QCVN 4-20:2010/BYT

V PH GIA THC PHM - CHT LM BNG

National technical regulation on Food Additive Glazing agent

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 cht lng, v sinh an ton i vi cc cht lm bng c s dng
vi mc ch lm ph gia thc phm.
2. i tng p dng
Quy chun ny p dng i vi:
2.1. T chc, c nhn nhp khu, xut khu, sn xut, bun bn v s dng cc
cht lm bng lm ph gia thc phm (sau y gi tt l t chc, c nhn).
2.2. C quan qun l nh nc c lin quan.
3. Gii thch t ng v ch vit tt:
3.1. Cht lm bng: l ph gia thc phm c cho thm vo b mt pha
ngoi ca thc phm nhm to bng hoc to lp bo v.
3.2. JECFA monograph 1 - Vol. 4 (JECFA monographs 1 - Combined
compendium of food additive specifications; Joint FAO/WHO expert committee on
food additives; Volume 4 - Analytical methods, test procedures and laboratory
solutions used by and referenced in the food additive specifications; FAO, 2006): 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.
3.3. M s C.A.S (Chemical Abstracts Service): M s ng k ha cht ca
Hip hi Ha cht Hoa K.
3.4. TS (test solution): Dung dch thuc th.
3.5. ADI (Acceptable daily intake): Lng n vo hng ngy chp nhn c.
3.6. INS (International numbering system): H thng m s quc t v ph gia
thc phm.

QCVN 4-20:2010/BYT
II. YU CU K THUT, PHNG PHP TH V LY MU
1. Yu cu k thut v phng php th i vi cc cht lm bng c quy
nh ti cc ph lc ban hnh km theo Quy chun ny nh sau:
1.1.
1.2.

Ph lc 1:
Ph lc 2:

1.3.
1.4.

Ph lc 3:
Ph lc 4:

1.5.

Ph lc 5:

Yu cu k thut v phng php th i vi sp ong

Yu cu k thut v phng php th i vi sp
Candelila
Yu cu k thut v phng php th i vi Shellac
Yu cu k thut v phng php th i vi du
khong
Yu cu k thut v phng php th i vi sp vi
tinh th

2. Cc yu cu k thut quy nh trong Quy chun ny c th theo JECFA

monograph 1 - Vol. 4, ngoi tr mt s php th ring c m t trong cc ph lc.
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 tng ng.

3. Ly mu theo hng dn ti Thng t 16/2009/TT-BKHCN ngy 02 thng 6

nm 2009 ca B Khoa hc v Cng ngh v hng dn 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.
III. YU CU QUN L
1. Cng b hp quy
1.1. Cc cht lm bng 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 Quy
nh v chng nhn hp chun, chng nhn hp quy v cng b hp chun, cng
b hp quy ban hnh km theo Quyt nh s 24/2007/Q-BKHCN ngy 28 thng 9
nm 2007 ca B trng B Khoa hc v Cng ngh v cc quy nh ca php lut.
2. Kim tra i vi cht lm bng
Vic kim tra cht lng, v sinh an ton i vi cc cht lm bng phi thc
hin theo cc quy nh ca php lut.

QCVN 4-20:2010/BYT
IV. TRCH NHIM CA T CHC, C NHN
1. T chc, c nhn 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 nhp khu, xut khu, sn xut, bun bn v s dng
cc cht lm bng sau khi hon tt ng k bn cng b hp quy v bo m cht
lng, v sinh an ton, ghi nhn ph hp vi cc quy nh ca php lut.
V. 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.
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.

QCVN 4-20:2010/BYT
Ph lc 1
YU CU K THUT V PHNG PHP TH
I VI SP ONG
1. Tn khc, ch s

Beeswax
INS 901

2. nh ngha

Sp ong c ly t t ong mt (h Apidae, v d Apis

mellifera L) sau khi rt ht hoc ly tm ht mt ong. T
ong c lm chy vi nc nng, hi nc hoc phi
di nh mt tri, sau sn phm tan chy c lc v
ng thnh bnh sp ong vng. Sp ong trng thu c
bng cch ty trng sp ong vng dng cc cht oxy ha
nh hydro peroxyd, acid sulfuric, hay nh sng mt tri. Sp
ong l mt hn hp cc ester ca cc acid bo v cn bo,
cc hydrocarbon v acid bo t do, v c mt phn nh cc
cn bo t do.

M s C.A.S.

8006-40-4 (sp ong vng)

8012-89-3 (sp ong trng)

3. Cm quan

Sp ong vng: cht rn mu vng hoc nu sng, khi lnh

th d v, khi v to thnh ming m c, dng ht, khng
c dng tinh th, nhit khong 35C tr nn mm do.
C mi c trng ca mt ong.
Sp ong trng: cht rn mu trng hay mu trng ng (lp
mng thng trong m), c mi nh c trng ca mt ong.

4. Chc nng

Cht lm bng, cht gii phng, cht n nh, cht to kt

cu cho ko cao su, cht mang cho ph gia thc phm (bao
gm mang hng v mang mu), cht lm c.

5. Yu cu k thut
5.1. nh tnh
tan

Khng tan trong nc, t tan trong cn, rt d tan trong

ether.

5.2. tinh khit

Khong nng chy

62 65C

Ch s acid

17 24

Ch s peroxyd

Khng c qu 5,0. (xem m t trong phn Phng php

th)

Ch s x phng ha

87 104

Sp carnauba

t yu cu (xem m t trong phn phng php th)

Ceresin, parafin v mt t yu cu (xem m t trong phn phng php th).

s sp khc
Cht bo, sp Nht

t yu cu (xem m t trong phn phng php th).

4

QCVN 4-20:2010/BYT
bn, colophan v x
phng
Glycerin v cc polyol
khc

Khng c qu 0,5% (tnh theo glycerin)

Ch

Khng c qu 2,0 mg/kg.

(xem m t trong phn phng php th).

6. Phng php th
6.1. tinh khit
Ch s peroxyd

Cn chnh xc 5 g mu vo bnh nn 200 mL. Thm 30 mL

dung dch cloroform v acid acetic (TT) 2:3 v y nt bnh
nn. Lm nng mu trong nc m v xoy trn ha tan
mu. ngui n nhit phng v thm 0,5 mL dung dch
kali iodid bo ha. y bnh nn bng nt v lc mnh trong
60 5 giy. Thm 30 mL nc lc u v chun ngay
bng dung dch natri thiosulfat dng ch th h tinh bt (TT).
Tin hnh thm trn mt mu trng.

Ch s peroxyd =

(a b) N 1000
m

Trong :
a = s mL natri thiosulfat dng cho mu th
b = s mL natri thiosulfat dng cho mu trng
N = nng ng lng ca natri thiosulfat
m = khi lng mu (g)
Sp carnauba

Cn khong 100 mg mu th vo mt ng nghim, thm 20

mL n-butanol. Nhng ng nghim vo chu nc ang si,
lc hn hp nh nhng n khi mu th ha tan hon ton.
Chuyn mu trong ng nghim vo mt cc c m cha
nc 60C, v yn cho nc ngui xung nhit
phng. Mt khi xp cc tinh th mn ging hnh kim to
thnh, tch khi lp dung dch m trong sut. Di knh hin
vi, cc tinh th xp hnh kim hoc cc bi hnh sao, khng c
khi v nh hnh, chng t khng c sp carnauba.

