CNG HA X HI CH NGHA VIT NAM

QCVN 4-9 : 2010/BYT

QUY CHUN K THUT QUC GIA

V PH GIA THC PHM - CHT LM RN CHC
National technical regulation on Food additives Firming agents

H NI - 2010

Li ni u
QCVN 4-9 :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 26/2010/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 LM RN CHC
National technical regulation on Food additives - Firming 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 lm rn chc 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 rn chc 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:
- Cht lm rn chc: l ph gia thc phm c s dng vi mc ch gi cho
cc m rau, qu chc v ti hoc kt hp vi cc cht keo ha to ra cht
gel.
- 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.
- M s C.A.S (Chemical Abstracts Service): M s ng k ha cht ca Hip
hi Ha cht Hoa K.
- TS (test solution): Dung dch thuc th.
- ADI (Acceptable daily intake): Lng n vo hng ngy chp nhn c.
- PTWI (Provisional Tolerable Weekly Intake): Lng n vo hng tun tm
thi chu ng c
- 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 lm rn chc 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 calci
citrat.
1.2. Ph lc 2: Yu cu k thut v phng php th i vi calci clorid.
1.3. Ph lc 3: Yu cu k thut v phng php th i vi nhm sulfat
(khan).
1.4. Ph lc 4: Yu cu k thut v phng php th i vi calci sulfat v nh
hnh.
1.5. Ph lc 5: Yu cu k thut v phng php th i vi nhm amoni
sulfat.

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 rn chc 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 rn chc
Vic kim tra cht lng, v sinh an ton i vi cc cht lm rn chc 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.
2. T chc, c nhn ch c nhp khu, xut khu, sn xut, bun bn v s dng
cc cht lm rn chc 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
YU CU K THUT V PHNG PHP TH I VI CALCI CITRAT
1. Tn khc, ch s

INS 333
ADI khng gii hn

2. nh ngha
Tn ha hc

Tricalci citrat; Mui Tricalci ca acid 2-hydroxy-1,2,3propantricarboxylic; Mui tricalci ca acid -hydroxy
tricarballynic.

M s C.A.S.

813-94-5

Cng thc phn t

C12H10Ca3O14.4H2O

Cng thc cu to
CH2COO

HO C COO

CH2COO

Ca3 . 9 H2O

2
Khi lng phn t

570,51

3. Cm quan

Bt mn mu trng, khng mi.

4. Chc nng

Cht lm rn chc, m, cht to phc kim loi.

5. Yu cu k thut
5.1. nh tnh
tan

Rt t tan trong nc, khng tan trong ethanol.

Citrat

Phi c phn ng c trng ca citrat

Calci

Phi c phn ng c trng ca Calci

5.2. tinh khit

Gim khi lng khi lm
kh

Khng thp hn 10,0% v c qu 14,0% (sy ti 150oC

trong 4 gi).

Florid

Khng c qu 30,0 mg/kg.

Kim t do v acid t do

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

Oxalat

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

Ch

Khng c qu 2,0 mg/kg.

5.3. Hm lng
C12H10Ca3O14

Khng thp hn 97,5% tnh theo ch phm lm kh.

6. Phng php th
6.1. nh tnh
Calci

- Th theo JECFA monograph 1 - Vol.4

- dung dch th c chun b nh sau: nung 0,5 g mu
th ti nhit thp nht c th, lm mt v ha tan cn
trong 10 ml nc, thm 1 ml acid acetic bng).

6.2. tinh khit

Florid

- Th theo JECFA monograph 1 - Vol.4

- Phng php I hoc III.

Kim t do v acid t do

Cn 1 g mu th, thm 5 ml nc, lc u trong 1 pht v

thm 2 git dung dch phenolphtalein (TS). Dung dch
khng c c mu hng. Thm 0,5 ml dung dch natri
hydroxyd 0,1 N, dung dch c mu hng.

