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CNG HO X HI CH NGHA VIT NAM

QCVN 4 - 17: 2010/BYT

QUY CHUN K THUT QUC GIA


V PH GIA THC PHM - CHT KH Y
National technical regulation on Food Additive Propellants

H NI - 2010

QCVN 4 -17: 2010/BYT

Li ni u
QCVN 4-17:2010/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 v sinh thc phm trnh duyt v c ban
hnh theo Thng t s 44/2010/TT-BYT ngy 22 thng 12
nm 2010 ca B trng B Y t.

QCVN 4 -17: 2010/BYT

QUY CHUN K THUT QUC GIA


V PH GIA THC PHM - CHT KH Y
National technical regulation on Food Additive Propellants

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 kh y 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 kh y 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 kh y: l ph gia thc phm dng kh c cho vo thc phm.
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 -17: 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 kh y 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 kh


nitrogen

1.2.

Ph lc 2:

Yu cu k thut v phng php th i vi kh


nitrogen oxyd

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 c gi tr 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 kh y 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 kh y
Vic kim tra cht lng, v sinh an ton i vi cc cht kh y phi thc
hin theo cc quy nh ca php lut.
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.

QCVN 4 -17: 2010/BYT


2. T chc, c nhn ch c nhp khu, xut khu, sn xut, bun bn v s dng
cc cht kh y 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 -17: 2010/BYT


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

Nitrogen
INS 941
ADI khng gii hn

2. nh ngha

Chuyn lun ny nh ngha Nitrogen vi hm lng


oxygen ti a l 1%, ch ph hp vi mt s i tng thc
phm. Mt s i tng thc phm khc yu cu tinh
khit cao hn (tng ng vi hm lng oxygen thp
hn).

Tn ha hc

Nitrogen

M s C.A.S.

7727-37-9

Cng thc ha hc

N2

Khi lng phn t

28,0

3. Cm quan

Kh hoc dng lng khng mu, khng mi.

4. Chc nng

Tc nhn lm lnh, cht kh y, kh dng trong bao gi

5. Yu cu k thut
5.1. nh tnh
Th ngn la

Ngn la b tt trong mi trng to ra bi mu th.

5.2. tinh khit


Oxygen

Theo hng sn xut cng b, nhng khng c qu 1%


(tt/tt) (m t trong phn Phng php th).

Carbon monoxyd

Khng c qa 10 l/l (m t trong phn Phng php


th).

5.3. Hm lng

Khng thp hn 99,0 % tt/tt.

6. Phng php th
6.1. tinh khit
Oxygen

S dng thit b phn tch oxygen vi detector c khong


lm vic t 0 - 100 l/l, gn vi mt pin in ha. Mu kh
th c dn qua detector in ha cha dung dch lng,
thng l dung dch kali hydroxyd. Oxygen trong mu kh
th s to nn s thay i tn hiu in. S thay i ny
c ghi li u ra ca pin in ha v t l vi hm
lng oxygen.
Hiu chun li thit b phn tch theo hng dn ca hng
sn xut. S dng b iu p ph hp v cc ng kim loi
khng r kh (airtight) dn kh chy qua thit b phn
tch. Vn hnh vi tc dng kh cho n khi t c
6

QCVN 4 -17: 2010/BYT


tn hiu n nh.
Carbon monoxyd

Cho khong 105050 ml mu kh th chy qua ng


detector o carbon monoxyd vi tc kh c ch nh
cho ng detector. Hm lng tng ng vi s thay i tn
hiu thu c khng c php qu 10 l/l.