Ceresin, parafin v mt Cn 3,0 g mu vo mt bnh cu y trn 100 mL, thm 30

mL dung dch kali hydroxyd 4% (kl/tt) trong ethanol khng
s loi sp khc
cha aldehyd v un nh di ng sinh hn hi lu trong 2
gi. Tho b ng sinh hn, nhng ngay vo mt nhit k.
Ngm bnh vo chu nc 80C v cho ngui, lin tc lc
xoy trn bnh. Khng c c kt ta trc khi nhit t
n 65C, mc d dung dch c th trng c.
Cht bo, sp Nht
bn, colophan v x
phng

un 1 g mu vi 35 mL dung dch natri hydroxyd 1:7 trong 30

pht, gi nguyn th tch bng cch thnh thong thm nc,
ri ngui hn hp. Sp s tch ra, v dung dch vn trong
5

QCVN 4-20:2010/BYT
sut. Lc hn hp lnh v acid ha dch lc bng acid
hydrocloric. Khng c kt ta to thnh.
Glycerin v cc polyol
khc

Cho 0,20 g mu vo mt bnh cu y trn, thm 10 mL dung

dch kali hydroxyd trong ethanol (TT), ni sinh hn hi lu v
un trong mt bnh cch thy trong 30 pht. Thm 50 mL acid
sulfuric long (TT), ngui v lc. Ra bnh v phu lc
bng acid sulfuric long (TT). Gp dch chit v dch ra, pha
long thnh 100,0 mL acid sulfuric long (TT). Ly 1,0 mL
dung dch vo mt ng nghim, thm 0,5 mL dung dch natri
periodat 1,07% (kl/tt) trong nc, lc u v yn trong 5
pht. Thm 1,0 mL dung dch fuchsin lm mt mu (xem
di), lc u. Kt ta phi tan ht. t ng vo mt cc c
m cha nc 40C. ngui, quan st trong khong 10
15 pht. Nu dung dch chuyn thnh mu tm xanh, mu
phi khng c m hn mu dung dch chun pha ng
thi theo cch tng t nhng dng 1,0 mL dung dch
glycerin 0,001% (kl/tt) trong acid sulfuric long (TT).
Dung dch fuchsin c kh mu

Ch

Ha tan 0,1 g fuchsin dng base trong 60 mL nc. Thm

dung dch gm 1 g natri sulfit khan (tinh khit thuc th) trong
10 mL nc. Thm t t 2 mL acid hydrocloric, va thm va
lc lin tc. Thm nc n 100 mL. yn, trnh nh
sng trong vng t nht 12 gi, loi mu bng than hot tnh
v lc. Nu dung dch tr nn c, lc trc khi dng. Nu
sau khi yn, dung dch chuyn sang mu tm, loi mu ln
na bng than hot tnh. Bo qun trnh nh sng.
- Th theo JECFA monograph 1 - Vol.4.
- Xc nh bng k thut quang ph hp th nguyn t thch
hp cho hm lng quy nh. La chn c mu th v
phng php chun b mu da trn nguyn tc ca phng
php m t trong JECFA monograph 1 - Vol.4 phn cc
phng php phn tch cng c.

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

INS 902

2. nh ngha

Sp candelilla th thu c bng cch un si cc nhnh

kh ca cy candelilla (Euphorbia antisyphilitica) trong nc
c acid ha bng acid sulfuric gii phng ra sp.
Sp tan chy ny sau c loi bo v cho ng c
li, tip theo c tinh ch bng cch x l vi acid sulfuric
v qua cc cng on p - lc.
Sp candelilla v c bn cha n-alkanes mch l (C 29 n
C33) vi cc ester ca cc acid v cc ru c mch carbon
chn (C28 n C34). Cc acid t do, ru t do, sterol, keo
trung tnh v cc cht khong cng c mt.
6

QCVN 4-20:2010/BYT
M s C.A.S.

8006-44-8

3. Cm quan

Dng cht rn, cng, rn, bng mu nu hi vng, c mi

thm khi lm nng.

4. Chc nng

Cht lm bng, cht to kt cu cho ko cao su, cht ph b

mt, cht mang cho ph gia thc phm (bao gm mang
hng v mang mu), cht lm c.

5. Yu cu k thut
5.1. nh tnh
Khng tan trong nc, tan trong toluen.

tan
hp th hng
ngoi

Ph hng ngoi ca mu th, c lm tan chy v

chun b phn tch trn mt tm kali bromid phi tng
ng vi ph hng ngoi ca sp candelilla tiu chun (xem
Ph lc).

5.2. tinh khit

Khong nhit tan
chy

68,50 72,50

Ch s acid

T 12 n 22

Ch s x phng ha

T 43 n 65.

Ch

Khng c qu 2 mg/kg.

6. Phng php th
tinh khit
- Th theo JECFA monograph 1 - Vol.4.
- Xc nh bng k thut quang ph hp th nguyn t thch
hp cho hm lng quy nh. La chn c mu th v
phng php chun b mu da trn nguyn tc ca
phng php m t trong JECFA monograph 1 - Vol.4 phn
cc phng php phn tch cng c.

Ch

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

INS 904

2. nh ngha

Senlac l nha polyester thu c t cnh kin , cht

nha tit ra t loi cn trng Laccifer (Tachardia) lacca Kerr
(H Coccidae). Senlac ty mu thu c nh qu trnh
ho tan cnh kin trong dung dch Na 2CO3 trong nc,
sau ty mu bng natri hypochlorit, kt ta cnh kin
ty mu bng dung dch H2SO4 long v sy kh; senlac
ty mu khng cha sp c iu ch bng cch x l
tip, theo sp c tch ra bng cch lc.

M s C.A.S

9000-59-3
7

QCVN 4-20:2010/BYT
3. Cm quan

Sellac ty mu: dng nha ht v nh hnh c mu

trng ti vng nht;
Senlac ty mu khng cha sp: dng nha ht v nh
hnh c mu vng sng.

4. Chc nng

Cht lm bng, cht ph b ngoi

QCVN 4-20:2010/BYT
5. Yu cu k thut
5.1. nh tnh
Phn ng mu

Phi c phn ng mu c trng.

tan

Khng tan trong nc; tan chm trong ethanol; t tan trong
aceton v ether.

Ch s acid

60 89 (xem m t trong phn Phng php th)

5.2. tinh khit

Gim khi lng khi
sy kh

Khng c qu 6,0 % (sy 400C trong 4 gi, sau

lm ngui n nhit phng trn silicagel trong 15 gi)

Rosin

t yu cu (xem m t trong phn Phng php th).

Sp

Senlac ty mu : khng c qu 5,5% ; Senlac ty

mu khng c sp: khng c qu 0,2%
(xem m t trong phn Phng php th)

Ch

Khng c qu 2,0 mg/kg.

6. Phng php th
6.1. nh tnh
Phn ng mu

Ch s acid

Cho vi git dung dch cha 1 g amoni molybdat trong 3

ml acid sulfuric vo 50 mg mu. Mu xanh l cy c
hnh thnh chuyn sang mu hoa c khi dung dch mu
c trung ho bng dung dch amoni hydroxyd 6N.
Cn chnh xc 1 g mu nghin mn v ho trong 50 ml
alcol trc c trung ho bng NaOH vi cht ch
th phenolphthalein, v chun bng dung dch KOH
0,1N. Xc nh im kt thc bng cch s dng
phenolphthalein TS hoc dng c o in th. Nu
phenolphthalein c dng, chun cho n khi mu
hng nht bn t nht trong 30 giy. Tnh ch s acid bng
cng thc:
Ch s acid = 56,1V x N/W
Trong :
V: Th tch dung dch NaOH (ml)
N: Nng dung dch NaOH
W: Khi lng mu (g) tnh theo cht kh.

6.2. tinh khit

QCVN 4-20:2010/BYT
Rosin

Ho tan 2 g mu trong 10 ml ethanol kh nc, v

thm t t 50 ml dung mi hexan va thm va lc.
Chuyn hn hp vo mt phu tch, ra 2 ln 50 ml nc
v loi b nc ra. Lc lp dung mi, c n kh v
thm 2 ml hn hp gm 1 phn th tch phenol lng v 2
phn th tch methylen chlorid vo phn cn kh va c
c. Khuy v chuyn mt phn hn hp vo h rng
ca a phn ng mu. Lm y h rng lin k bng hn
hp gm 1 phn th tch brom v 4 phn th tch methylen
clorid, y c hai h rng bng mt knh ng h. Khng
c mu ta hoc mu xanh indigo m c hnh thnh
trong hoc bn trn lp dch lng cha cn mu.