Oxalat

Cn 1 g mu th, ha tan trong 5 ml dung dch m ca acid

hydrocloric long (TS), lc hn hp nu cn. Thm 2 g natri
acetat v pha long bng nc n 10 ml. Sau 1 gi,
dung dch khng c c.

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 350 mg (chnh xc n mg) mu th c

lm kh trc ti 100 oC trong 4 gi, ha tan trong 10 ml
nc, 2 ml acid hydrocloric long (TS) v pha long bng
nc n 100 ml. Khuy bng my khuy t, trong khi
khuy, s dng buret thm khong 30 ml dung dch dinatri
ethylendiamintetraacetat 0,05 M sau thm 15 ml dung
dch natri hydroxyd (TS) v 300 mg ch th xanh da tri
hydroxynaphtol. Tip tc chun n im kt thc dung
dch c mu xanh da tri .
Mi ml dung dch dinatri ethylendiamintetraacetat 0,05 M
tng ng vi 8,303 mg C12H10Ca3O14.

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

INS 509
ADI khng gii hn

2. nh ngha
Tn ha hc

Calci clorid.

M s C.A.S.

10043-52-4

Cng thc ha hc

Dng khan: CaCl2

Dng dihydrat: CaCl2.2H2O
Dng hexahydrat: CaCl2.6H2O

Khi lng phn t

Dng khan: 110,99

Dng dihydrat: 147,02
Dng hexahydrat: 219,08

3. M t

Dng khan: dng cc d chy ra hoc dng khi xp,

mu trng.
Dng dihydrat: Dng mnh hoc ht mu trng, cng, d
chy ra.
Dng hexahydrat: Tinh th khng mu rt d chy ra.

4. Chc nng

Cht lm rn chc

5. Yu cu k thut
5.1. nh tnh
tan

Dng khan: D tan trong nc v trong ethanol

Dng dihydrat: D tan trong nc, tan trong ethanol.
Dng hexahydrat: Tan tt trong nc v trong ethanol.

Clorid

Phi c phn ng c trng ca clorid.

Calci

Phi c phn ng c trng ca calci.

5.2. tinh khit

Kim t do

Khng c qu 0,15% tnh theo Ca(OH)2.

Mui ca Magnesi v kim

loi kim

Khng c qu 5,0%.

Florid

Khng c qu 40,0 mg/kg.

Ch

Khng c qu 2,0 mg/kg.

5.3. Hm lng CaCl2

Dng khan: Khng c thp hn 93,0%

Dng dihydrat: Khng c thp hn 99,0% v khng
c qu 107,0% quy ra CaCl2.2H2O
Dng hexahydrat: Khng c thp hn 98,0% v khng
c qu 110,0% quy ra CaCl2.6H2O

6. Phng php th
6.1. tinh khit
Kim t do

Cn 1 g mu th, ha tan trong 20 ml nc va un si,

ngui, thm 2 git dung dch phenolphtalein (TS). Nu dung
dch c mu hng th mu hng ny b mt i khi thm 2 ml
dung dch acid hydrocloric 0,02 N.

Mui ca Magnesi v kim

loi kim

Cn 1 g calci clorid khan (hoc khi lng dng hydrat ha

tng ng), ha tan trong 50 ml nc, thm 500 mg
amoni clorid, lc u v un si trong 1 pht. Thm nhanh
40 ml dung dch acid oxalic (TS), khuy u n khi kt ta
hon ton. Thm ngay 2 git dung dch methyl (TS), thm
tng git dung dch amoniac (TS) n khi dung dch bt u
kim, ngui dung dch. Chuyn hn hp vo ng ong
100 ml, pha long bng nc ti 100 ml. yn trong 4 gi
hoc qua m, sau gn ly dch trong pha trn qua giy
lc kh. Ly 50 ml dch lc vo mt a platin, thm 0,5 ml
acid sulfuric v cho bay hi hn hp n gn cn trn b
cch thy nc si. Cn thn cho bay hi n kh trn ngn
la v tip tc un n khi cc mui amoni b phn hy hon
ton v bay hi. Cui cng nung cn ti khi lng khng
i. Khi lng cn khng c qu 25 mg.

