CNG HA X HI CH NGHA VIT NAM

QCVN 4-4 : 2010/BYT

QUY CHUN K THUT QUC GIA

V PH GIA THC PHM - CHT CHNG NG VN
National technical regulation on Food additives - Anticaking agents

H NI - 2010

Li ni u
QCVN 4-4 :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 21/2010/TT-BYT
ngy 20 thng 5 nm 2010 ca B trng B Y t.

QUY CHUN K THUT QUC GIA

V PH GIA THC PHM - CHT CHNG NG VN
National technical regulation on Food additives Anticaking agents
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 chng ng vn 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 chng ng vn 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 chng ng vn: l ph gia thc phm c s dng vi mc ch
gim s kt dnh gia cc thnh phn ca thc phm.
3.2. JECFA monograph 1 - Vol. 4 (JECFA monographs 1 - Combined
compendium of food addiditive 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. PTWI (Provisional Tolerable Weekly Intake): Lng n vo hng tun tm
thi chu ng c.
3.7. INS (International numbering system): H thng m s quc t v ph gia
thc phm.
II. YU CU K THUT, PHNG PHP TH V LY MU
1. Yu cu k thut v phng php th i vi cc cht chng ng vn 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 mui ca cc acid bo.

1.2. Ph lc 2: Yu cu k thut v phng php th i vi oxyd magnesi.

1.3. Ph lc 3: Yu cu k thut v phng php th i vi cc mui natri,
kali, calci ferrocyanid.
1.4. Ph lc 4: Yu cu k thut v phng php th i vi dioxyd silic v
nh hnh.
1.5. Ph lc 5: Yu cu k thut v phng php th i vi calci silicat.
1.6. Ph lc 6: Yu cu k thut v phng php th i vi natri nhm silicat.
1.7. Ph lc 7: Yu cu k thut v phng php th i vi calci nhm silicat.
1.8. Ph lc 8: Yu cu k thut v phng php th i vi nhm silicat.
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 chng ng vn 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 chng ng vn
Vic kim tra cht lng, v sinh an ton i vi cc cht chng ng vn 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 yu cu 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 chng ng vn 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.

Ph lc 1
QUY NH K THUT V PHNG PHP TH I VI
MUI CA CC ACID BO
1. Tn khc, ch s

Salts of fatty acids

INS 470
ADI khng gii hn

2. nh ngha

Cc sn phm ny cha mui calci, kali v natri ca cc acid

myristic, oleic, palmitic, stearic hoc hn hp cc acid ny
thu c t m v du n. Sn phm thng mi cn c
phn loi da trn:
- Ch s x phng ha;
- im ng c ca cc acid bo thu c t cc mu
trn;
- Ch s iod;
- Cn cn li sau khi nung bao gm c hm lng cc
cation;
- m.

3. Cm quan

Tinh th rn hoc bn rn, bng, mu trng hoc vng nht,

hoc bt mu trng hoc trng vng.

4. Chc nng

Cht chng ng vn, Cht nh ha.

5. Yu cu k thut
5.1. nh tnh
tan

Cc mui kali v natri tan trong nc v ethanol, cc mui

calci khng tan trong nc, ethanol v ether.

Cation

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

Thnh phn acid bo

S dng Phng php nh lng nhn dng tng mu

bo. Cc acid bo chim lng ln nht phi ph hp vi
thnh phn cng b trn nhn sn phm.

5.2. tinh khit

Cc acid bo t do

Khng c qu 3,0%.

Cc cht khng x
phng ha

Khng c qu 2,0%.

Ch

Khng c qu 2,0 mg/kg.

5.3. Hm lng cc
mui acid bo

Khng thp hn 95,0% tng cc mui acid bo, tnh theo

khi lng kh.

6. Phng php th
6.1. nh tnh
Cation

un nng 1 g mu th vi hn hp gm 25 ml nc v 5 ml
acid hydrocloric. Cc acid bo to thnh ni trn b mt
thnh mt lp rn hoc du, tan trong hexan. Sau khi lm
ngui, gn ly lp nc v cho bay hi n kh. Ha tan
cht rn cn li trong nc v th cc cation thch hp.

6.2. tinh khit

Cc acid bo t do

Xc nh cc acid bo t do theo hng dn trong phn

Phng php xc nh Acid bo t do. Tnh hm lng acid
bo t do, s dng h s tng ng (e) bng vi 1/10
khi lng phn t ca mui.

Cc cht khng x
phng ha

Cc cht khng x phng ha l ton b lng sn phm c

mt trong cc cht bo sau khi c x phng ha vi cc
hydroxyd kim loi kim v chit bng mt dung mi nht
nh, vn khng bay hi trong cc iu kin xc nh ca
php th.
Cc cht ny bao gm cc lipid c ngun gc t nhin nh
cc sterol, cc ru no mch di hn, cc phm mu v cc
hydrocarbon cng nh bt k mt tp cht no khng bay
hi 1030C c mt trong sn phm.
Cn khong 5 g (chnh xc n 0,01 g) mu th c
trn u vo bnh cu y trn 250 ml. Thm 50 ml dung
dch kali hydroxyd ~ 0,5 N v thm mt t bt. Gn bnh
vo sinh hn hi lu, un nh trong 1 gi. Ngng un. Thm
100 ml nc ct qua u sinh hn v lc.
Sau khi lm mt, chuyn dung dch vo phu chit. Trng
ra bnh v bt vi ln bng diethyl ether (tng cng
khong 100 ml) v dch ra vo phu tch. ng nt v
lc mnh trong 1 pht, u n x p sut bng cch lt
ngc phu tch v m kha vi.
yn phu tch cho n khi 2 pha hon ton tch lp. Sau
rt ly cng trit cng tt dung dch x phng vo phu
chit th 2.
Chit dung dch x phng ethanol trong nc thm hai ln
na, mi ln vi 100 ml diethyl ether theo cch trn. Gp 3
dch chit ether vo 1 phu tch c sn 40 ml nc.
Nh nhng quay trn phu tch cha dch chit v 40 ml
nc. Nu lc qu mnh trong giai on ny, nh tng c
th hnh thnh. hn hp tch lp hon ton v rt b lp
nc di. Ra lp ether hai ln na vi 40 ml nc, lc
u v loi b lp nc di sau khi hn hp phn lp.
Vi mi dung dch ra rt ra 2 ml, sau quay trn phu
tch quanh trc, i vi pht, rt b phn tch ra, ng kha
vi khi ether bt u chy qua.
Ra dung dch ether nhiu ln bng 40 ml dung dch kali
hydroxyd 0,5 N, 40 ml nc, ra thm mt ln bng 40 ml

