Cng thc ha hc

CH2Cl2

Cng thc cu to

Khi lng phn t

84,93

3. Cm quan

Cht lng trong, khng mu, khng chy

4. Chc nng

Dung mi chit

5. Yu cu k thut
5.1. nh tnh
tan

t tan trong nc, c th trn ln vi ethanol v ether

Ch s khc x

n20D: 1,423 - 1,425

Trng lng ring

d2525: 1,323 - 1,327

5.2. tinh khit

Nc

Khng c qu 0,02%

Khong chng ct

t 39oC t 41oC

Cn khng bay hi

Khng c qu 2 mg/100 ml

Clor t do

t yu cu m t trong phn phng php th

acid

Khng c qu 0,002% (kl/kl) (tnh theo HCl)

kim

Khng c qu 0,01% (kl/kl) (tnh theo NaOH)

Ch

Khng c qu 1 mg/kg

5.3. Hm lng CH2Cl2 Khng thp hn 99,0%

76

CNG BO/S 1217 + 1218/Ngy 23-12-2015

6. Phng php th
6.1. Th nh tnh
tan

TCVN 6469:2010

Ch s khc x

TCVN 6469:2010

Trng lng ring

TCVN 6469:2010

6.2. Th tinh khit

Nc

TCVN 8900-1:2012

Khong chng ct

TCVN 6469:2010

Cn khng bay hi

TCVN 8900-2:2012

Clor t do

Ly 10 ml mu, thm 10 ml dung dch Kali iodid 10% v 1 ml

dung dch th h tinh bt, lc u trong 2 pht. tch
lp, lp nc khng c c mu xanh.

acid

Ly 100 ml nc ct mi un si ngui ( c trung

ha vi thuc th phenolphthalein) vo bnh nn nt mi
dung tch 500 ml. Thm 100 ml dung dch mu v lc u.
tch lp, ly pha nc vo mt bnh nn, thm 0,5 ml
dung dch th phenolphthalein v chun bng dung
dch Natri hydroxyd 0,1 N cho n khi dung dch c mu
hng bn. Tnh hm lng (%, kl/kl) acid trong mu th
theo acid hydrochloric. 1 ml dung dch NaOH 0,1 N tng
ng vi 0,00365 g HCl.

kim

Ly 100 ml nc ct mi un si ngui ( c trung

ha vi thuc th phenolphthalein) vo bnh nn nt mi
dung tch 500 ml. Thm 100 ml dung dch mu v lc u.
tch lp, ly pha nc vo mt bnh nn, thm 0,5 ml
dung dch th phenolphthalein v chun bng dung
dch acid hydrochloric 0,1 N cho n khi dung dch c mu
hng bn. Tnh hm lng (%, kl/kl) kim trong mu th
theo natri hydroxyd. 1 ml dung dch HCl 0,1 N tng ng
vi 0,004 g NaOH.

Ch

TCVN 8900-6:2012
TCVN 8900-7:2012
TCVN 8900-8:2012

5.3. Th nh lng

Nguyn l:
Mu th c phn tch trn h thng sc k kh s dng
ct mao qun v detector FID. nh lng diclomethan,
cc tp cht v cc cht n nh bng phng php so snh
din tch pic vi cht ngoi chun.

CNG BO/S 1217 + 1218/Ngy 23-12-2015

77

Thit b:
H thng sc k kh s dng ct mao qun (di 25 m,
ng knh trong 0,53 mm, lp pha tnh dy 2 m 5%
phenyl/95% methylsilicon hoc ct di 30 m, ng knh
trong 0,32 mm, lp pha tnh 1,8 m 6% cyanoproyl-phenyl/
methylpolysiloxan) v detector FID c b phn bm mu
chia dng v khng chia dng.
iu kin thit b:
Nhit bung bm mu: 150oC
Nhit Detector: 250oC
Nhit l: 40oC, ng nhit
Kh mang: He, tc 4,4 ml/pht
Chia dng: 98 ml/pht
Chun:
Pha dung dch chun bng cch thm cc cht vi t l
nh sau:
Methyl clorid: 0,014% (kl/kl)
Vinyl clorid: 0,007
Ethyl clorid: 0,0084
Propylen oxid: 2,4
Vinyliden clorid: 0,0098
Trans-1,2-Dicloroethylen: 0,017
Cloroform: 0,012
Cyclohexan: 0,047
2-methyl-2-buten: 0,009
vo DCM siu tinh khit. ng trong l thy tinh c nt
cao su (septum) kn. Cc cht c ly bng syranh, cn
(chnh xc n mg). Bm vo l cha DCM qua septum
sau cn syranh cn li xc nh lng cht pha.
DCM pha chun phi c kim tra tp cht trc khi
s dng.
Tin hnh:
Dung dch chun c pha long thnh dy cc dung dch
chun lm vic t 10 n 300 ppm (mg/kg), ring propylen
oxid c pha thnh dy t 0,06 n 2,4% (kl/kl). Dung
dch chun v dung dch mu c bm vo h thng sc
k kh, th tch mu ty chn t 1 n 5 l (s dng ch