Sp

Cn chnh xc 10 g mu nghin mn v 2,5 g Na 2CO3

vo cc cao dung tch 200 ml. Thm vo 150 ml nc
nng, ngm cc trong cch thy si v khuy cho n khi
mu c ho tan. y cc bng mt knh ng h, gia
nhit trong 3 gi khng khuy, sau lm ngui trong
chu nc lnh. Khi sp ni ln b mt, lc hn hp qua
giy lc khng tro tc trung bnh, chuyn sp sang giy
v ra phu lc bng nc. Rt 5 -10 ml ethanol vo phu
lc lm kh nhanh. Gi giy vo mt t giy lc rng,
buc bng mt si dy nh v lm kh bng cch gia nhit
nh. Chit bng cloroform trong dng c chit xut lin tc
thch hp trong 2 gi, s dng bnh lm kh v cn
khi lng trc hng sp trch ly v dung mi. C
dung mi, lm kh sp 105 0C cho ti khi lng khng
i, tnh % sp.

Ch

- Th theo JECFA monograph 1 - Vol.4.

- Xc nh bng k thut quang ph hp th nguyn t
thch hp cho hm lng quy nh. La chn c mu th
v phng php chun b mu da trn nguyn tc ca
phng php m t trong JECFA monograph 1 - Vol.4
phn cc phng php phn tch cng c.
Ph lc 4

YU CU K THUT V PHNG PHP TH

I VI DU KHONG
1. Tn khc, ch s

2. nh ngha

Liquid parafin, liquid petrolatum, food grade mineral oil,

white mineral oil
INS 905a
Hn hp ca cc hydrocarbon lng naphthalin v parafin
tinh ch vi im si trn 350 0C; thu c t cc cng on
tinh ch du khong th khc nhau (v d: chng ct, trch
ly v kt tinh) v lm sch tip bng acid v/hoc x l
hydrogen ha c xc tc; c th cha cc cht chng oxy
ho c chp thun dng cho thc phm.

M s C.A.S

8012-95-1

3. Cm quan

Dng du lng khng mu, trong sut, pht ra hunh quang

10

QCVN 4-20:2010/BYT
di nh sng ban ngy; khng mi

11

QCVN 4-20:2010/BYT
4. Chc nng

Cht lm bng, cht chng dnh, cht bi trn, cht ph bo

v

5. Yu cu k thut
5.1. nh tnh
tan

Khng tan trong nc, t tan trong ethanol, tan trong ether

t chy

t chy to ra ngn la sng chi v c mi ging mi

parafin

5.2. tinh khit

nht 1000C

Khng nh hn 11 cSt

S carbon im
chng ct 5%

Khng nh hn 28
im si im chng ct 5% cao hn 4220C

Khi lng phn t

trung bnh

Khng nh hn 500

acid hoc kim

t yu cu.

Cc cht d than ho

t yu cu.

Hydrocarbon a vng
thm

t yu cu.

Parafin rn

t yu cu (xem m t trong phn Phng php th).

Ch

Khng c qu 1,0 mg/kg.

6. Phng php th
tinh khit
acid hoc kim

Cho 20 ml nc si vo 10 ml mu v lc mnh trong 1

pht. Tch lp dung dch nc v lc. Cho 0,1 ml dung dch
phenolphthalein TS vo 10 ml dung dch lc c. Dung
dch khng mu. Khng c qu 0,1 ml dung dch NaOH
0,1N thm vo thay i thnh mu hng.

Cc cht d dng than

ho

Cho 5 ml mu vo ng th c np thu tinh trc

c ra sch bng hn hp dch ra acid chromic. Thm
5 ml dung dch H2SO4 TS v gia nhit trong cch thy si
trong 10 pht. Sau khi ng th trong chu trong 30 giy,
ly ra nhanh v trong khi y np lc 3 ln tht mnh theo
phng thng ng vi bin 10 cm. Lp li sau mi t
30 giy. Khng c ng th ngoi cch thy qu 3 giy
cho mi ln lc. Kt thc sau 10 pht tnh t thi gian bt
u t ng th vo cch thy cho n khi ly ra khi cch
thy. Mu gi nguyn mu v acid khng tr nn sm mu
hn mu chun c chun b bng cch trn trong mt
ng th tng t 3 ml st (III) clorid TSC, 1,5 ml cobalt
clorid TSC v 0,5 ml CuSO 4, hn hp ny c ph bng 5
12

QCVN 4-20:2010/BYT
ml du khong bn trn.
Parafin rn

Ch

Lm kh lng mu thch hp bng cch gia nhit 100 0C

trong 2 gi v lm ngui trong bnh ht m trn acid H 2SO4
m c. Cho vo ng thu tinh c ng knh trong
khong 25 mm, y ng v ngm ng vo trong chu nc
. Sau 4 gi, cht lng to thnh phi trong c th
nhn thy d dng mt vch mu en rng 0,5 mm trn nn
trng gi thng ng pha sau ng thy tinh.
- Th theo JECFA monograph 1 - Vol.4.
- Xc nh bng k thut quang ph hp th nguyn t
thch hp cho hm lng quy nh. La chn c mu th
v phng php chun b mu da trn nguyn tc ca
phng php m t trong JECFA monograph 1 - Vol.4
phn cc phng php phn tch cng c.

13

QCVN 4-20:2010/BYT
Ph lc 5
YU CU K THUT V PHNG PHP TH
I VI SP VI TINH TH
1. Tn khc, ch s

Petroleum wax;
INS 905c

2. nh ngha

Sp vi tinh th l hn hp tinh ch ca cc hydrocarbon bo

ho, rn ch yu l parafin nhnh, thu c t du m.

3. Cm quan

Dng sp khng mu hoc trng, hi trong m, khng v v

khng mi

4. Chc nng

Cht gum cao su, cht ph bo v, cht chng to bt, cht

lm bng

5. Yu cu k thut
5.1. nh tnh
tan

Khng tan trong nc, tan rt t trong ethanol, t tan trong

diethyl ether v hexan.

Ch s khc x

n (100, D): 1,434 1,448

Ph hp th hng ngoi

Ph hp th hng ngoi ca mu nng chy v chun b

trn mt tm caesi hoc kali bromid tng ng vi ph
trong phn Ph lc

5.2. tinh khit

nht 1000C

Khng c nh hn 11 mm2/giy
Xem m t trong phn Phng php th

S carbon im
chng ct 5%

Khng c qu 5% cc phn t c s carbon nh hn 25

Xem m t trong phn Phng php th

Khi lng phn t

trung bnh

Khng nh hn 500
Xem m t trong phn Phng php th

Cn sau khi nung

Khng c qu 0,1%
Xem m t trong phn Phng php th

Mu sc

Xem m t trong phn Phng php th

Lu hunh

Khng c qu 0,4%
Xem m t trong phn Phng php th

Ch

Khng c qu 3,0 mg/kg.