Florid

- Th theo JECFA monograph 1 - Vol.4, phng php III.

Ch

- Th theo 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.

6.2. nh lng

Cn khong 1 g (chnh xc n mg) mu th hoc khi

lng dng hydrat ha quy ra tng ng, cho vo cc
thy tinh 250 ml, ha tan trong hn hp gm 5 ml dung dch
acid hydrocloric long (TS) v 100 ml nc. Chuyn vo
bnh nh mc 250 ml, pha long bng nc n vch. Ly
50 ml dung dch ny vo mt bnh nn, thm 100 ml nc,
15 ml dung dch natri hydroxyd (TS), 40 mg ch th murexid
(amoni purpurat) v 3 git dung dch xanh naphtol (TS) v
chun vi dung dch dinatri ethylendiamintetraacetat
0,05M n khi dung dch c mu xanh da tri m.
Mi ml dung dch dinatri ethylendiamintetraacetat 0,05M
tng ng vi 5,55 mg CaCl2; tng ng vi 7,35 mg
CaCl2.2H2O; tng ng vi 10,95 mg CaCl2.6H2O.

Ph lc 3
YU CU K THUT V PHNG PHP TH I VI NHM SULFAT (KHAN)
1. Tn khc, ch s

Aluminium sulfate
INS 520
PTWI = 1 mg/kg th trng

2. nh ngha
Tn ha hc

Nhm sulfat.

M s C.A.S.

10043-01-3

Cng thc ha hc

Al2(SO4)3

Khi lng phn t

342,13

3. Cm quan

Bt mu trng, dng hnh a bng sng, hoc mnh tinh

th; khng mi.

4. Chc nng

Cht lm rn chc.

5. Yu cu k thut
5.1. nh tnh
tan

D tan trong nc, khng tan trong ethanol.

pH

Dung dch mu th 5% c pH

Nhm

Phi c phn ng c trng ca nhm.

Sulfat

Phi c phn ng c trng ca sulfat.

2,9.

5.2. tinh khit

o
Gim khi lng khi nung Khng c qu 5,0% (Nung ti 500 C trong 3 gi).

Cc kim v kim th

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

Florid

Khng c qu 30,0 mg/kg.

Selen

Khng c qu 30,0 mg/kg.

Ch

Khng c qu 5,0 mg/kg.

5.3. Hm lng Al2(SO4)3 Khng thp hn 99,5% tnh theo ch phm sau khi nung.
6. Phng php th
6.1. tinh khit
Cc kim v kim th

Thm vi git dung dch methyl (TS) vo dung dch ang

si gm 2 g mu th tan trong 150 ml nc. Sau thm
dung dch amoniac (TS) n khi mu ca dung dch bt u
chuyn sang mu vng r rt. Thm nc nng hiu
chnh th tch v ng th tch ban u, lc khi dung dch