6.2. nh lng
Xc nh bng sc k kh vi cc iu kin o nh sau:
Ct tch:
vt liu: thp khng r
chiu di : 2m
ng knh trong: 2 mm
cht nhi ct: ry phn t ph hp, c kh nng hp th
cc phn t c ng knh n 0,5 nm.
Kh mang:
- Kh: heli (khng thp hn 99.995 % (v/v) He)
- Tc dng kh: 40 ml/min
Detector: Detector dn nhit
Injector: injector vng
Nhit ct: 50C
Nhit detector: 130C
Kh i chiu (a): khng kh
Kh i chiu (b): Nitrogen (khng thp hn 99.999 % (tt/tt)
ca N2, thp hn 1 ppm CO, thp hn 5 ppm O2)
Tin hnh:
Bm kh i chiu (a). iu chnh th tch bm v iu kin
o sao cho chiu cao ca peak nitrogen trn sc chim
t nht l 35 % ton thang ghi. Php th s khng chnh
xc nu sc khng tch c r rt nitrogen v oxygen.
Bm mu th v kh i chiu (b). Peak chnh trong sc
thu c ca mu th phi c din tch bng t nht l
99,0% din tch ca peak chnh thu c trong sc ca
kh i chiu (b).

QCVN 4 -17: 2010/BYT


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

Nitrogen oxyde, dinitrogen monoxyde,


INS 942
ADI khng gii hn

2. nh ngha
Tn ha hc

Dinitrogen monoxyd

M s C.A.S.

10024-97-2

Cng thc ha hc

N2O

Khi lng phn t

44,01

3. M t

Kh khng mu, khng mi.

4. Chc nng

Cht kh y, cht chng oxi ha, kh dng trong bao gi,


cht to bt

5. Yu cu k thut
5.1. nh tnh
o

tan

1 th tch mu th ha tan trong 1,5 th tch nc ( 20 C,


760 mm Hg)

Th ngn la

G vn, nung nng khi tip xc vi nitrogen oxyd s chy


bng thnh ngn la (phn bit vi nitrogen).

Th Pyrogallol

t yu cu (phn bit vi oxygen).

5.2. tinh khit


Carbon monoxyd

Khng c qa 10 l/l.

Nitric oxyd v nitrogen


dioxyd

Khng c qa 5 l/l.

Cc Halogen v
hydrogen sulfid

Khng c qa 5 l/l.

Arsin and phosphin

t yu cu.

5.3. Hm lng

Khng thp hn 97,0 % (tt/tt).

6. Phng php th
6.1. nh tnh
Th Pyrogallol

Ly khong 100 ml kh th vo ng dung tch 100 ml, u


ng c gn kha vi. M kha vi, nhanh chng thm vo
dung dch 500mg pyrogallol / 2ml nc mi pha v dung
dch 12 g kali hydroxyd/ 8 ml nc mi pha. Lp tc ng
8

QCVN 4 -17: 2010/BYT


kha vi li, lc u. Kh th khng b hp th v dung dch
khng chuyn thnh mu nu.

QCVN 4 -17: 2010/BYT


6.2. tinh khit

Ch : Vi cc php th sau y, phi gi bnh kh th ti


nhit phng t nht l 6 gi trc khi tin hnh php th.
Trong tt c cc php th, bnh kh th phi c gi thng
ng, khi chuyn kh, van kh ra phi hng ln trn. Nu
khng c ch dn no khc th dn kh vi tc khng i l
4 L/gi v tin hnh php th hoc tnh ton kt qu tham
chiu vi kh 20C v 760 mm Hg.