Hydrocarbon a vng
thm

Mu th phi p ng cc gii hn hp th tia cc tm khi

tin hnh phn tch nh c m t trong Phng php
th.
Bc sng (nm)

hp th cc i/chiu di
ng truyn (cm)
14

QCVN 4-20:2010/BYT
280 - 289

0,15

290 - 299

0,12

300 - 359

0,08

360 - 400

0,02

6. Phng php th
tinh khit
nht 1000C

(ASTM D 445 c chp nhn vi s cho php t Sch

thng nin Tiu chun ASTM bn quyn ca Hip hi M
v Th nghim v Vt liu, 100 Harbor Drive, West
Conshohocken, PA 19.428 bn sao ca tiu chun ASTM
hon chnh c th c mua trc tip t ASTM, in thoi
610-832.
9.585,
fax:
610-832-9555,
e-mail:
service@astm.org,
website: http://www.astm.org)
S dng nht k mao qun thu tinh, hiu chnh v c
kh nng o nht ng hc vi lp li ch c 1/20
trng hp vt qu 0,35%. Ngm nht k trong chu cht
lng nng nhit 0,10C thch hp i vi mu th, m
bo trong sut qu trnh o, lc no mu th trong nht k
cng di b mt cht lng trong chu t nht l 20 mm.
Cho mu vo nht k theo cch ch dn thit k thit b. Gi
mu trong chu khong 30 pht. iu chnh th tch mu
n vch qui nh theo thit k ca nht k. Dng p lc
iu chnh mc trn cng ca mu n v tr cch pha trn
ca vch mc th nht khong 5 mm trong nhnh mao
qun ca thit b. Cho mu chy t do, o, thi gian cn
thit cho mt khum ca cht lng chuyn t vch nh mc
th nht n vch nh mc th hai. Thi gian o c tnh
bng giy vi sai lch 0,2 giy Nu thi gian nh hn 200
giy, chn nht k c mao qun c ng knh nh hn v
lp li cch lm. o thi gian chy ln hai. Nu c hai ln o
c sai s trong khong 0,2%, nht ng hc c tnh
bng gi tr trung bnh. Nu c hai ln o khng tng ng
th lp li cch xc nh sau khi lm sch v lm kh cn
thn nht k.
nht 1000C (mm2/giy) = C x t
Trong :
C: H s hiu chnh nht k (mm2/giy)
t: thi gian chy (giy)

S carbon im
chng ct 5%

S carbon l s nguyn t carbon trong mt phn t. Xc

nh s carbon c trong mu bng sc k kh. Di y ch
ra mt s iu kin hot ng in hnh xc nh n s
carbon n 45.
Chiu di ct (m)

25

30

15
15

QCVN 4-20:2010/BYT
ng
(mm)

knh

trong

0,32

0,53

0,25

DB-1
methyl
silicon

RTX-1
methyl
silicon

DB-5 5%
phenyl
methyl
silicon

dy lp phim mng
(m)

0,25

0,25

0,25

Kh mang

heli

heli

heli

Tc dng (ml/pht)

1,56

5,0

2,3

Tc tuyn (cm/giy)

33

35

60

800C

800C

800C

10

3800C

3400C

3500C

ngui trn
ct

ngui
trn ct

ngui
trn ct

Detector

FID

FID

FID

Nhit

3800C

3400C

3750C

1,0

1,0

1,0

Pha tnh

Chng trnh nhit

Nhit ban u
Tc
(0/pht)

nng

nhit

Nhit cui cng

K thut bm

Dung tch mu (l)

Lu : Bng cch ti u ho chiu di ct tch v/hoc

nhit ct, cc loi sp vi s carbon cao hn 45 cng c
th phn tch c.
Cc chun hiu chun v nh tnh:
Cc mu chun ca parrafin thng thng bao ph khong
s carbon ca mu c tinh khit ln hn 95%.
Chun tuyn tnh

16

QCVN 4-20:2010/BYT
Chun b mt hn hp bit khi lng ca cc n parafin
c chui carbon C16 C65, ho tan hn hp trong cyclohexan.
S dng nhng lng tng ng ca mi loi parafin
cn chnh xc n 1%. Cc dung dch c nng 0,01 %
(tnh theo khi lng) c th c s dng. Khng nht thit
phi bao gm mi n-parafin trong hn hp ny min l n
cha C16, C44, v c C60 nu xc nh s lng carbon cao
hn lin quan) v t nht mt trong mi n - parafin th t.
Cht chun ny phi c y cht ngn nga tht thot
dung mi.
Dung dch ni chun:
Chun b dung dch gc cha 0,5% (theo khi lng w/w) n
C16 trong n hexan ( tinh khit ti thiu 98%) bng cch
cn chnh xc 0,4 g n C 16 cho vo bnh nh mc dung tch
100 ml. Thm 100 ml cyclohexan v cn li. Ghi khi lng n
C16 ( WISTP ) ti trong khong 0,001 g v khi lng ca
dung dch gc ( WS ) ti trong khong 0,1 g. Chun b dung
dch ni chun long bng cch pha mt phn dung dch gc
vi 99 phn cyclohexan. Tnh nng dung dch ni chun
theo cng thc sau:

Trong :
CISTP: Nng ca n C16 trong dung dch ni chun long (%
theo khi lng)
WS: Khi lng dung dch gc (g)
Kim tra mu trng:
Bm 1 l dung mi. Khng c pick no c pht hin trong
khong thi gian lu m sp ra gii.
phn gii ct:
Bm 1 l dung dch 0,05% mi n C 20 v n C24 trong
cyclohexan. phn gii ct R khng c nh hn 30 c
tnh ton theo cng thc sau:

Trong :
d: Khong cch gia cc i pic ca n C20 v n C24 (mm)
W1: Pic bng mt na chiu cao ca n C20 (mm)
W2: Pic bng mt na chiu cao ca n C24 (mm)
tuyn tnh:
Phn tch chun tuyn tnh. Cc h s p ng khi lng
tnh ton lin quan n hexadecan phi trong khong 0,90
1,10.
lp li thi gian lu:
Phn tch chun tuyn tnh 2 ln. Cc thi gian lu i vi
17

QCVN 4-20:2010/BYT
phn tch 2 ln phi khng chnh lch hn 0,1 pht.
Hiu chun i vi xc nh n parafin:
Xc nh thi gian lu ca tng n parafin trong chui C 16
C44 ( hoc C60 nu xc nh s carbon cao hn lin quan )
bng cch bm lng nh ca mi parafin hoc ring bit
hoc trong hn hp bit trc.
Ly mu:
Gia nhit mu ti nhit cao hn 10 0C so vi nhit sp
c nu chy hon ton. Trn u bng cch khuy... s
dng ng nh git sch, nh mt vi git ln trn mt tm l
nhm sch, ng c v b thnh tng ming. L nhm
thng c cha sn mt mng mng bng du. Trc khi s
dng, du ny phi c loi b bng cch ra l nhm bng
cc dung mi nh hexan hoc cn khong.
Cch tin hnh:
Cn chnh xc 0,01 g mu ( W mu ) thu c theo m t trong
phn ly mu, cho vo mt l thu tinh c dung tch 15 ml.
Thm khong 12 ml dung dch ni chun long, y np l v
cn chnh xc khi lng ca dung dch ni chun pha long
thm vo ( WINSTD ). Lc l cho n khi sp ho tan hon ton,
s dng cch gia nhit nh nu cn thit.
Bm 0,5 1,0 l dung dch mu. Ghi li sc k v lu gi
tn hiu detector. Pic t dung dch ni chun phi c phn
gii hon ton khi din tch mu sp. Da vo thi gian lu
nh thu c trong phn Hiu chun i vi xc nh n
parafin, nh tnh cc pic parafin. S dng vch thng ng
ln ng nn nm ngang, ly tch phn tn hiu ca
detector. Tng cng din tch ca tt c cc pic ca mi s
carbon. Theo quy c, cc pic gn s carbon n l nhng pic
ra gii gia thung lng ngay pic parafin (C n-1) v thung lng
tng ng tip sau pic parafin (Cn).