dung dch kali hydroxyd, sau ra t nht 2 ln na bng

40 ml nc. Lin tc ra bng nc cho n khi dung dch
ht mu hng khi th bng ch th l dung dch
phenolphthalein.
Chuyn nh lng tng lng nh dung dch ether qua u
ca phu tch vo bnh cu sy kh v cn b (chnh
xc n 0,0001 g).
Lm bay hi dung mi bng cch ct trn b cch thy
nc si. Thm 5 ml aceton v loi b hon ton dung mi
bay hi bng cch thi khng kh nh, nghing bnh cu khi
quay trong b cch thy.
Sy kh phn cn cn li nhit 1032 C trong 15 pht,
t bnh cu theo phng gn nh nm ngang. Lm ngui
trong bnh ht m v cn (chnh xc n 0,0001 g). Lp li
qu trnh sy trong mi 15 pht lin tip cho n khi chnh
lch gia 2 ln cn lin tip nh hn 0,0015g.
Ch : Nu khng thu c khi lng khng i sau 3 ln
sy kh, cc cht khng x phng ha c th b nhim
bn.
Sau khi cn, ha tan phn cn trong 4 ml diethyl ether,
thm 20 ml ethanol c trung ha (dung dch c mu
hng khi thm ch th l dung dch phenolphthalein(TS).
Chun bng dung dch kali hydroxyd trong ethanol 0,1 N
chun ha (pha dung dch kali hydroxyd trong ethanol c
nng gn ng 1 N bng cch ha tan 60 g kali hydroxyd
trong 50 ml nc v nh mc thnh 1 l bng ethanol; pha
long dung dch ny 1:10 bng ethanol) n khi dung dch c
mu pht hng.
Hiu chun khi lng cn cn li theo hm lng acid t
do trong mu trng. Tnh hm lng cht khng x phng
ha, theo % (kl/kl) bng cng thc sau:
[100 (m1 0,281 T V)] / m
trong :
m = khi lng (g), ca phn mu th,
m1 = khi lng (g), ca cn cn li.
V = th tch dung dch kali hydroxyd chun ha nng
dng chun .
T = Nng chnh xc ca dung dch kali hydroxyd dng
chun .
Ch

Th theo JECFA monograph 1 - Vol. 4.

S dng k thut hp th nguyn t thch hp vi hm
lng ch nh xc nh. La chn c mu th v phng
php chun b mu da trn nguyn tc ca phng php
m t ti JECFA monograph 1 - Vol. 4 phn cc phng
php phn tch cng c).

6.3. nh lng

Nguyn tc:
X phng ha cc mui v ester ha cc acid bo bng
methanol, c mt bo triflorid, methanol kim. Tin hnh sc
k kh lng ca cc ester methyl ca acid bo.
Phn A - Chun b cc ester methyl ca acid bo
Thit b
- Bnh y trn c nhm 50 v 100 ml.
- Sinh hn hi lu, chiu di hiu dng 20 n 30 cm, c
khp ni nhm tng thch vi bnh cu.
- Cc phu tch 250 ml.
- ng ng vo dn kh nit.
- ng nghim c nt thy tinh nhm.
- Pipet chia , c th tch t nht l 10 ml, c gn qu bp
cao su, hoc pipet t ng.
Thuc th
- Heptan, dng cho sc k (Ch 2 v 4)
- Du nh c ct li (nhit si t 40-60 ), ch s
brom < 1, khng c cn, hoc hexan (Ch 2)
- Natri sulfat khan
- Dung dch Natri hydroxyd trong methanol ~ 0,5 N: Ha tan
2g natri hydroxyd trong 100 ml methanol cha khng qu
0,5% (kl/kl) nc. Nu gi dung dch tng i lu c th to
thnh mt lng nh kt ta mu trng ca natri. iu ny
khng nh hng n kt qu iu ch methyl ester.
- Dung dch bo triflorid trong methanol, 12 n 25% (kl/kl) .
Ch phm thng mi sn c l dung dch 14 v 50% (ch
2)
Cnh bo: Bo triflorid c. V vy th nghim vin khng nn
pha dung dch bo triflorid trong methanol t methanol v
boron triflorid. (ch 3).
- Dung dch bo ha natri clorid trong nc.
- Dung dch methyl, 1 g/l trong ethanol 60% (tt/tt)
- Nit, c hm lng oxy < 5 mg/kg
Tin hnh
Do bo triflorid c, cc th nghim sau tt nht nn tin hnh
trong t ht. Cc dng c thy tinh phi c ra bng nc
ngay sau khi s dng.
Sy kh mu nhit 105 C n khi lng khng i, c
2 gi th kim tra khi lng 1 ln. Cn khong 350 mg (chnh
xc n mg) mu sy kh. C th ly lng mu ln hoc
nh hn 350 mg, tuy nhin, th tch ca bnh cu v lng
thuc th s dng phi ph hp vi s liu trong bng sau:

khi lng
NaOH 0.5 Dung dch BF3
Th tch bnh
mu
N
trong methanol
(mg)
(ml)
(ml)
(ml)
100-250
50
4
5
250-500
50
6
7
500-700
100
8
9
750-1000
100
10
12
Cho lng acid bo nh vo bnh cu ph hp. Thm vi
lng ph hp dung dch bo triflorid trong methanol. un si
trong vng 2 pht.
Thm 2 n 5 ml heptan (ch 4) (lng chnh xc khng
nh hng n phn ng) qua u trn ca sinh hn vo
hn hp ang un si v tip tc un si trong 1 pht.
Ngt ngun nhit, ly sinh hn ra. Thm lng nh dung
dch natri clorid bo ha v lc nh bnh bng cch quay trn
bnh vi ln.
Thm dung dch natri clorid bo ha vo bnh cu sao cho
mc cht lng ngang c bnh. yn cho hn hp tch lp
v chuyn khong 1 ml lp trn (lp heptan) vo ng nghim
c nhm v thm vo mt lng nh natri sulfat khan loi
ht nc. Nu lng mu ly l 350 mg, dung dch ny cha
khong 7-17% methyl ester v c th bm trc tip vo ct
sc k kh-lng. Nu khng th pha long dung dch bng
heptan t c nng methyl ester l 5-10% (ch 5).
thu hi ton b lng ester kh, chuyn dung dch mui
v lp heptan vo phu tch. Tch ring cc lp. Chit phn
dung dch mui 2 ln bng 50 ml du nh. Gp dch chit du
nh thu c vo phn dung dch heptan, ra bng 20 ml
nc n khi ht acid (th bng ch th methyl). Lm kh
bng natri sulfat khan, lc v cho bay hi dung mi trong b
cch thy v thi kh nit (ch 6 v 7). Vi cc mu c khi
lng nh hn 500 mg phi gim th tch dung mi v nc
s dng theo t l tng ng.
Bn cnh phng php trn cn c mt s phng php
khc khng s dng n bo triflorid. C th thay cc thuc th
methyl ha, nh dung dch natri hydroxyd 0,5N trong methanol
v dung dch bo triflorid 12-25 %, trong methanol bng:
- Kali hydroxyd 1 N trong methanol, (phn ng vi cht bo
khi c mt lng d methanol c hm lng nc nh);
- Dung dch natri methylat (iu ch bng cch ha tan 1 g
natri kim loi trong 100 ml methanol c hm lng nc
nh).
Ch
1. Nu cc cht khng x phng ha gy cn tr, pha long
dung dch x phng ha vi nc v loi b cc cht khng
x phng ha bng cch chit vi diethyl ether hoc hexan.
Acid ha dung dch nc x phng v tch ly cc acid bo.
iu ch cc methyl ester t cc acid bo theo hng dn.