Carbon monoxyd

Nguyn tc:
Tin hnh php th vi phn mu th u tin ly ra t bnh
kh. Ly 5 L nitrogen oxyd th v 5,0 L khng kh khng
cha carbon monoxyd lm mu chng. Chnh lch th
tch dung dch natri thiosulfat 0,002 N dng chun
trong 2 th nghim khng c qu 0,5 ml.
Thit b:
Thit b bao gm cc phn c ni thnh chui nh sau:
- ng hnh ch U c cha silicagel khan nhi trong crom
trioxyd.
- Bnh ra kh (loi dreschel) cha 100 dung dch kali
hydroxyd 40% kl/tt.
- ng hnh ch U ng cc vin kali hydroxyd.
- ng hnh ch U ng phosphor pentoxyd phn tn trong
bt dng vin nung chy.
- ng ng anhydrid iodic (I2O5) kt tinh li, dng vin,
c sy kh 200C v gi nhit 120C. Anhydrid
iodic khan c nhi trong ng t trong cc ct chiu di
lp anhydrid iodic l 1cm, cc lp anhydrid iodic cch nhau
bi phn bng thy tinh dy 1 cm sao cho tng chiu di hiu
dng l 5 cm.
- Bnh c cha 2 ml dung dch kali iodid (TS) v 3 git dung
dch h tinh bt (TS)
Tin hnh
Sc 5,0 L khng kh khng cha carbon dioxyd qua thit b.
Nu cn, lm mt mu xanh ca dung dch iod bng cch
thm vo mt lng ti thiu dung dch natri thiosulfat
0,002 N mi pha. Tip tc sc kh qua thit b cho n khi th
tch dung dch natri thiosulfat 0,002 N cn dng khng ln
hn 0,045 ml, sau khi sc 5 L khng kh khng cha
carbon dioxyd.
Dn kh chy t bnh kh qua thit b o, vi th tch v tc
dng kh nh m t trong chuyn lun. Chuyn ton b
lng vt iod to thnh vo bnh phn ng bng cch cho
1 L khng kh khng cha carbon monoxyd chy qua thit b.
Chun lng iod c gii phng bng dung dch natri
thiosulfat 0,002 N.
Tin hnh lm mu trng song song, vi kh khng c
carbon monoxyd. Hiu th tch natri thiosulfat 0,002 N cn
dng gia 2 ln chun khng c ln hn gii hn
cho trong cc chuyn lun.

Nitric oxyd v nitrogen

Nguyn tc:
10

QCVN 4 -17: 2010/BYT


dioxyd

Tin hnh php th sau khi 5 L mu th dng trong php th


carbon monoxyd c rt ra khi bnh kh. Dn kh chy
qua dung dch cha kali permanganat 2,5 % (kl/tt) v acid
sulfuric 1,2 % (kl/tt) v chy vo ng ly mu chn khng c
dung tch 1 L vi tc kh l 15,0 L/gi. Dn kh cho n khi
p sut trong ng t c 50 mm di p sut kh quyn,
o theo p k thu ngn. Tnh th tch kh 20C v 760 mm
Hg.
Dung dch acid sulfanilic/naphthylendiamin (TS):
- Dung dch I: Ha tan 2 g acid sulfanilic (TS) vo hn
hp 10 ml acid acetic bng v 180 ml nc.
- Dung dch II: Ha tan 0,2 g naphthylendiamin
dihydroclorid vo 10 ml dung dch acid acetic bng
50% (tt/tt) un nng nh v pha long thnh 200 ml
bng nc.
Trn 9 th tch dung dch I vi 1 th tch dung dch II
Tin hnh
Cho 20,0 ml dung dch acid sulfanilic /naphthylendiamin (TS)
vo ng ly mu bng cch nhng y ng vo a cha hn
hp v cn thn m vi kha. Lc ng, sau yn trong
10 pht (thnh thong lc mt ln). Chun b dung dch i
chng bng cch thm 0,25 ml dung dch natri nitrit
0.00308% (kl/tt) vo 20,0 ml dung dch acid sulfanilic
/naphthylendiamin (TS). o hp th quang ca lp dung
dch thu c dy 1 cm ti bc sng 550 nm v hiu chnh
kt qu theo 1,0 L kh ti 20C v 760 mmHg.
hp th quang o c th nghim ca 1,0 L mu th
khng c vt qu gi tr tng ng ca dung dch i
chng.

Cc halogen v
hydrogen sulfid

Ch : Trong th nghim sau, phi dn kh vo mt bnh thy


tinh kn, y phng. ng ny c ni vi (a) mt ng dn c
ng knh trong 1 mm; cch y bnh 2 mm v (b) ng dn
kh ra. ng dn kh c nhng ngp trong thuc th
su t 12 n 14 cm.
Cho 10,0 L mu kh th chy qua 49 ml nc c cha 1 ml
dung dch bc nitrat (TS). Dung dch khng b sm mu. Sau
5 pht, nu nh dung dch b c, c mu trng sa, c
ca dung dch khng c php m hn c ca ca
hn hp gm 1 ml dung dch bc nitrat (TS), 20 ml dung dch
clorid chun (5 mg Cl/1L) v 0,15 ml acid nitric long (TS),
c pha long bng nc thnh 50 ml v yn trong 5
pht.