18

QCVN 4-20:2010/BYT

Hnh 1: Tng s carbon (sc k vi ng nn nm

ngang)
Tnh kt qu:
i vi mi s carbon, hm lng tnh theo % khi lng
c tnh theo cng thc sau:
Ai
WISTD
Ci = ----------- x RRFi x -------------- x CISTD
AISTD
Wmu
Trong :
Ci: Hm lng hydrocarbon c s carbon i (% theo khi
lng)
Ai: Tng din tch ca cc hydrocarbon vi s carbon i
AISTD: Din tch ca pick ni chun n C16
RRFi: H s p ng lin quan n n C16
WINSTD: Khi lng dung dch ni chun long
Wmu: Khi lng mu sp
CISTD: Nng n C16 trong dung dch ni chun long
Hm lng tng hp ca cc thnh phn c s carbon nh
hn 25 khng c qu 5%.
Khi lng phn t
trung bnh

S dng phn b s carbon thu c trong phn th v S

carbon ti im chng ct 5% tnh khi lng phn t trung
bnh theo cng thc sau:

Trong :
i: S carbon
Ci: Hm lng cc thnh phn c s carbon i (%)

19

QCVN 4-20:2010/BYT
Cn sau khi nung

Cn chnh xc 2 g mu cho vo a s hoc platin bit

khi lng v gia nhit trn ngn la. Mu bay hi m khng
thot ra mi hng. Nung nhit khng qu sc ti cho
n khi khng cn carbon. Lm ngui trong bnh ht m v
cn.

Mu sc

Lm tan chy khong 10 g mu trong chu hi nc v cho 5

ml cht lng vo ng th vi sinh bng thu tinh sch, kch
thc 16 x 150 mm: cht lng c lm m, tan chy khng
c sm mu hn dung dch c to ra bng cch trn
hn hp gm 3,8 ml st (III) clorid TS (FNP 5) v 1,2 ml cobal
clorid TS (FNP 5) trong ng th tng t, so snh hai ng
bng phn chiu nh sng tng phn vi nn mu trng,
cc ng th c gi trc tip tng phn vi nn mt gc
m khng c hunh quang.

Lu hunh

(ASTM D 2622 Xem php th i vi nht 100 0C v

Bn quyn cho php)
Xc nh bng php o ph tia X s dng cc iu kin sau:
Dng c, thit b:
- My quang ph tia X c trang b pht hin tia mm
trong di 537 .
- ng truyn quang ca heli
- Thit b phn tch chiu cao xung hoc cc thit b phn bit
nng lng khc
- Detector c thit k pht hin cc tia X bc sng di
Tinh th phn tch ph hp vi tn sc ca tia X K lu
hunh trong khong gc ca thit b quang ph c s
dng. Pentaerythritol v germani l ph bin nht mc d
nhng cht t phn chiu hn nh EDDT, ADP v thch anh
c th c dng.
ng tia X pht bc x K lu hunh.
ng tia X vi mc tiu vonfram, platin hoc crom.
nhy chun:
Cc cht petroleum lng cha lu hunh cc nng xp
x khong gia th hiu chun c s dng cho php th.
Chun hiu chnh:
Chun b chun hiu chnh bng cch pha cn thn lng din-butyl sulfid (chun tinh khit cao vi mt phn tch c
chng nhn, sn xut c bit nh mt cht hiu chnh cho
phng php ny, lun c sn ca Cng ty Philips Petroleum,
Bartlesville, OK, M) vi du trng (cha nh hn 5 mg/kg).
Cc nng chun chnh xc c chun b gm 0,1; 0,25;
0,5 v 1,0% (theo trng lng).
ng chun:
o bc x lu hunh pht ra thc t mi chun hiu chnh.
V th cng , di dng s m thc trn giy, vi
nng lu hunh.
20

QCVN 4-20:2010/BYT
duy tr gi tr ng chun vi s thay i nh v nhy
cc thit b, o nhy chun ti cc khong thi gian
thng xuyn trong cc ngy chy. Thit lp t l tnh ca
chun ny bng cch o nhy ca chng ti cc khong
thi gian thng xuyn trong qu trnh chun b ng hiu
chun. Tnh h s hiu chnh i vi cc thay i nhy ca
thit b hng ngy bng cng thc sau:

Trong :
A: S m ca nhy chun c xc nh ti thi im
hiu chnh
B: S m ca nhy chun c xc nh ti thi gian
phn tch
Cch tin hnh:
mu trong cng o thch hp. Mc d bc x lu hunh
xuyn qua ch mt khong nh trong mu, phn tn t cc
mu v mu c th khc nhau n mc m mt lng c th
hoc mt lng ti thiu mu phi c s dng.
t mu trong chm tia X v cho php kh quyn quang hc
tia X n trng thi cn bng. Xc nh cng ca bc
x K lu hunh ti 5,373 bng cch o tc m ti
nhng ch gc chnh xc t cho bc sng ny. o tc
m nn ti 5,190 .
Tnh kt qu:
Hm lng lu hunh trong mu c tnh theo cng thc
sau:

Trong :
R: Tc m thc c hiu chnh
CK: Tng s m thu c ti 5,373 i vi mu
S1: Thi gian cn thit thu c cc s C K (giy)
CB: Tng s m thu c ti 5,190 i vi nn
S2: Thi gian cn thit thu c cc s C B (giy)
F: Tc m ti 5,373 / tc m ti 5,190 i vi
mu khng cha lu hunh
F: H s hiu chnh i vi cc thay i nhy thit b hng
ngy.
S dng tc m thc hiu chnh, c nng lu
hunh t ng chun.

21

QCVN 4-20:2010/BYT
Ch

- Th theo JECFA monograph 1 - Vol.4.

- Xc nh bng k thut quang phhp th nguyn t thch
hp cho hm lng quy nh. La chn c mu th v
phng php chun b mu da trn nguyn tc ca phng
php m t trong JECFA monograph 1 - Vol.4 phn cc
phng php phn tch cng c.

Hydrocarbon a
vng thm

Hng dn chung:
Do nhy ca php th, kh nng sai s pht sinh t nhim
bn l kh ln. iu quan trng nht l tt c dng c thu
tinh phi c c ra sch nghim ngt loi b tt c cc
cht hu c nh du, m, d lng cht ty ra,... Kim tra
tt c dng c thy tinh, bao gm c nt v cc van, di nh
sng t ngoi pht hin bt k nhim hunh quang cn
st li. Nh mt bin php phng, khuyn ngh thc hnh
ra tt c dng c thy tinh vi isooctane tinh khit ngay
trc khi s dng. Khng s dng bt k m bi trn no
hoc khp ni. Ht sc cn thn trnh nhim cc mu
sp trong vic x l v m bo khng c bt k cht
khng lin quan pht sinh t bao b khng thch hp l iu
cn thit. Bi v mt s cc hydrocarbon a vng tm c
trong th nghim ny rt d b oxy ha bi nh sng, ton b
quy trnh phi c thc hin di nh sng du.
Thit b, dng c:
- Phu chit: dung tch 250 ml, 500 ml, 1.000 ml v tt nht l
loi c dung tch 2.000 ml, c kho van bng polymer
tetrafluoroethylen.
- Bnh cha: dung tch 500 ml, c trang b mt khp ni
thon chun 24/40 ni ti y bnh v mt khp ni cu trn
nh bnh ni vi ngun cung cp nitrogen. Khp ni thch
hp phi c trang b cc mc thu tinh.
- Ct sc k: di 180 mm, ng knh trong 15,7 0,1 mm,
c trang b vi mt a thu tinh xp th, kho van polymer
tetrafluoroethylen v mt khp ni thon chun 24/40 c l
lp v tr cui i din. (chiu di ton b ca ct vi khp
ni c l lp l 235 mm).
- a: c lm bng polymer tetrafluoroethylen ng knh
2 inch, dy 3/16 inch c l gia va kht thn ct sc k.
- o gia nhit: hnh nn, dng cho phu chit dung tch 500
ml. (c s dng vi b kim sot bin nhit).
- Bnh ht: Bnh lc dung tch 250 ml hoc 500 ml.
- ng sinh hn: khp ni 24/40, ni vi ng kh, chiu di
khng bt buc
- Bnh c (khng bt buc): Tt c bnh thu tinh dung tch
250 ml hoc 500 ml c trang b vi np y thon chun c
ng dn vo v ra cho php nitrogen qua ngang b mt ca
cht lng c c.
- Dng c chng ct chn khng: tt c bng thu tinh (
lm sch dimethyl sulfoxid); bnh ct dung tch 2 lt c o gia
22