2. Khi o sc k kh lng ca cc methyl ester, mt s thuc

th, c bit l bo triflorid trong methanol c th to nn cc
pic ngu nhin trn sc (trong vng cc ester c mch
C20-C22 nu dng bo triflorid trong methanol). Do vy cn
phi kim tra li mi t thuc th mi bng cch iu ch
cc methyl ester ca acid oleic tinh khit, v o sc k. Nu
xut hin pic ngu nhin, phi b khng dng thuc th. Cc
thuc th khc nhau khng c php cho pic gy nhiu n
cc pic ca cc methyl ester ca cc acid bo trong qu trnh
chy sc k.
Dung dch bo triflorid trong methanol phi c bo qun
trong t lnh.
3. Nu bt buc phi iu ch dung dch bo triflorid t bo
trifluorid dng kh, nn dng phng php sau: Cn khi
lng ca bnh cu 2 l cha 1 l methanol. Lm lnh trong b
nc . Vn gi nguyn bnh trong b nc , sc kh
BF3 t chai kh (cylinder) qua ng dn thy tinh vo dung
dch methanol cho n khi hp th c 125 g BF3. Tin
hnh th nghim trong t ht. Phi cho BF3 chy qua ng
thy tinh trc khi t ng vo v rt ng ra khi methanol
trnh trng hp cht lng b ht vo h thng van ca chai
kh. Khng c cho kh chy nhanh qu c hi kh trng
ra khi bnh. Thuc th pha theo cch ny bn trong 2 nm.
4. Nu mu khng c cc acid bo cha 20 hoc nhiu hn
20 nguyn t carbon, c th thay heptan bng hexan (hn
hp ca cc ng phn C7 tinh khit c th c kim tra
bng sc k kh lng)
5. Nu khng c lng mu nh yu cu, c th ly 10
mg, thm ch t hn, min l lng thuc th v kch thc
ca cc dng c thy tinh c gim theo t l tng ng.
6. Cc dung dch methyl ester cn c phn tch cng sm
cng tt. Nu cn, bo qun dung dch heptan cha cc
methyl ester trong mi trng kh tr trong t lnh. Nu cn
phi bo qun trong thi gian di, nn bo v cc methyl ester
khi s oxi ha bng cch thm vo dung dch cc cht chng
oxi ha nng khng nh hng n kt qu phn tch, v
d nh 0,05 g/l EHT (2,6-di-tert-butyl-4-methyl phenol).
Trong trng hp cn thit, c th bo qun cc methyl ester
kh sch dung mi bng kh tr trong t lnh trong 24 gi,
hoc lu hn nu gi ng lnh su trong ng kn trong
chn khng.
7. Mt phn cc methyl ester d bay hi nht c th b mt
nu thi gian bay hi dung mi ko di, hoc nu dng kh
nit qu mnh,
o ph hng ngoi, phi loi b dung mi cng trit
cng tt.
o sc k kh lng, loi b dung mi.

Phn B - Sc k kh lng i vi cc ester methyl ca acid

bo
Thit b
Thit b thng thng dng cho sc k kh lng, dng ct nhi
v detector ion ha ngn la (ch 1). Bt k mt thit b
no cho hiu qu v phn gii cao vi cht bo cn xc
nh u ph hp.
Sc k kh lng
H thng bm mu: H thng bm mu phi c khng gian
cht nh nht c th. Nu c, phi nng c nhit
cao hn nhit ct t 20 n 50 C.
L: L phi cung cp cho ct nhit t nht l 220oC v phi
duy tr c nhit cn thit trong khong 1 C.
Nu dng chng trnh t nhit , nn dng thit b c ct i.
Ct nhi:
- Ct: Ct phi c lm t vt liu tr vi cht cn phn
tch: thy tinh hoc nu khng th dng thp khng r (ch
2). Chiu di: 1 n 3 m, nn dng ct tng i ngn nu
c cc acid mach di (C20+). xc nh cc acid bo C4 v
C6, nn dng ct 2 m; ng knh trong t 2 n 4 mm.
Nhi ct
- Cht mang: Diatomit ra acid v c silan ha, hoc
cc cht mang tr ph hp khc c khong bin thin
ng knh hp (25 m) trong khong c ht t 125-200 m,
c ht trung bnh phi tng ng vi ng knh trong v
chiu di ct.
- Pha tnh: Dng polyester ca mt cht lng phn cc (v d
diethylen glycol polysuccinat, butandiol polysuccinat, ethylen
glycol polyadipat ...) hoc bt k cht lng no khc (v d
cyanosilicon ...) tha mn cc iu kin di y. Pha ng
phi chim 5 n 20 % dung lng nhi. Dng mt pha tnh
khng phn cc, ty theo tng php tch c th.
- Hot ha ct mi ch to: Tho ct ra khi detector. Nu c
th, t t nng nhit l n 185 C v dn dng kh tr
qua ct vi tc 20-60 ml/pht trong t nht l 16 gi ti
nhit ny, v thm 2 gi na ti 195 C.
Detector: Cc vn hnh di y tng ng vi detector ion
ha ngn la (ch 1)
Syring: c dung tch ti a l 10 l, chia n 0,1 l.
My ghi:
Nu s dng ng ghi tnh thnh phn hn hp phn
tch, phi dng mt my ghi in t c chnh xc cao.
My ghi phi tng thch vi thit b o. Cc c trng ca
my o phi nh sau:
- Tc p ng di 1,5 giy, tt nht l di 1 giy (tc
p ng l thi gian cn bt ghi chy t 0 n 90 %
theo 100 % tn hiu)