cn nng. Ly 75 ml dung dch ny, cho bay hi n kh v

nung n khi lng khng i. Lng cn cn li khng
c qu 4 mg (khong 0,4%).
Florid

Huyn ph vi
Cho cn thn, t t khong 56 g calci oxyd (c hm lng
clorid thp - khong 2 mg/kg) vo 250 ml nc, thm t t
250 ml acid percloric 60% vo, khuy u. Thm vi vin bi
thy tinh, un nng n khi khi acid percloric bay ra nhiu,
lm mt, thm 200 ml nc v tip tc un. Lp li qu
trnh pha long ny thm 1 ln, ngui v lc nu c kt
ta silic dioxid. Rt dch lc trong, va rt va khuy vo
1000 ml dung dch natri hydroxyd 1/10, kt ta lng
xung, gn b lp dch trong. Loi mui natri ra khi ta
bng cch ra 5 ln trong bnh ly tm ln, mi ln ra lc
mnh. Cui cng lc kt ta thnh huyn ph v pha long
n 2000 ml. Bo qun huyn ph trong chai c nt gn
parafin, trc khi dng cn lc u. 100 ml huyn ph ny
c xem nh mu trng (cha flor mc khng ng k)
v x l theo hng dn trong phn "Tin hnh th" bt
u t giai on "Nung trong thi gian ngn ti 600o...".
Thit b chng ct
Ni bnh cu ct 125 ml vi 1 sinh hn, ng thi ni vi
ng mao qun v nhit k sao cho u ng mao qun v
nhit k ngp vo dung dch trong bnh. Ni ng mao qun
vi mt phu nh git hoc b phn sinh hi nc.
gim thiu nn trng do florid thi t thy tinh, thit b ct
c x l trc nh sau: X l tt c cc dng c thy
tinh cn s dng vi dung dch natri hydroxyd 10% nng,
tip theo xi qua vi nc v trng bng nc ct. Ti
thiu 1 ln/ngy, x l thm bng cch un si 15-20 ml
dung dch acid sulfuric 1/2 trong h thng ct n khi h
thng y khi acid, ngui, b acid, ti x l vi dung
dch natri hydroxyd 10%, trng ra ton b h thng ct.
Tin hnh th
Cn 1,67 g (chnh xc n mg) mu, cho vo bnh cu ct,
thm 25 ml dung dch acid sulfuric 1/2. Ct n khi t nhit
160o, sau duy tr nhit ti 160o n 165o bng
cch thm nc t phu nh git vo bnh, thu ly 300 ml
dch ct. Oxy ha dch ct bng cch thm 2-3 ml dung dch
hydrogen peroxyd 30% khng c florid ( c loi b
sulfit), yn hn hp vi pht, cho bay hi trn a platin
c sn lng d huyn ph vi.
Nung trong thi gian ngn ti 600 o v sau lm mt v
tm t tro vi khong 10 ml nc. y a platin bng
mt knh ng h, cn thn thm vo lng acid
percloric 60% ha tan tro.

Cho dch trn a platin qua phu nh git v bnh ct c

cha sn vi vin bi thy tinh (tt c thit b ct va mi x
l), lng acid percloric 60% ho tan tro v trng
chuyn dung dch t a platin vo phu khng qu 20 ml.
Thm 10 ml nc v vi git dung dch bc perclorat 1/2
qua phu nh git vo bnh. Tip tc tin hnh theo hng
dn trong chuyn lun th gii hn florid, phng php I Phng php ln mu vi Thori nitrat, bt u t giai on
"Chng ct n khi nhit t 135o...".
Selen

- Th theo JECFA monograph 1 - Vol.4 - Phng php II.

- Cn 0,2 g mu.

Ch

- Th theo 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.

6.2. nh lng

Cn khong 4 g (chnh xc n mg) mu th, chuyn vo

bnh nh mc 250 ml. Ha tan v pha long bng nc
n vch, lc u. Dng pipet ly 10 ml dung dch ny cho
vo cc 250 ml, thm 25 ml dung dch dinatri
ethylendiamintetraacetat 0,05 M, un si nh trong 5 pht.
Lm mt, v khuy u, trong khi khuy thm (theo ng
th t) 20 ml dung dch m pH 4,5 (77,1 g amoni acetat
v 57 ml acid acetic bng trong 1000 ml), 50 ml ethanol, 2
ml dung dch dithizon (TS). Chun vi dung dch km
sulfat 0,05 M n khi dung dch chuyn t mu tm xanh
sang mu hng. Tin hnh lm mu trng song song, dng
10 ml nc thay cho mu.
Mi ml dung dch dinatri ethylendiamintetraacetat 0,05 M
tng ng vi 8,553 mg Al2(SO4)3.

Ph lc 4
YU CU K THUT V PHNG PHP TH I VI CALCI SULFAT
1. Tn khc, ch s

Calcium sulfate
INS 516
ADI khng gii hn

2. nh ngha
Tn ha hc

Calci sulfat.