QCVN 4-20:2010/BYT
nhit; sinh hn Vigreaux c bao chn khng (hoc tng
ng) c chiu di khong 45 cm v u chng ct ni vi
ng sinh hn c th chia nhnh lnh. Dng polymer
tetrafluoroethylen bc ngoi cc khp ni thu tinh ngn
ng bng. Khng c s dng m cc kho van hoc
cc khp ni.
- Cc cng o quang ph: cc cng o lm t thch anh nu
chy, chiu di ng truyn quang 5,0 0,005 cm; mt loi
cng o khc ch kim tra hiu sut ca thit b quang ph,
c chiu di ng truyn quang hc 1,000 0,005 cm. Vi
nc ct trong cc cng o, xc nh xem c chnh lch
hp th hay khng.
- Thit b quang ph: Di quang ph 250 400 nm vi chiu
rng khe ph 2 nm hoc nh hn, theo cc iu kin hot
ng ca thit b o hp th , thit b quang ph cng
phi p ng cc yu cu thc hin sau y:
lp li hp th : 0,01 ti hp th 0,4
chnh xc hp th : 0,05 ti hp th 0,4
lp li bc sng: 0,2 nm
chnh xc bc sng: 1,0 nm
- Bnh kh nitrogen: nitrogen tinh khit trong bnh kh nn
c trang b b iu p v van kim sot dng kh ti 5
p.s.i.g.
Nguyn vt liu v ho cht:
- Dung mi hu c: Tt c dung mi c s dng trong qui
trnh phi ph hp vi cc c tnh k thut v php th c
m t trong phn cc c tnh k thut ny. Isooctan, benzen,
aceton v methyl alcol c ch r trong danh sch di y
s phi qua php th sau:
Cho lng dung mi xc nh vo trong bnh tam gic dung
tch 250 ml. thm vo 1 ml n hexadecan tinh khit v c trn
chu hi nc di dng nitrogen (o l nhm ri bao quanh
bnh s lm tng tc c). Ngng c khi cn li khng qu 1
ml cn. (Cho mt phn 10 ml isooctan tinh khit vo cn t
benzen, c li v lp li mt ln na m bo loi hon
ton benzen).
Cch khc, thi gian c c th gim bng cch s dng bnh
c ty chn. Trong trng hp ny dung mi v n
hexandecan c cho vo trong bnh t trong ni cch thy,
lp h thng ng v mt dng nitrogen c cho vo qua
ng ng vo trong khi ng ng ra c ni vi mt by
dung mi v ng chn khng nh l cch ngn bt k
dng ngng no quay ngc li vo bnh.
Ho tan 1 ml cn hexadecan trong isooctan v nh mc ti
vch. o hp th trong cng o c chiu di ng truyn
5 cm so vi isooctan lm i chng. hp th dung dch
ca cn dung mi (tr methyl alcol) khng vt qu 0,01/cm
chiu di ng truyn trong khong bc sng 280 nm v
400 nm. i vi methyl alcol, hp th phi bng 0.
- Isooctan (2,2,4 trimethylpentan): Dng 180 ml cho php
th c miu t trong on trc. Lm sch nu cn bng
23

QCVN 4-20:2010/BYT
cch cho qua ct cha silica gel hot ho (loi 12, Cng ty
ho cht Davison, Baltimore, Maryland, hoc tng ng)
c chiu di khong 90 cm v ng knh 5 8 cm.
- Benzen tinh khit: Dng 150 ml cho php th. Lm sch nu
cn bng chng ct hoc bng cch khc.
- Aceton tinh khit: Dng 200 ml cho php th. Lm sch nu
cn bng chng ct.
- Hn hp ra gii:
+ Benzen 10% trong isooctan: Dng pipet ly 50 ml benzen
cho vo bnh nh mc c np y thu tinh dung tch 500 ml,
iu chnh n th tch 500 ml bng isooctan v lc u.
+ Benzen 20% trong isooctan: Dng pipet ly 50 ml benzen
cho vo bnh nh mc c np y thu tinh dung tch 250 ml,
iu chnh n th tch 250 ml bng isooctan v lc u.
+ Hn hp aceton benzen nc: Cho 20 ml nc vo 380
ml aceton v 200 ml benzen, v trn u.
- n hexadecan, 99% khng c olefin: Pha 1 ml n
hexadecan n th tch 25 ml bng isooctan v o hp th
trong cng o 5 cm so vi isooctan lm i chng gia 280
400 nm. hp th trn mt cm ng truyn khng vt
qu 0. Lm sch nu cn bng lc thm qua silicagel hot
ho hoc bng chng ct.
- Methyl alcol tinh khit: Dng 10,0 ml methyl alcol. Lm sch
nu cn bng chng ct.
- Dimethyl sulfoxid: tinh khit, trong, mu trng nc, nhit
nng chy thp nht 180C.
Pha 120 ml dimethyl sulfoxid vi 240 ml nc ct trong phu
chit dung tch 500 ml, lc u v ngui trong 5 -10 pht.
Thm 40 ml isooctan vo dung dch v chit bng cch lc
phu mnh trong 2 pht. Ht lp nc pha di vo phu
chit th hai c dung tch 500 ml v lp li qu trnh tch vi
40 ml isooctan. Ht v loi b lp tan trong nc. Ra mi
phn chit c 40 ml ba ln bng cc phn 50 ml nc ct.
Thi gian lc cho mi ln ra l 1 pht. Loi b cc lp tan
trong nc. Lc phn chit u tin qua Na 2SO4 khan
c ra bng isooctan (xem Na2SO4 khan trong phn
Nguyn vt liu v ho cht i vi chun b phu lc) vo
trong bnh tam gic hoc bnh c ty chn. Ra phu chit
th nht bng phn chit 40 ml isoocatan th hai v lc qua
Na2SO4 vo trong bnh. Sau ra ln lt phu chit th
hai v th nht bng 10 ml isooctan, v cho dung mi qua
Na2SO4 vo trong bnh. Thm 1 ml n hexadecan v c
isooctan trn cch thy c ui hi bng kh nitrogen. Ngng
c khi khng qu 1 ml cn cn li. Cho 10 ml isooctan vo
cn v li c ti khi cn 1 ml hexadecan. Lp li, cho 10 ml
isooctan vo cn v c ti 1ml hexadecan m bo loi b
hon ton tt c cc cht bay hi. Ho tan 1 ml hexadecan
trong isooctan va 25 ml. o hp th trong cc cng o
c chiu di ng truyn 5 cm so vi isooctan l i chng.
hp th ca dung dch khng c qu 0,02/cm chiu di
ng truyn trong di 280 400 nm. ( Ch : Vic kh p
24