- rng ca giy: ti thiu l 25 cm

- Tc giy: 25-100 cm/gi.
B tch phn Integrator hoc my tnh (ty chn)
C th tnh mt cch nhanh v chnh xc nu dng b tch
phn in t hoc my tnh. Trong trng hp ny phi c
c tn hiu tuyn tnh vi nhy ph hp, v hiu chnh
cho lch ng nn phi tha ng.
Ha cht
- Kh mang: Kh tr (nit, heli, argon ...) kh, v cha t hn
10 mg/kg oxy.
- Kh ph tr: Hydro (tinh khit ti thiu 99,9%) khng c cc
tp cht hu c, khng kh hoc oxy.
- Cc cht chun so snh: Hn hp ca cc methyl ester,
hoc cc ethyl ester ca mt cht du bit trc thnh
phn, tt nht l tng t vi cht bo cn phn tch.
Tin hnh
iu kin th
Xc nh cc iu kin chy ti u: Cc gi tr cho trong bng
1 v 2 cho di y v nguyn tc c th cho cc kt qu
mong mun:
Bng 1
ng knh trong ca ct
Kh mang cung cp
2 mm
15-25 ml/pht
3 mm
20-40 ml/ pht
4 mm
40-60 ml/ pht
Bng 2
Nng ca pha tnh
Nhit
5%
175 oC
10%
180 oC
15%
180 oC
20%
185 oC
Nu c, injector phi nhit khong 200 oC v
detector phi nhit bng hoc cao hn nhit ct.
V nguyn tc dng kh hydro cung cp cho detector ion ha
ngn la phi c tc bng mt na tc kh mang, v
tc kh oxy phi bng khong 5 n 10 ln tc kh
hydro.
Xc nh hiu sut v phn gii (ty chn)
Tin hnh phn tch mu chun methyl stearat. La chn
kch thc mu, nhit ct tch v tc kh mang sao
cho pic ca methyl stearat xut hin 15 pht sau pic dung
mi v cao khong 3/4 tn hiu ton thang.
- Phn tch:
Dng mu kim tra l 0,1 n 2 l dung dch heptan ca cc
methyl ester, pha theo hng dn trong phn A. Trong
trng hp khng c cc ester trong dung dch, chun b
dung dch c nng khong 10% trong heptan v bm 0,1
n 1 l dung dch ny.

Cc iu kin tin hnh c cho di y. Tuy nhin, c

th lm vic vi nhit ct thp hn nu xc nh cc acid
c mch carbon di C12 hoc nhit cao hn nu xc
nh cc acid bo trn C20.
i khi c th s dng chng trnh t nhit cho c 2
trng hp trn. Nu mu c cha cc methyl ester ca cc
acid bo di C12, phi bm mu nhit 100 C (hoc
nhit t 50 60 C nu c acid butyric) v ngay lp tc
tng nhit vi tc tng nhit t 4 - 8 C/pht ty chn.
Trong mt s trng hp c th gp c 2 qui trnh li: sau khi
tng nhit, tip tc ra gii ti nhit khng i cho n khi
tt c cc hp phn c ra gii ra. Nu thit b khng vn
hnh vi chng trnh nhit , lm vic ti 2 nhit c
nh trong khong t 100 n 195 C.
Biu th kt qu
Phn tch nh tnh
Phn tch hn hp cht chun so snh c thnh phn
bit trong cc iu kin s dng o mu th. o khong
cch lu (hoc thi gian lu) cho cc ester bo tng ng.
Dng giy bn logarit, v th biu din s ph thuc ca
logarit khong cch lu (hoc thi gian lu) vo s nguyn
t carbon ca cc acid; trong iu kin ng nhit th ca
cc ester mch thng c cng khng bo ha phi l cc
ng thng. gn nh song song vi nhau.
Nhn dng cc pic ca mu th t cc th ny, nu cn
th dng php ni suy. Phi trnh cc iu kin o lm xut
hin cc pic b che ph (masked peaks), c ngha l
phn gii khng ln tch c 2 hp phn.
Phn tch nh lng
Xc nh thnh phn
Tr cc trng hp c bit, s dng phng php chun
ha din tch, c ngha l gi thit rng ton b cc hp phn
u c biu din trn sc , sao cho tng din tch cc
pic th hin 100 % cc hp phn (tng ra gii).
Bng mt qui trnh chun ha ph hp (dng hn hp cht
chun tham chiu hoc dng cht chun ni), xc nh tng
khi lng ca cc acid bo trong mu kh. Tnh hm lng
mui ca cc acid bo vi cc cation c trng trong mu.
Tng hm lng Mui Acid Bo khng c ln hn 95%
khi lng mu kh. Ngoi ra, nu c cc ch tiu cho hm
lng ca mi acid bo ghi trn nhn sn phm, mu phi
tha mn c cc ch tiu ny.
Ch
1. C th s dng my sc k kh - lng dng thit b o
dn nhit ca kh (catharometer) (lm vic trn nguyn tc
o s thay i dn nhit). Cc iu kin o khi c
thay i nh sau:

Ct
- chiu di: 2 n 4 m
- ng knh trong: 4 mm
- cht mang: ng knh ht trong khong 160 n 200 m
- pha tnh: 15 n 25%
Kh mang: heli, nu khng th dng hydro, c hm lng oxy
cng nh cng tt. Khng dng kh ph tr
- Tc kh: thng trong khong t 60 n 80 ml/pht
Nhit
Injector: cao hn t 40 oC n 60 oC so vi nhit ct
Ct: 180 oC to 200 oC
Phn tch nh lng: phi hiu chnh theo cc h s thu
c khi phn tch hn hp so snh ca cc ester c thnh
phn bit trong cng iu kin o vi mu th.
2. Nu trong mu c cc thnh phn khng no cha nhiu
hn 3 ni i, chng c th b phn hy trn ct thp khng r.

Ph lc 2
QUY NH K THUT V PHNG PHP TH I VI MAGNESI OXYD
1. Tn khc, ch s

INS 530
ADI khng gii hn

2. nh ngha
Tn ha hc

Magnesi oxyd

M s C.A.S.

1309-48-4

Cng thc ha hc

MgO

Khi lng phn t

40,31

3. Cm quan

Dng bt trng, bng, thng gi l magnesi oxyd nh

hoc dng bt trng tng i cht, thng gi l magnesi
oxyd nng. 5g magnesi oxyd nh chim th tch t 40 n
50 ml, trong khi 5 g magnesi oxyd nng chim th tch t
10 n 20 ml.

4. Chc nng

Cht chng ng vn

5. Yu cu k thut
5.1. nh tnh
tan

Thc t khng tan trong nc, khng tan trong ethanol.

Tnh kim

Mu th c tnh kim vi giy qu t.