Arsin v phosphin

Dung dch DDC bc/Quinolin (TS): ha tan 50 mg bt mn


bc nitrat vo 100 ml quinolin v thm vo 0,2 g bc
diethyldithiocarbamat. S dng thuc th ngay sau khi pha.
Tin hnh: dn 10,0 L kh th, tc 1,0 L/pht chy qua
mt ng thy tinh nhi bng tm dung dch ch acetat (TS) c
u sc kh hnh vm bng thy tinh xp, xp 100, vo
mt ng c ng knh trong khong 2,5 cm, c cha 5 ml
11

QCVN 4 -17: 2010/BYT


dung dch DDC bc/Quinolin (TS). u sc kh gn nh tip
xc vi y ca ng. Mu ca dung dch DDC bc/Quinolin
(TS) khng c thay i.

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QCVN 4 -17: 2010/BYT


6.3. nh lng

Dng buret kh (xem hnh v) c dung tch 100 ml. Phn trn
ca buret c vi 2 chiu gn vi 2 ng mao qun, mt ng
mao qun (ng A) c dng a kh vo thit b, ng
mao qun kia (ng B) c ni vi sinh hn (C) v p k
(M). Phn dui ca buret c vi 1 chiu ni vi bnh thy
ngn bng mt ng cao su. Phn trn ca buret kh c
chia t 0 n 5 ml, theo thang 10 vch/1 ml; v phn di
c chia t 99,5 n 100,5 ml, theo thang 10 vch/1 ml.
ng mao qun (B) c ni vi mt ng ni mao qun thng
ng to thnh khp ni 4 chiu, phn di ng ni ca
khp ni c ni vi mt ng ngng sinh hn (C) c dung
tch 60 ml. ng bn phi ca khp ni c ni vi mt p
k thy ngn (M). Vi (D) ca ng ni trn m thng vi
khng kh bn ngoi.

ng 3 vi kh li v nhng ng sinh hn vo nitrogen lng


n ngang phn trn ca ng sinh hn. Bng cch iu chnh
vi 2 chiu v bnh thy ngn ng, to mi trng bn chn
khng trong h thit b vi p sut ty t Po 50 n 60 mm
Hg (o chnh xc). p sut ny phi c gi khng i
trong 10 pht hin th rng thit b kn kh.
M vi 2 chiu vo ng (A) v lp y buret v ng (A) bng
thy ngn. ng vi 2 chiu. Ni ng cao su vo van thot
kh ca bnh ng nitrogen oxyd v cho dng nitrogen oxyd
chy qua ng cao su trong 1 pht. Trong khi cho kh chy
qua, ni ng cao su vi ng (A) v ngay lp tc m vi 2
chiu vo ng (A). Cho 100 ml nitrogen oxyd chy vo buret
bng cch h thp bnh thy ngn. ng vi 2 chiu li.
Nng bnh thy ngn cao trn ng (A) v h thp mc
nitrogen lng xung ngang mc gia ng sinh hn. Cn thn
m vi buret ni thng vi sinh hn hi lu v cho thy ngn
dng vo buret n ngang vi. ng vi li. Nng mc
nitrogen lng ln sao cho ngp ton b sinh hn. c s ch
p sut v i n khi p sut n nh trong vng 2 pht.
t bnh thy ngn vo v tr y, m vi buret ni thng vi
sinh hn hi lu. Dch chuyn bnh thy ngn sao cho s ch
13

QCVN 4 -17: 2010/BYT


trn p k bng vi p sut ban u Po. ng vi buret li v
bng cch dch chuyn bnh thy ngn to p sut kh trong
buret bng vi p sut kh quyn. Th tch kh trong buret
(ml) biu th th tch kh khng ngng t trong 100 ml kh
nitrogen oxyd. Th tch kh khng ngng t khng c qu
3 ml. C sau mi lot 10 th nghim li cho khng kh vo
buret bng cch m vi (D), tho ht nitrogen lng ra khi
sinh hn v sinh hn m n nhit phng.

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