QCVN 4-20:2010/BYT
ng c tnh hp th ny c th l do cc tp cht hu c
trong nc ct. S lp li ca php th khng c dimethyl
sulfoxid s pht hin ra chng. Nu cn thit p ng cc
c im k thut, lm sch nc bng chng ct li, cho
chy qua mt loi nha trao i ion, hoc bng cch khc).
Lm sch nu cn thit bng cch sau: Cho 6 ml dung dch
H3PO4 v 50 g Norit A (carbon kh mu, kim) hoc tng
ng vo 1,5 lt dimethyl sulfoxid trong bnh c np y thu
tinh dung tch 2 lt. y np bnh v dng my khuy t
(thanh khuy bc polymer tetrafluoroethylen) khuy dung mi
trong 15 pht. Lc dimethyl sulfoxid qua bn lp giy c rnh
(18,5 cm) (Schleicher & Schuell s 597 hoc tng ng).
Nu dch lc ban u cha bt carbon, lc li theo ging cch
trn cho n khi dch lc thu c trong. Bo qun sulfoxid
trnh khng kh v m trong sut qu trnh ny bng cch ph
ln dung mi trong phu v bnh thu bng mt lp isooctan.
Chuyn phn lc c vo phu chit dung tch 2 lt v ht ra
dimethyl sulfoxid cho vo bnh dung tch 2 lt ca thit b
chng ct chn khng v ct p sut khong 3 mmHg hoc
thp hn. Loi b phn phn on 200 ml u ca dung dch
chng ct c v thay bnh hng dch chng ct c bng
mt bnh sch. Tip tc chng ct cho n khi thu c
khong 1 lt sulfoxid. Khi hon tt qu trnh chng ct, cht
phn ng cn phi c bo qun trong cc chai c np y
thu tinh v n d ht m v phn ng vi mt s dng c
cha bng kim loi khi c mt ca khng kh.
- H3PO4 tinh khit 85%
- Natri borohydrid 98%
- MgO ( Sea Sorb 43, Cng ty thit b thc phm, chi nhnh
Westvaco, c phn phi bi cc hng ho cht, hoc
tng ng): Cho 100 g MgO vo mt cc ln, thm vo
700 ml nc ct to thnh mt cht sn st long, gia nhit
trn cch thy trong 30 pht v thnh thong khuy. Lc u
khuy u m bo tt c cc cu t MgO u c thm
nc. S dng phu Buchner v giy lc c ng knh ph
hp, lc ht. Tip tc lc ht cho n khi nc khng cn
chy nh git t phu na. Chuyn cht hp th sang mt
mng thu tinh c lt bng l nhm ( loi ht du chng
dnh). Lm v magnesi bng tha sch v tri cht hp th
ny trn tm l nhm mt lp dy 1 2 cm. Sy 160 10C
trong 24 gi. Gi nh magnesi bng ci gi v chy. Ry cht
hp th c gi qua kch thc ry 60 180 mesh. Dng
magnesi cn li trn ry 180 mesh.
- Celite 545 (Cng ty Johns Manville, t to ct, hoc
tng ng)

25

QCVN 4-20:2010/BYT
- Hn hp MgO Celite 545 (2 + 1) theo khi lng: Cho 2
phn MgO (60 180 mesh) v 1 phn Celite 545 theo khi
lng ln lt vo bnh thu tinh c np y ln trn
cho ph hp. Lc mnh trong 10 pht. Chuyn hn hp sang
mt mng thu tinh c lt bng l nhm ( loi ht du
chng dnh) v tri hn hp trn tm l nhm mt lp dy 1
2 cm. Li gia nhit hn hp 160 10C trong 2 gi v bo
qun trong bnh c y cht.
- Na2SO4 khan, tinh khit, tt nht dng dng ht: i vi
mi bnh cha Na2SO4 tinh khit c s dng, thit lp nh
sau, ra trc Na2SO4 cn thit cung cp cc b lc nh
yu cu trong phng php: Cho khong 35 g Na 2SO4 khan
vo trong phu thu xp th c dung tch 30 ml hoc phu lc
dung tch 65 ml c cht bng thu tinh; ra ln lt cc phn
15 ml dung mi ch nh cho n khi phn ra 15 ml c
hp th bng 0/cm chiu di ng truyn ti bc sng 280
400 nm khi c o nh m t trong phn Dung mi hu
c. Thng dng 3 phn ca dung mi ra l .
Cch tin hnh:
Trc khi thc hin phn tch mu, o hp th trong cng
o c chiu di ng truyn 5 cm ti di bc sng 250
400 nm i vi mu trng bng cch thc hin cch tin
hnh, khng c mu sp, nhit phng, ghi ph sau giai
on chit v sau khi hon thnh cch tin hnh nh m t.
hp th trn 1 cm chiu di ng truyn sau giai on
chit khng c qu 0,04 ti khong bc sng 250 400
nm; hp th trn 1 cm chiu di ng truyn sau hon
thnh cch tin hnh khng c qu 0,07 ti khong bc
sng 250 299 nm, v cng khng vt qu 0,045 ti
khong bc sng 300 400 nm. Nu trong c hai ph xut
hin pic ca benzen c trng trong vng 250 260 nm, loi
b benzen bng cch tin hnh trong phn Dung mi hu
c v ghi li hp th.
Cho 300 ml dimethyl sulfoxid vo trong phu chit dung tch 1
lt v thm vo 75 ml H3PO4. Lc u cc thnh phn trong
phu v yn trong 10 pht. (Phn ng gia sulfoxid v
acid to nhit. X p sau khi lc, sau ng np phu li).
Thm vo 150 ml isooctan v lc u cc dung mi. Ht ra
tng lp ring bit v gi trong cc bnh thu tinh c np y.
Cho 1 kg mu i din ca sp, hoc nu lng ny khng
c th cho ton b mu vo trong mt cc c dung tch gp
khong ba ln th tch ca mu v gia nhit trn cch thy
si, thnh thong khuy cho n khi sp nng chy hon ton
v ng nht. Cn bn phn 25 0,2 g sp nng chy cho
vo cc cc dung tch 100 ml ring bit. D tr ba trong bn
phn phn tch lp sau nu cn. mt phn mu bit
khi lng ngay sau khi nng chy li trn cch thy si vo
phu chit dung tch 500 ml c cha 100 ml hn hp sulfoxid
v H3PO4 cn bng trc, gia nhit trong o nhit nhit
va cao lm nng chy sp. (Ch : Trong qu trnh
gia nhit trc hn hp sulfoxid v acid, nh k m np y
ca phu chit gim p sut).
26

QCVN 4-20:2010/BYT
Nhanh chng hon thnh vic chuyn mu vo phu trong o
gia nhit vi cc phn isooctan cn bng trc, lm m cc
nu cn thit, v s dng tng th tch 50 ml dung mi. Nu
sp tch ra khi dung dch trong ton b cch lm ny,
phu chit ng np trong o gia nhit cho n khi sp tan
li hon ton. (nh k m np y ca phu chit gim p
sut).
Khi sp chy tan thnh dung dch, ly phu chit ra khi o
gia nhit v lc mnh trong 2 pht. Chun b sn 3 phu chit
dung tch 250 ml vi mi phu cha 30 ml dung mi isooctan
cn bng trc. Sau khi tch pha lng, ngui cho n
khi phn ch yu ca dung dch sp isooctan bt u hnh
thnh kt ta. Lc xoy nh phu chit khi kt ta lc u
xut hin thnh trong ca phu chit nhm lm tng nhanh
hn qu trnh ny.
Ly cn thn lp pha di, lc chm qua lp bng thu tinh
mng va t lng trong phu lc vo trong phu chit th
nht dung tch 250 ml, ra ln lt bng cc phn 30 ml
isooctan cha trong cc phu chit dung tch 250 ml cn li.
Thi gian lc i vi mi ln ra l 1 pht. Lp li qu trnh
chit bng cch thm hai phn hn hp sulfoxid v acid, thay
phu trong o gia nhit sau mi ln chit m bo sp tan
trong dung dch v ra ln lt mi phn chit thu c bng
ba phn isooctan ging nhau.
Tp trung cc phn chit thu c (tng th tch 300 ml) cho
vo phu chit (tt nht dng loi phu c dung tch 2 lt) c
cha 480 ml nc ct, lc v ngui trong mt vi pht sau
khi phn chit thu c cui cng c thm vo. Thm 80
ml isooctan vo dung dch v chit bng cch lc mnh phu
trong 2 pht. Rt ra lp tan trong nc pha di trong
phu chit th hai (tt nht dng loi 2 lt) v lp li qu trnh
chit bng 80 ml isooctan. Rt ra v loi b lp tan trong
nc. Ra mi phn chit thu c 80 ml ba ln vi cc
phn 100 ml nc ct. Thi gian lc cho mi ln ra l 1
pht. Loi b cc lp tan trong nc. Lc phn chit th nht
qua Na2SO4 khan c ra trc bng isooctan (xem
Na2SO4 trong phn Nguyn vt liu v ho cht i vi
chun b phu lc) vo trong bnh tam gic (hoc bnh c ty
chn). Ra phu chit th nht bng phn chit 80 ml
isooctan th hai v cho qua Na 2SO4. Sau ra ln lt
phu chit th hai v th nht bng mt phn 20 ml isooctan
v cho dung mi qua Na2SO4 vo trong bnh. Thm 1 ml n
hexadecan v c isooctan trong cch thy c thi kh
nitrogen. Ngng c khi cn li khng qu 1 ml cn. Thm 10
ml isooctan vo phn cn, c li ti 1 ml hexadecan v lp li
qu trnh ny mt ln na.
Chuyn ton lng phn cn trong isooctan vo bnh nh
mc dung tch 25 ml, nh mc ti th tch 25 ml v lc u.
o hp th ca dung dch trong cc cng o c chiu di
ng truyn 5 cm so vi isooctan l i chng ti di bc
sng 280 400 nm (cn thn khng mt dung dch trong
qu trnh mu y cng o).
27