Magnesi

Phi c phn ng c trng ca magnesi.

5.2. tinh khit

Gim khi lng khi sy
kh

Khng c qu 5,0% sau khi nung nhit t 800 oC

n 825oC n khi lng khng i

Kim (t do) v cc mui

ho tan

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

Calci oxyd

Khng c qu 1,5%.

Ch

Khng c qu 2,0 mg/kg.

5.3. Hm lng MgO

Khng c thp hn 96,0% sau khi nung nhit

khong 800 oC.

6. Phng php th
6.1. nh tnh
Magnesi

Phi c phn ng c trng ca magnesi.

6.2. tinh khit

Kim (t do) v cc mui
ho tan

Cn 2 g mu th, chnh xc n mg, ho tan vo 100 ml

nc ct v un si trong 5 pht trong mt cc thu tinh c
np v lc nng. Ly 50 ml dch lc ngui, cho thm

ch th methyl (TS) v chun vi dung dch acid

sulfuric 0,1 N. Th tch acid s dng chun khng
c qu 2 ml. Cho bay hi 25 ml dch lc n kh v sy
kh 105 oC trong 1h. Lng cn cn li khng c qu
10 mg.
Oxyd calci

Cn 400 mg mu th, chnh xc n 0,1 mg, ho tan vo

mt hn hp gm 3 ml dung dch acid sulfuric v 22 ml
nc ct. Cho thm 50 ml ethanol v yn hn hp qua
m. Nu tinh th ca magnesi sulfat tch ra, ho tan bng
cch lm nng hn hp n 50 0C. Lc qua chn lc bng
s nung trc v cn b, sau ra kt ta vi ln bng
hn hp ethanol v acid sulfuric long (TS) vi t l th tch
2:1. Nung chn v cn, ngui v cn. Khi lng
calci sulfat thu c nhn vi 0,4119, tng ng vi
lng calci oxyd c trong mu th.

Ch

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

- Xc nh bng k thut 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 ti JECFA monograph 1 - Vol. 4 phn cc phng
php phn tch cng c.

6.3. nh lng

Nung khong 400 mg mu th n khi lng khng i

nhit t 800-825 oC trong mt chn platin cn b. Cn
chnh xc mu th sau khi nung v ha tan trong 25,0 ml
acid sulfuric 1N, un si nh loi ht carbon dioxyd, sau
ngui. Thm dung dch ch th methyl (TS) v
chun acid d bng dung dch natri hydroxyd 1 N. Ly
th tch dung dch acid sulfuric 1N thc s dng trn tr
i th tch dung dch acid sulfuric tng ng lng CaO
trong mu th (h s tng ng l 1 ml dung dch acid
sulfuric 1N tng ng vi 28,04 mg CaO). Hiu s ny
chnh l th tch dung dch acid sulfuric dng trung ho
oxyd manegsi.
Mi ml dung dch acid sulfuric 1N tng ng vi 20,16
mg MgO.

Ph lc 3
QUY NH K THUT V PHNG PHP TH I VI
CC MUI NATRI, KALI, CALCI FEROCYANID
1. Tn khc, ch s

Sodium ferocyanide, Potassium ferocyanide, Calcium

ferocyanide; Yellow prussiate of lime, potash, soda; natri,
calci, kali hexacyanoferrat
INS 535 (natri ferocyanid)
INS 536 (Kali ferocyanid)
INS 538 (Calci ferocyanid)
ADI = 0 - 0,025 mg/kg th trng

2. nh ngha
Tn ha hc
Ch s C.A.S.

Cng thc ha hc

Natri, kali, calci ferocyanid;

Natri, kali, calci hexacyanoferrat II.
13601-19-9 (natri ferocyanid)
13943-58-3 (Kali ferocyanid)
1327-39-5 (Calci ferocyanid)
Na4Fe(CN)6.10H2O
K4Fe(CN)6.3H2O
Ca2Fe(CN)6.12H2O

Khi lng phn t

484,1 (natri ferocyanid)

422,4 (Kali ferocyanid)
508,3 (Calci ferocyanid)

3. Cm quan

Tinh th hoc bt tinh th mu vng.

4. Chc nng

Cht chng ng vn

5. Yu cu k thut
5.1. nh tnh
tan

Tan trong nc, cc mui K, Na khng tan trong ethanol.

Ferocyanid

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

Natri (i vi mui natri)

Phi c phn ng c trng ca natri.

Kali (i vi mui kali)

Phi c phn ng c trng ca kali.

Calci (i vi mui calci)

Phi c phn ng c trng ca calci.

5.2. tinh khit

Cyanid

Khng pht hin.

Fericyanid

Khng pht hin.

Arsen

Khng c qu 3,0 mg/kg.

Ch

Khng c qu 5,0 mg/kg.

5.3. Hm lng
ferocyanid

Khng c thp hn 99,0% tng ng theo ferocyanid.

6. Phng php th
6.1. nh tnh
Ferocyanid

Ly 10 ml dung dch mu th 10%, thm 1 ml dung dch st

(III) clorid (TS), xut hin kt ta mu xanh sm.

6.2. tinh khit

Cyanid

Ha tan 10 g ng sulfat vo hn hp gm 8 ml nc v 2
ml dung dch amoniac (TS). Tm t 1 bng giy lc bng
dung dch ny, cho bng giy lc tm ha cht vo
lung kh hydro sulfid. Khi nh 1 git dung dch mu th 1%
ln bng giy lc x l ha cht (c mu nu). Trn
bng giy khng c xut hin m trn mu trng.

Fericyanid

Ha tan khong 10 mg mu th trong 10 ml nc, nh 1

git dung dch ny ln lam knh (hoc phin s dng th
nh git). Thm 1 git dung dch ch nitrat 1%, tip theo l
vi git dung dch acid acetic 2 N lnh bo ha benzidin.
Khng c xut hin kt ta xanh hoc mu xanh.

Arsen

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

- Phng php II.

Ch

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

- Xc nh bng k thut 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 ti JECFA monograph 1 - Vol. 4 phn cc phng
php phn tch cng c.