78

CNG BO/S 1217 + 1218/Ngy 23-12-2015

bm mu chia dng). Xy dng ng chun biu th mi
tng quan gia din tch pic v nng cht cn phn
tch. Nng cc ph gia v sn phm ph c xc nh
bng cch so snh vi ng chun. Tng nng cc
cht n nh v tp cht phi thp hn 1,0%. Th t ra gii
v thi gian lu:
Methyl clorid: 2,8
Vinyl clorid: 3,0
Ethyl clorid: 3,5
Propylen oxyd: 4,1
2-methyl-2-buten: 4,5
Vinyliden clorid: 4,6
Dichloromethan: 5,3
Trans-1,2-Dicloroethylen: 5,9
Cloroform: 8,7
Cyclohexan: 10,5
Cacbon tetraclorid: 12,0

CNG BO/S 1217 + 1218/Ngy 23-12-2015

79

Ph lc 13
YU CU K THUT V PHNG PHP TH I VI CC HEXAN
1. Tn khc, ch s

Hexanes

2. nh ngha

Thut ng hexanes c s dng ch cc hydrocacbon

c 6 cacbon trong mch thu c t qu trnh cracking
du ha, thnh phn ch yu l n-hexan, 2-methylpentan,
3-methylpentan, ngoi ra cn c th ln lng nh n-pentan,
iso-pentan, cyclohexan, n-heptan, dimethylbutan v
methylcyclopentan.

Tn ha hc

Hexan

Cng thc ha hc

C6H14

Khi lng phn t

86,18

3. Cm quan

Cht lng trong, khng mu, d bt la, c mi c trng

ca du ha, khng c c cn v huyn ph

4. Chc nng

Dung mi chit

5. Yu cu k thut
5.1. nh tnh
tan

Khng tan trong nc, tan trong ether, cn v aceton

Ch s khc x

n20D: 1,381-1,384 (n-hexan tinh khit: khong 1,375)

Trng lng ring

d2020: 0,665 - 0,687 (n-hexan tinh khit: khong 0,660)

5.2. tinh khit

Khong chng ct

95% tt/tt ct ti 64oC n 70oC

pH

Trung tnh i vi ch th methyl da cam

Cn khng bay hi

Khng c qu 0,0005% kl/tt

Sulphur

Khng c qu 5,0 mg/kg

Benzen

Khng c qu 0,05% (tt/tt)

Ch

Khng c qu 1,0 mg/kg

Cc hydrocacbon thm t yu cu (m t trong phn phng php th)

a vng (PAHs)
6. Phng php th
6.1. Th nh tnh
tan

TCVN 6469:2010

Ch s khc x

TCVN 6469:2010

Trng lng ring

TCVN 6469:2010

6.2. Th tinh khit

Khong chng ct

TCVN 6469:2010

80

CNG BO/S 1217 + 1218/Ngy 23-12-2015

pH

TCVN 6469:2010

Cn khng bay hi

TCVN 8900-2:2012

Sulphur

JECFA monograph 1 - Vol.4

Benzen

Nguyn l:
Phng php ni b: cho methyl ethyl keton (MEK) vo
mu th hexan sau bm vo my sc k kh vi 2 ct
c ni bi mt van chia dng (theo hnh 1). Cho mu
th qua trc ct cha pha khng phn cc (ct A),
methyl silicon, tch cc hydrocacbon khng phn cc.
Sau khi octan c ra gii, dng mu c thi tip qua
ct cha pha phn cc cao (ct B). Cc thnh phn khng
c ra gii ct A s c chuyn sang ct B phn
tch cc hp cht thm v hp cht khng thm. Xc
nh cc thnh phn ra gii bng detector ion ha ngn
la v xy dng biu ct. Cc din tch pic c o v
nng mi cht c tnh bi phng php ni chun.

Thit b:
Dng sc k kh vi detector ion ha ngn la.
Ct A - Ct lm bng thp khng r, chiu di ct 0,8 m,
ng knh ngoi 3,2 mm, bc bng 10% methyl silicon,
c ht 60-80 mesh.
Ct B- Ct lm bng thp khng r, chiu di ct 4,6 m,
ng knh ngoi 3,2 mm, bc bng 25% 1,2,3-tris
(2-cyanoethoxy)propan (TCEP), c ht 80-100 mesh.