QCVN 4-20:2010/BYT
Hiu chnh cc gi tr hp th i vi bt k hp th no
c ngun gc t ho cht c xc nh bi tin hnh cch
lm khng c mu sp. Nu hp th khng vt qu gii
hn c m t ti Cc c tnh k thut, sp p ng cc
c tnh k thut v hp th tia cc tm. Nu hp th hiu
chnh trn mi cm chiu di ng truyn vt qu gii hn
quy nh ti Cc c tnh k thut, tin hnh nh sau:
Chuyn ton lng dung dch isooctan vo bnh c lp
khp ni 24/40 dung tch 125 ml v c isooctan trong chu
cch thy di dng nitrogen ti th tch 1 ml hexadecan.
Thm 10 ml methyl alcol v khong 0,3 g natri borohydrid
(Gim thiu tip xc borohydrid vi bu kh quyn. Mt dng
c nhng o c th c s dng). Ngay lp tc, rp bnh vi
mt sinh hn lm ngui bng nc c g lp mt khp ni
24/40 v ng lm kh dn vo trong bnh, khuy cho n khi
borohydrid tan, yn trong 30 pht nhit phng, thnh
thong lc xoy. Ti im kt thc ca giai on ny, tho
bnh v c methyl alcol trong cch thy c thi kh nitrogen
cho n khi natri borohydrid bt u tch ra khi dung dch.
Sau thm 10 ml isooctan v c ti th tch cn li khong
2 3 ml. Lp li, cho 10 ml isooctan v c n th tch
khong 5 ml. Lc xoy bnh lp li nhiu ln m bo
ra cn natri borohydrid.
Lp a polymer tetrafluoroethylen ln phn trn ca thn ct
sc k, sau ct sc k vi a trn bnh ht v ht chn
khng (p sut khong 135 mmHg). Cn 14 g hn hp
magnesi oxyd v Celite 545 (t l 2/1) v hn hp cht hp
ph vo trong ct sc k vi cc lp dy khong 3 cm. Sau
khi thm vo mi lp, san bng phn trn ca cht hp ph
bng thanh knh phng hoc pittng kim loi bng cch nhn
xung tht chc cho n khi cht hp th c nhi vo. Ni
lng vi ml trn cng ca mi lp hp ph bng thanh kim loi
trc khi b sung lp k tip. Tip tc nhi theo cch ny cho
n khi tt c 14 g cht hp ph c cho vo ct. San bng
phn u ca cht hp ph bng thanh knh phng hoc
pittng kim loi bng cch nhn xung tht chc to ra
su ca lp cht hp ph khong 12,5 cm. Tt chn khng v
kho bnh ht. Ni bnh nhn dung tch 500 ml vo bn trn
ct sc k v lm m ct trc bng cch cho 100 ml
isooctan qua ct. iu chnh p sut kh nitrogen tc h
xung ca isooctan ra ngoi ct l 2 3 ml/pht. Ngng p
lc ngay trc khi isooctan cui cng t n mc ca cht
hp ph. (Ch : Khng cho php mc cht lng rt di
mc hp ph bt c khi no).
Tho bnh cha ra v gn 5 ml dung dch isooctan m c
vo ct v li s dng p lc nh y cht lng rt xung ch
trn mc cht hp ph. Nhanh chng hon thnh vic chuyn
tng t vi hai phn 5 ml isooctan, lc xoy bnh nhiu ln
mi ln m bo ra cn. Ngay trc khi ra 5 ml cui
cng t n nh ca cht hp ph, thm 100 ml isooctan
vo bnh nhn v tip tc thm qua vi tc 2 3 ml/pht.
Ngay trc khi isooctan cui cng t n mc hp ph,
28

QCVN 4-20:2010/BYT
thm 100 ml dung dch benzen 10% trong isooctan vo bnh
nhn v tip tc thm qua vi tc cp trn. Ngay
trc khi hn hp dung mi t n mc cht hp ph, thm
25 ml dung dch benzen 20% trong isooctan vo bnh nhn v
tip tc cho thm qua vi tc 2 - 3 ml/pht cho n khi tt
c hn hp dung mi ny c loi b ra khi ct. Loi b
tt c dung mi ra gii thu c n thi im ny. Thm
300 ml hn hp aceton benzen nc vo bnh nhn v
cho thm qua ct ra gii cc hp cht a vng. Thu thp
cc phn ra gii vo trong mt phu chit sch dung tch 1 l.
ct chy cho n khi hu ht cc hn hp dung mi c
ly ra. Ra phn dch ra gii ba ln vi cc phn 300 ml
nc ct, lc u cho mi ln ra. (Vic b sung mt lng
nh NaCl to iu kin cho qu trnh phn tch). Loi b lp
dung dch nc sau mi ln ra. Sau khi tch ln cui cng,
lc benzen d qua Na2SO4 khan c ra trc bng
benzen (xem Na2SO4 trong phn Nguyn vt liu v ho
cht i vi chun b phu lc) vo trng bnh tam gic dung
tch 250 ml (hoc vo trong bnh c ty chn). Ra phu chit
2 ln na, mi ln vi 20 ml benzen cng c lc qua
Na2SO4. Thm 1 ml n hexadecan v loi hon ton benzen
bng cch c di dng nitrogen, s dng cch tin hnh
c bit loi benzen nh m t phn trc mc Dung
mi hu c.
Chuyn ton lng cn vi isooctan vo bnh nh mc dung
tch 25 ml v iu chnh n th tch 25 ml. o hp th ca
dung dch trong cc cng o c chiu di ng truyn 5 cm
so vi isooctan l i chng khong bc sng 250 400
nm. Hiu chnh vi bt k hp th no xut pht t cc
ho cht nh xc nh bng cch thc hin khng c mu
sp. Nu quang ph cho thy cc pic benzen c trng trong
vng 250 - 260 nm, c dung dch loi b benzen theo cch
tin hnh trong phn "Dung mi hu c". Ha tan cn,
chuyn ton lng v iu chnh th tch n th tch 25 ml
trong bnh nh mc bng isooctan. Ghi hp th mt ln
na. Nu hp th hiu chnh khng vt qu gii hn
c m t trong phn Cc c tnh k thut, ch tiu sp p
ng k thut v hp th tia cc tm.
Ph lc

Ph hng ngoi

Sp vi tinh th

29

QCVN 4-20:2010/BYT

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