6.3. nh lng

Cn khong 3 g (chnh xc n 0,1 mg) mu th cho vo

cc 400 ml. Ha tan trong 225 ml nc v thm cn thn
25 ml dung dch acid sulfuric (TS). Khuy u, trong khi
khuy thm 1 git dung dch orthophenanthrolin (TS) v
chun vi dung dch ceri IV sulfat 0,1 N n khi dung
dch chuyn t mu cam sang mu vng r rt.
Mi ml dung dch ceri (IV) sulfat 0,1 N tng ng vi:
48,41 mg Na4Fe(CN)6.10H2O
42,24 mg K4Fe(CN)6.3H2O
50,83 Ca2Fe(CN)6.12H2O

Ph lc 4
QUY NH K THUT V PHNG PHP TH I VI
SILIC DIOXYD V NH HNH
1. Tn khc, ch s

2. nh ngha

Silicon dioxyde, Silica

INS 551
ADI khng gii hn
Cc ch phm c quy nh bi quy chun ny bao gm:
silica dng aerogel (silic dioxyd kt ta); silicagel dehydrat.
Ch phm thng mi cn c phn loi da trn ch tiu
gim lhi lng khi l kh v cc mui c th ion ha.

Tn ha hc

Silic dioxyd

M s C.A.S.

7631-86-9

Cng thc ha hc

(SiO2)x

Khi lng phn t

60,09 (SiO2)

3. Cm quan

Silica dng aerogel: silica cu trc siu mn dng bt hay

ht nh.
Silica hydrat ha: l silic dioxyd kt ta, hydrat ha dng
bt v nh hnh, hoc ht.

4. Chc nng

Cht chng ng vn.

5. Yu cu k thut
5.1. nh tnh
tan

Khng tan trong nc v ethanol; Tan trong acid hydrofloric

v trong kim (80oC - 100oC).
(Cnh bo: acid hydrofloric rt c, c tnh n mn, khng
c tip xc vi da. Tin hnh thao tc trong t hood).

Silic

Phi c phn ng c trng ca silic.

5.2. tinh khit

Gim khi lng khi nung Khng c qu 6% tnh theo ch phm lm kh (sy
ti 105oC n khi lng khng i).
Ch

Khng c qu 5,0 mg/kg.

5.3. Hm lng SiO2

Dng aerogel: Khng thp hn 90,0% SiO2 tnh theo ch

phm sau khi nung.
Dng hydrat ha : Khng thp hn 89,0% SiO2 tnh theo
ch phm sau khi nung.

6. Phng php th
6.1. nh tnh
Silic

Th tnh bay hi ca SiF4. (Xem phn nh lng).

6.2. tinh khit

o
Gim khi lng khi nung Dng aerogel: nung ti 600 C n khi lng khng i.
Dng hydrat ha: nung ti 900 oC n khi lng khng
i.

Ch

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

Xc nh bng k thut 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).

6.3. nh lng

Cn khong 2 g (chnh xc n 0,1 mg) mu th, chuyn

vo mt chn nung platin cn b. Nung ti 1000 oC trong
1 gi, ngui trong bnh ht m v cn, tnh mc gim
khi lng (m1). Tm t tro vi 7 - 8 git ethanol, 3 git
acid sulfuric c v cn thn thm va acid hydrofloric
tm ht phn tro t. Cho bay hi n kh trn bp in
(95 - 105 oC), sau thm 5 ml acid hydrofloric, lc xoay
trn nh a ra thnh a v cho bay hi n kh.
Nung phn cn cn li trn ngn la bng n t
Meker, ngui trong bnh ht m v cn, tnh mc gim
khi lng (m2).
S chnh lch gia m1 v m2 biu th khi lng SiO2 trong
mu th.

Ph lc 5
QUY NH K THUT V PHNG PHP TH I VI CALCI SILICAT
1. Tn khc, ch s

2. nh ngha

Calcium silicate;
INS 552
ADI khng gii hn
Calci silicat hoc polysilicat c sn xut bng hng lot
cc phn ng gia cc hp cht cha silic (nh t
diatomit v cc hp cht calci t nhin (nh vi, vi thnh
phn gm cc nguyn t khc nh magnesi). Ch phm
thng mi cn c phn loi da trn cc yu t v
hm lng calci, silic dioxyd, gim khi lng khi lm kh,
gim khi lng khi nung, pH ca dung dch c trong
nc 10%, dung trng, m, sulfat v clorid.

Tn ha hc

Calci silicat

M s C.A.S.

1344-95-2

3. Cm quan

Bt rt mn mu trng hoc trng nh vi dung trng thp

v hp th nc cao.

4. Chc nng

Cht chng ng vn.

5. Yu cu k thut
5.1. nh tnh
tan

Khng tan trong nc v ethanol.

Silicat

Phi c phn ng c trng ca silicat

Calci

Phi c phn ng c trng ca calci

5.2. tinh khit

Florid

Khng c qu 50,0 mg/kg.

Aming

Khng c c.

Ch

Khng c qu 2,0 mg/kg.

6. Phng php th
6.1. nh tnh
Silicat

Cn khong 500 mg mu th, trn vi khong 200 mg

natri carbonat khan v 2 g kali carbonat khan, un nng
hn hp trn chn nung bng platin hoc niken n khi
hn hp chy hon ton. ngui v thm 5 ml nc,
yn trong 3 pht. un nh y chn nung tch phn b
nung chy ra khi chn. Dng 50 ml nc trng v
chuyn phn ny vo cc. Thm acid hydrocloric vo n
khi khng cn si bt, sau thm d 10 ml acid
hydrocloric, cho bay hi hn hp n kh trn b cch

thy nc si. Lm mt v thm 20 ml nc, un si v

lc hn hp qua giy lc khng tro. Cn silica khng tan
s b gi li trn giy lc (ch gi li phn dch lc th
calci). Chuyn phn cn keo vo mt a platin v thm
cn thn 5 ml acid hydrofloric (Cnh bo: acid hydrofloric
rt c, c tnh n mn, khng c tip xc vi da.
Tin hnh thao tc trong t hood). Ta rn s b ha tan
(nu khng tan lp li qu trnh cho bay hi vi acid
hydrofloric. un nng v gi mt a thy tinh (u a c
1 git nc) trong lung hi thot ra. Git nc u a
s tr nn c.
Calci

Trung ha dch lc thu c trong phn th silicat bng

dung dch amoniac (TS) dng ch th l 2 git dung dch
methyl (TS). Thm tng git dung dch acid hydrocloric
long (TS) n khi dung dch c tnh acid. Tip theo thm
dung dch amoni oxalat (TS), trong dung dch xut hin ta
calci oxalat. Ta ny khng tan trong acid acetic nhng
tan trong acid hydrocloric.

6.2. tinh khit

Florid

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

chuyn lun th gii hn florid phng php I hoc II.
- Cn 1 g mu

Aming

Phng php soi knh hin vi in t (tm thi): Mu th

c nghin ng nht n mc c th. S dng knh
hin vi in t quan st ti thiu 100 ln, kim tra tng
phn t ca mu, nu pht hin ra bt c vt liu dng si
th mu th khng t.