Ch s C.A.S.

7778-18-9

Cng thc ha hc

Dng khan: CaSO4

Dng dihydrat: CaSO4.2H2O

Khi lng phn t

Dng khan: 136,14

Dng dihydrat: 172,18

3. Cm quan

Bt mn mu trng n trng vng, khng mi

4. Chc nng

Cht lm rn chc, cht to phc kim loi, thc n cho

nm men, cht iu ha cho bt nho.

5. Yu cu k thut
5.1. nh tnh
tan

t tan trong nc, khng tan trong ethanol.

Calci

Phi c phn ng c trng ca calci.

Sulfat

Phi c phn ng c trng ca sulfat.

5.2. tinh khit

Gim khi lng khi lm
kh

Dng khan: Khng c qu 1,5%

Dng dihydrat: Khng c qu 23% v khng nh hn
19%

Florid

Khng c qu 30,0 mg/kg.

Selen

Khng c qu 30,0 mg/kg.

Ch

Khng c qu 2,0 mg/kg.

5.3. Hm lng CaSO4

Khng thp hn 99,0% tnh theo ch phm lm kh.

6. Phng php th
6.1. tinh khit
Gim khi lng khi lm
kh

- Th theo JECFA monograph 1 - Vol.4. Sy ti 250o n

khi lng khng i.

Florid

- Th theo JECFA monograph 1 - Vol.4, Phng php I

hoc III.

Selen

- Th theo JECFA monograph 1 - Vol.4, Phng php II.

- Cn 0,2 g mu.

Ch

- Th theo 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.

6.2. nh lng

Cn khong 250 mg (chnh xc n mg) mu th lm

kh ha tan trong 150 ml nc v 4 ml dung dch acid
hydrocloric long, un si nu cn ha tan hon ton,
ngui. Thm 15 ml dung dch natri hydroxyd (TS) v 40
mg ch th murexid v 3 ml dung dch xanh lc naphtol (TS)
v chun vi dung dch dinatri ethylendiamintetraacetat
0,05 M n khi dung dch c mu xanh da tri m.
Mi ml dung dch dinatri ethylendiamintetraacetat 0,05 M
tng ng vi 6,807 mg CaSO4.

Ph lc 5
YU CU K THUT V PHNG PHP TH I VI NHM AMONI SULFAT
1. Tn khc, ch s

Ammonium alum;
INS 523
PTWI = 1 mg/kg th trng

2. nh ngha
Tn ha hc

Nhm amoni sulfat.

M s C.A.S.

7784-25-0

Cng thc ha hc

AlNH4(SO4)2.12H2O

Khi lng phn t

453,32

3. Cm quan

Tinh th ln, khng mu, hoc dng ht mu trng, hoc

dng bt; khng mi.

4. Chc nng

m, tc nhn trung ha, cht n nh mu.

5. Yu cu k thut
5.1. nh tnh
tan

D tan trong nc, khng tan trong ethanol.

Nhm

Phi c phn ng c trng ca nhm.

Amoni

Phi c phn ng c trng ca amoni.

Sulfat

Phi c phn ng c trng ca sulfat.

5.2. tinh khit

Cc kim v kim th

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

Florid

Khng c qu 30,0 mg/kg.

Selen

Khng c qu 30,0 mg/kg.

Ch

Khng c qu 3,0 mg/kg.

5.3. Hm lng
AlNH4(SO4)2.12H2O

Khng thp hn 99,5% AlNH4(SO4)2.12H2O

6. Phng php th
6.1. Th tinh khit
Cc kim v kim th

Kt ta hon ton nhm trong dung dch gm 1 g mu

trong 100 ml nc bng cch thm va dung dch
amoniac (TS) kim ha nh dung dch, th bng dung
dch methyl (TS) v lc. Cho bay hi dch lc n kh v
nung n khi lng khng i. Lng cn cn li khng
c qu 5 mg.