CNG BO/S 1217 + 1218/Ngy 23-12-2015

81

Ni ct A vi ct B (nh hnh 1), s dng van chia dng.

Thi kh Heli qua c hai ct vi tc xp x 40 ml/pht.
t van v tr ngc dng (backflush) v ci t tc
dng ct B l 40 ml/pht (hnh 2)

Vt liu v thuc th:

Methyl Ethyl Keton (MEK) > 99,9%
Benzen > 99%
Isooctan > 99%
n-Nonan > 99%
Hiu chun:
Xc nh thi gian cn thit trc khi thay i van, trong
s thay i h thng ct v iu kin thc nghim nh
sau: chun b mt hn hp gm 5% th tch isooctan trong
n-nonan. Vi h thng c m t nh hnh 2a, bm 1 l
hn hp isooctane, n-nonan v tin hnh ra gii. o thi
gian (theo giy) t khi bm n khi isooctan c ra gii
nhng n-nonan cha ra gii. Vn ngc van vo thi
im gn na thi gian ra gii ca isooctan. Tip tc qu
trnh chy, thu c mt ph ca isooctan vi mt t hoc
khng c n-nonan.
Chun ha:
Dung dch chun: chun b 7 dung dch chun benzen t 0
n 1% th tch trong bnh cu dung tch 100 ml, pha
long, nh mc bng isooctan n 100 ml thu c dy
dung dch chun vi hm lng benzen nh sau:

82

CNG BO/S 1217 + 1218/Ngy 23-12-2015

% Th tch

ml

0,5

0,5

0,25

0,25

0,1

0,1

0,05

0,05

0,01

0,01

0,005

0,005

Dung dch hiu chun: Ly chnh xc 0,5 ml dung dch MEK

vo bnh cu dung tch 100 ml, nh mc n vch bng
dung dch chun u tin v lc u. Lp li vi cc dung
dch chun khc. Phn tch sc k cc dung dch hiu
chun vi cc iu kin nh trn, mu bm khong 3 l.
Hiu chun: o din tch pic v tnh t l din tch pic ca
benzene v MEK. Lp ng chun nng ca benzene
so vi t l din tch pic thu c. ng hiu chun phi
thng. Xc nh thi gian lu ca mi thnh phn cn xc
nh trong mu th.
Tin hnh:
Dung dch th: Ly chnh xc 0,5 ml MEK vo bnh nh
mc dung tch 100 ml. nh mc n vch bng mu th
v lc u. o ph mu i din t dung dch th. Nhn
bit cc pic ca benzene v chun MEK t thi gian lu
cc pic ca dung dch chun. Th t ra gii l cc
hydrocacbon khng thm, benzene, MEK v toluen. o din
tch pic ca benzene v MEK.
Tnh ton:
Xc nh t l din tch pic ca benzen v MEK. c t
ng cong hiu chun% th tch pic ca benzen tng
ng vi t l din tch pic xc nh. Nu tnh kt qu
theo khi lng, chuyn i thnh % khi lng theo cng
thc sau:
% Khi lng benzen = V/D * 0,8844
Trong :
V l% th tch benzen,
D l t khi ca mu ti 15,6oC, theo th tch hoc % khi
lng bezen gn mc 0,005%.

CNG BO/S 1217 + 1218/Ngy 23-12-2015

Ch

83

TCVN 8900-6:2012
TCVN 8900-7:2012
TCVN 8900-8:2012

Cc hydrocacbon thm Ly 25 ml mu cho vo phu chit 125 ml, thm 25 ml hexan

a vng (PAHs)
lc u v thm 5 ml dimethyl sulfoxid lc u trong 1 pht,
yn cho tch lp, chuyn lp di vo mt phu chit
khc, thm 2 ml hexan lc u v yn cho tch lp.
Tch ly lp pha di v o hp th quang t 260 nm
n 420 nm. Thm 5 ml dimethyl sulfoxyd, 25 ml hexan,
lc u trong 1 pht. Chun b dung dch phn tch
trimethyl pentan cha 7,0 mg naphtalen (trn lt) v o
hp ph ca dung dch ti bc sng 275 nm, s dng
trimethylpentan lm mu trng. Ti khong bc sng t
260 nm n 420 nm, hp ph ca dung dch th bng
1/3 dung dch phn tch ti 275 nm.
S dng hexan, dimethyl sulfoxyd v trimethylpentan cht
lng phn tch cho ph t ngoi.