Ch

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

- Xc nh bng k thut 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 6
QUY NH K THUT V PHNG PHP TH I VI NATRI NHM SILICAT
1. Tn khc, ch s

2. nh ngha

Sodium aluminosilicate; Sodium silicoaluminate;

INS 554
ADI khng gii hn
Gm cc dng ca natri nhm silicat hydrat. Ch phm
thng mi cn c phn loi da trn hm lng nhm
oxyd, silic dioxyd, natri oxyd, gim khi lng khi lm kh,
gim khi lng khi nung v pH ca khi hn dch trong
nc.

Tn ha hc

Natri nhm silicat

3. Cm quan

Bt v nh hnh hoc ht nh mu trng, khng mi

4. Chc nng

Cht chng ng vn.

5. Yu cu k thut
5.1. nh tnh
tan

Khng tan trong nc v ethanol, t tan trong acid mnh v

hydroxyd kim.

Natri

Phi c phn ng c trng ca natri.

Nhm

Phi c phn ng c trng ca nhm.

Silicat

Phi c phn ng c trng ca silicat.

5.2. tinh khit

Ch

Khng c qu 5,0 mg/kg.

6. Phng php th
6.1. nh tnh
Silicat

Cn khong 500 mg mu th, trn vi khong 200 mg natri

carbonat khan v 2 g kali carbonat khan, un nng hn hp
trn chn nung bng platin hoc niken n khi hn hp
chy hon ton. ngui v thm 5 ml nc, yn trong
3 pht. un nh y chn nung tch phn b nung chy
ra khi chn. Dng 50 ml nc trng v chuyn phn
ny vo cc. Thm acid hydrocloric vo n khi khng cn
si bt, sau thm d 10 ml acid hydrocloric, cho bay hi
hn hp n kh trn b cch thy nc si. Lm mt v
thm 20 ml nc, un si v lc hn hp qua giy lc
khng tro. Cn silica khng tan s b gi li trn giy lc
(ch gi li phn dch lc th nhm). Chuyn phn cn
keo vo mt a platin v thm cn thn 5 ml acid
hydrofloric (Cnh bo: acid hydrofloric rt c, c tnh n
mn, khng c tip xc vi da. Tin hnh thao tc
trong t hood). Ta rn s b ha tan (nu khng tan lp li

qu trnh cho bay hi vi acid hydrofloric. un nng v gi

mt a thy tinh (u a c 1 git nc) trong lung hi
thot ra. Git nc u a s tr nn c.
6.2. tinh khit
Ch

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

- Xc nh bng k thut 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 7
QUY NH K THUT V PHNG PHP TH I VI CALCI NHM SILICAT
1. Tn khc, ch s

Aluminium calcium silicate; Calcium aluminosilicate;

Calcium silicoaluminate; sodium calcium silicoaluminate.
INS 556
PTWI = 1 mg/kg th trng

2. nh ngha
Tn ha hc

Calci aluminosilicat

3. Cm quan

Bt mn mu trng, trn chy.

4. Chc nng

Cht chng ng vn.

5. Yu cu k thut
5.1. nh tnh
tan

Khng tan trong nc v ethanol.

5.2. tinh khit

Gim khi lng khi nung Khng thp hn 14 % v khng c qu 18%.
(nung ti 1000o n khi lng khng i).
Gim khi lng khi sy

Khng c qu 10%.
(sy ti 105o trong 2 gi).

Florid

Khng c qu 50,0 mg/kg.

Ch

Khng c qu 5,0 mg/kg.

5.3. Hm lng SiO2,

Al2O3, CaO, Na2O

Khng thp hn 44,0% v khng c qu 50,0% SiO2

Khng thp hn 3,0% v khng c qu 5,0% Al2O3
Khng thp hn 32,0% v khng c qu 38,0% CaO
Khng thp hn 0,5% v khng c qu 4,0% Na2O.

6. Phng php th
6.1. tinh khit
Florid

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

chuyn lun th gii hn florid phng php I hoc II
- Cn 1 g mu v th.

Ch

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

- Xc nh bng k thut 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).

6.2. nh lng

Silic dioxyd:
Cn khong 500 mg (chnh xc n mg) mu th c
lm kh trc ti 105 oC trong 2 gi, cho vo cc 250 ml.
Ra thnh cc bng vi ml nc, sau thm 30 ml acid
percloric 72 % v 15 ml acid hydrocloric. un trn bp n
khi khi trng thot ra dy c. ngui v thm 15 ml
acid hydrocloric v un n khi khi trng bay ra. ngui
v thm 70 ml nc, lc qua giy lc Whatman No. 40
(hoc tng ng). Ra giy lc v ta nhiu ln bng
nc loi b hon ton acid percloric. Chuyn ton b
giy lc v ta vo chn nung platin cn b v nung ti
900o n khi lng khng i. Tm t tro bng vi git
nc, sau thm 15 ml acid hydrocloric v 8 git acid
sulfuric. un nng trn bp in n khi khi trng ca lu
hunh trioxyd xut hin. ngui, thm 5 ml nc, 10 ml
acid hydrofloric v 3 git acid sulfuric, sau cho bay hi
n kh trn bp. Cn thn un nng trn ngn la n khi
khng cn khi trng ca lu hunh trioxyd bay ra. Sau
nung ti 900o n khi lng khng i. S gim khi
lng t giai on thm acid hydrofloric biu th khi lng
SiO2 c trong mu th.
(Cnh bo: acid hydrofloric rt c, c tnh n mn, khng
c tip xc vi da. Tin hnh thao tc trong t hood)
Nhm oxyd:
un chy cn thu c trong phn xc nh dioxyd silic vi
2 g kali pyrosulfat trong 5 pht. ngui v ha tan trong
nc, cho vo bnh nh mc 250 ml, pha long n vch
bng nc. Ly 100 ml dung dch ny vo cc 600 ml,
thm 100 ml nc v 5 git xanh bromothymol (TS) v un
nng n si nh. Thm tng git amoni hydroxyd n khi
dung dch c mu xanh da tri, un si trong 5 pht ui
ht amoniac d. Lc qua giy lc Whatman No. 41 (hoc
tng ng), ra ta 6 ln, mi ln vi dung dch amoni
clorid 1/50 nng. Chuyn giy lc v cn vo chn nung
platin cn b, ha than giy lc v nung trn n Meker
n khi lng khng i. Khi lng cn sau khi tr i
khi lng tro ca giy lc nhn vi 2,5 biu th khi lng
Al2O3 trong mu th.
Calci oxyd:
Gp dch ra v dch lc trong phn xc nh silic dioxyd,
khuy u v dng buret 50 ml thm khong 30 ml dung
dch dinatri ethylendiamintetraacetat 0,05 M v 300 mg ch
th xanh hydroxynaphtol, tip tc chun n im tng
ng, dung dch c mu xanh da tri.
Mi ml dung dch dinatri ethylendiamintetraacetat 0,05 M
tng ng vi 2,804 mg CaO.
Natri oxyd:
Cn khong 500 mg (chnh xc n mg) mu th c
sy kh trc ti 105o trong 2 gi, chn nung platin cn
b. Tm t bng 8 - 10 git nc. Thm 25 ml acid