Florid

Huyn ph vi
Cho cn thn, t t khong 56 g calci oxyd (c hm lng
clorid thp - khong 2 mg/kg) vo 250 ml nc, thm t t
250 ml acid percloric 60% vo, khuy u. Thm vi vin bi
thy tinh, un nng n khi khi acid percloric bay ra nhiu,
lm mt, thm 200 ml nc v tip tc un. Lp li qu
trnh pha long ny thm 1 ln, ngui v lc nu c kt
ta silic dioxyd. Rt dch lc trong, va rt va khuy vo
1000 ml dung dch natri hydroxyd 1/10, kt ta lng
xung, gn b lp dch trong. Loi mui natri ra khi ta
bng cch ra 5 ln trong bnh ly tm ln, mi ln ra lc
mnh. Cui cng lc kt ta thnh huyn ph v pha long
n 2000 ml. Bo qun huyn ph trong chai c nt gn
parafin, trc khi dng cn lc u.(100 ml huyn ph ny
c xem nh mu trng cha flor mc khng ng k
khi c, ct v chun theo JECFA monograph 1 - vol. 4,
chuyn lun th gii hn Florid, phng php 1 - Phng
php so mu dng thuc th Thori nitrat) .
Tin hnh th
Cn 1,67 g (chnh xc n mg) mu, cho vo bnh cu ct,
thm 25 ml dung dch acid sulfuric 1/2. Ct n khi t nhit
160o, sau duy tr nhit ti 160o n 165o bng
cch thm nc t phu nh git vo bnh, thu ly 300 ml
dch ct. Oxy ha dch ct bng cch thm 2-3 ml dung dch
hydrogen peroxyd 30% khng c florid ( c loi b
sulfit), yn hn hp vi pht, cho bay hi trn a platin
c sn lng d huyn ph vi.
Nung trong thi gian ngn ti 600o v lm mt v tm
t tro vi khong 10 ml nc. y a platin bng mt
knh ng h, cn thn thm vo lng acid percloric
60% ha tan tro. Cho dch trn a platin qua phu
nh git v bnh ct c cha sn vi vin bi thy tinh (tt c
thit b ct va mi x l), lng acid percloric 60% ho
tan tro v trng chuyn dch t a platin vo phu khng
qu 20 ml. Thm 10 ml nc v vi git dung dch bc
perclorat 1/2 qua phu nh git vo bnh. Tip tc tin hnh
theo hng dn trong chuyn lun th gii hn florid,
phng php I - Phng php ln mu vi Thori nitrat, bt
u t giai on "Chng ct n khi nhit t 135o...".

Selen

- Th theo JECFA monograph 1 - Vol.4, Phng php II.

- Cn 0,2 g mu.

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.

6.2. nh lng

Cn khong 1 g (chnh xc n mg) mu th. Ha tan

trong 50 ml nc, thm 50 ml dung dch EDTA 0,05 M v
20 ml dung dch m pH 4,5 (77,1 g amoni acetat v 57 ml
acid acetic bng trong 1000 ml), un si nh trong 5 pht.
Lm mt, thm 50 ml ethanol, 2 ml dung dch dithizon
(TS). Chun vi dung dch km sulfat 0,05 M n khi
dung dch c mu hng nht. Tin hnh lm mu trng
song song.
Mi ml dung dch EDTA 0,05 M tng ng vi 22,67 mg
AlNH4(SO4)2.12H2O.

Ph lc 8
YU CU 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 c 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 lm rn chc.

5. Tnh cht
5.1. nh tnh
tan

Khng tan trong nc v ethanol v cc acid v c.

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 trong 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, b sung nc dn dn gi th tch
khng i. 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 X 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 (TS) trong 15 pht.
ngui v lc v cho bay hi 50 ml dch lc n kh, sau
nung 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 (tm thi): Mu th
c nghin ng nht n mc c th. S dng knh hin
vi in t ti thiu 100 hin vi trng, kim tra tng tiu
bn 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.