percloric 70% v 10 ml acid hydrofloric (Cnh bo: acid

hydrofloric rt c, c tnh n mn, khng c tip xc
vi da. Tin hnh thao tc trong t hood). un trn bp n
khi khi trng ca acid percloric thot ra. Thm 10 ml acid
hydrofloric v li un n khi c khi trng thot ra v ha
tan phn cn li vi nc va thu c 250 ml.
Chnh quang k ngn la v bc sng o 589 nm. Hiu
chnh nn v khng bng cch o s truyn quang qua
nc v t truyn quang 100% khi o dung dch chun
cha 200 g natri (dng clorid) / ml. o t l truyn quang
ca 3 dung dch 50; 100; 150 g natri (dng clorid) / ml. V
th biu th tng quan gia % truyn quang v nng
natri. t dung dch mu vo my o v c % truyn
quang. Da vo ng chun xc nh nng natri (C)
trong dung dch mu th v tnh hm lng Na2O trong
mu theo cng thc sau:
250 x C x

1,348
1000

-F

Trong :
F l lng natri oxyd tng ng vi natri sulfat c mt
trong mu, v c xc nh nh sau:
Hiu chnh i vi hm lng sulfat:
Cn khong 12,5 g (chnh xc n mg) mu th c
lm kh trc ti 105o trong 2 gi v khuy bng my
khuy cao tc vi 240 ml nc trong t nht 5 pht. Chuyn
hn hp vo ng ong 250 ml, y ng ong, ln ngc
ng vi ln trn u mu, xc nh dn ca dung
dch c, s dng cu o dn thch hp. dng
ng chun, o dn ca cc dung dch chun cha
50; 100; 200 v 500 mg natri sulfat / 100 ml. Da vo
ng chun xc nh nng natri sulfat trong dung dch
mu (C) (mg/100 ml) v tnh h s hiu chnh (F) theo cng
thc sau:
w
F = 0,437 x 2,5 x C x
W
Trong :
w l khi lng mu th ly xc nh natri oxyd.
W l khi lng mu th ly chun b hn hp vi nc
trn.

Ph lc 8
QUY NH K THUT V PHNG PHP TH I VI NHM SILICAT
1. Tn khc, ch s

2. nh ngha

Aluminium silicate; Cao lanh (nh hoc nng)

INS 559
PTWI = 1 mg/kg th trng
L nhm silicat hydrat ha c trong t nhin, loi phn
ln cc tp cht bng cch gn ra v sy kh. Ch phm
thng mi cn c phn loi da trn cc tiu ch v
clorid, tp cht, c ht, gim khi lng khi lm kh, gim
khi lng khi nung v gi tr pH.

3. M t

Bt mm, hi trng, khng c sn, khng mi.

4. Chc nng

Cht chng ng vn.

5. Yu cu k thut
5.1. nh tnh
tan

Khng tan trong nc, ethanol v cc acid khong.

Tnh do

Ly 8 g mu th thm 5 ml nc v trn u. Hn hp phi

c tnh do.

Silicat

Phi c phn ng c trng ca silicat

Nhm

Phi c phn ng c trng ca nhm

5.2. tinh khit

Cc cht tan trong nc

Khng c qu 0,3 %.

Cc cht tan trong acid

Khng c qu 2,0 %.

Aming

Khng c c.

Ch

Khng c qu 5,0 mg/kg.

6. Phng php th
6.1. nh tnh
Silicat

Cn khong 500 mg mu th, trn vi khong 200 mg natri

carbonat khan v 2 g kali carbonat khan, un nng hn hp
trn chn nung bng platin hoc niken n khi hn hp
chy hon ton. ngui v thm 5 ml nc, yn trong
3 pht. un nh y chn nung tch phn b nung chy
ra khi chn. Dng 50 ml nc trng v chuyn phn
ny vo cc. Thm acid hydrocloric vo n khi khng cn
si bt, sau thm d 10 ml acid hydrocloric, cho bay hi
hn hp n kh trn b cch thy nc si. Lm mt v
thm 20 ml nc, un si v lc hn hp qua giy lc
khng tro. Cn silica khng tan s b gi li trn giy lc
(ch gi li phn dch lc th nhm). Chuyn phn cn

keo vo mt a platin v thm cn thn 5 ml acid

hydrofloric (Cnh bo: acid hydrofloric rt c, c tnh n
mn, khng c tip xc vi da. Tin hnh thao tc
trong t hood). Ta rn s b ha tan (nu khng tan lp li
qu trnh cho bay hi vi acid hydrofloric. un nng v gi
mt a thy tinh (u a c 1 git nc) trong lung hi
thot ra. Git nc u a s tr nn c.
Nhm

Thm dung dch amoniac (TS) vo dch lc thu c trong

phn th silicat. Trong dung dch xut hin ta keo mu
trng, ta ny khng tan khi thm d dung dch amoniac
(TS) nhng tan trong dung dch natri hydroxyd (TS).

6.2. tinh khit

Cc cht tan trong nc

Cc cht tan trong acid

Aming

Ch

Cn 5 g (chnh xc n mg) mu th, un si vi 50 ml

nc trong 30 pht, thnh thong b sung nc duy tr
th tch ban u. Lc v cho bay hi dch lc n kh, sy
ti 105o trong 1 gi v cn.
Hm lng cc cht tan trong nc (%) = m/[10 W]
Trong :
m = Khi lng cn (mg)
W = khi lng mu th (g).
Cn 2 g (chnh xc n mg) mu th, un hi lu si vi
100 ml dung dch acid hydrocloric long(TS) trong 15 pht.
ngui, lc v cho bay hi 50 ml dch lc n kh, sau
nung nh n khi lng khng i v cn.
Hm lng cc cht tan trong acid (%) = m/[5 X W]
Trong :
m = Khi lng cn (mg)
W = khi lng mu th (g).
Phng php soi knh hin vi in t (d kin): Mu th
c nghin ng nht n mc c th. S dng knh hin
vi in t vi ti thiu 100 hin vi thng, kim tra tiu bn
t mu, nu pht hin ra bt c vt liu dng si th mu
th khng t.
- Th theo hng dn ti JECFA monograph 1 - Vol.4 .
- Xc nh bng k thut 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.