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CNG HO X HI CH NGHA VIT NAM

QCVN 4 13 : 2010/BYT

QUY CHUN K THUT QUC GIA


V PH GIA THC PHM - CHT N NH

National technical regulation on Food Additive - Stabilizers

H NI - 2010

QCVN 4 - 13 : 2010/BYT

Li ni u
QCVN 4-13:2010/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 - 13 : 2010/BYT

QUY CHUN K THUT QUC GIA


V PH GIA THC PHM - CHT N NH
National technical regulation on Food Additive Stabilizers

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 n nh 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 n nh 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 n nh: l ph gia thc phm c s dng vi mc ch duy tr s
phn tn ca hai hay nhiu thnh phn nhm to nn s ng nht cho sn 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 MTDI (Maximum tolerable daily intake): Lng n vo hng ngy ti a 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 n nh c quy
nh ti cc ph lc ban hnh km theo Quy chun ny nh sau:
3

QCVN 4 - 13 : 2010/BYT
1.1.

Ph lc 1:

Yu cu k thut v phng php th i vi


Polyvinylpyrolidon

1.2.

Ph lc 2:

Yu cu k thut v phng php th i vi calci lactat

1.3.

Ph lc 3:

Yu cu k thut v phng php th i vi kali


dihydrocitrat

1.4.

Ph lc 4:

Yu cu k thut v phng php th i vi dinatri


hydrogen phosphat

1.5.

Ph lc 5:

Yu cu k thut v phng php th i vi dikali


hydrogen phosphat

1.6.

Ph lc 6:

Yu cu k thut v phng php th i vi tricalci


phosphat

1.7.

Ph lc 7:

Yu cu k thut v phng php th i vi amoni


polyphosphat

1.8.

Ph lc 8:

Yu cu k thut v phng php th i vi natri


hydrogen carbonat

1.9

Ph lc 9 :

Yu cu k thut v phng php th i vi kali


carbonat

1.10

Ph
10 :

lc

Yu cu k thut v phng php th i vi amoni


hydrogen carbonat

1.11

Ph
11 :

lc

Yu cu k thut v phng php th i vi kali clorid

1.12

Ph
12 :

lc

Yu cu k thut v phng php th i vi kali


dihydrogen phosphat

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.

QCVN 4 - 13 : 2010/BYT
III. YU CU QUN L
1. Cng b hp quy
1.1. Cc cht n nh 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 n nh
Vic kim tra cht lng, v sinh an ton i vi cc cht n nh 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 n nh 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 - 13 : 2010/BYT
Ph lc 1
YU CU K THUT V PHNG PHP TH
I VI POLYVINYLPYROLIDON
1. Tn khc, ch s

Povidone, PVP, Polyvinylpyrrolidone


INS 1201
ADI = 0-50 mg/kg

2. nh ngha
Tn ha hc

Polyvinylpyrolidon, poly-[1-(2-oxo-1-pyrolidinyl)- ethylen]

M s C.A.S.

9003-39-8

Cng thc phn t

(C6H9NO)n

Cng thc cu to

Khi lng phn t

Ch phm c di khi lng phn t thp: khong 40000.


Ch phm c di khi lng phn t cao: khong 360000.

3. Cm quan

Bt trng ti nu nht, ch phm thng mi gm 2 dng


khi lng phn t, gi tr khi lng phn t chung l
trung bnh cng gia tr khi lng phn t ca 2 dng.

4. Chc nng

Tc nhn lm trong, cht n nh, cht lm dy, t dc


vin nn, tc nhn phn tn.

5. Yu cu k thut
5.1. nh tnh
tan

Tan trong nc, ethanol v cloroform; khng tan trong


ether

pH

3,0 7,0 (dung dch 5%)

To kt ta

Phi c phn ng to kt ta c trng.

5.2. tinh khit


Nc

Khng c qu 5%.

nht tng i

T 1,188 ti 1,325 i vi ch phm c khi lng phn t


thp, v t 3,225 ti 5,662 i vi ch phm c khi lng
phn t cao (m t trong phn Phng php th).

QCVN 4 - 13 : 2010/BYT
Tro ton phn

Khng c qu 0,02%.

Aldehyd

Khng c qu 0,2% (tnh theo acetaldehyd)

Hm lng monomer

Khng c qu 1,0% (tnh theo vinylpyrolidon) (m t


trong phn Phng php th).

Hydrazin

Khng c qu 1,0 mg/kg (m t trong phn Phng


php th).

Ch
5.3. Hm lng Nitrogen

Khng c qu 2,0 mg/kg.


Khng c nh hn 12,2% v khng qu 13,0% Nitrogen
(N) tnh theo ch phm khan.

6. Phng php th
6.1 nh tnh
To kt ta

Thm 5 acid hydrocloric long (TT), 5 ml nc v 2 ml


dung dch kali dicromat 1/10 vo 5 ml dung dch ch phm
th 1/50. Xut hin ta vng.
Thm 5 ml dung dch ch phm th 1/50 vo 75 mg cobalt
nitrat v 0,3 g amoni thiocyanat ha tan trong 2 ml
nc, lc u v acid ha bng acid hydrocloric long (TT).
Xut hin ta mu xanh nht.
Thm 1 acid hydrocloric 25% (TT), 5 ml bari clorid 5% v 1
ml dung dch acid phosphomolybdotungstic 5% vo 5 ml
dung dch ch phm th 1/50. Khi ta trng ln to thnh,
ta ny dn dn chuyn sang mu xanh khi di nh
sng ban ngy (Ch : s xut hin mu xanh di nh
sng ban ngy dng phn bit polyvinylpyrolidon vi
polyethylen oxyd, cht ny cho ta tng t vi thuc th
trn nhng vn gi nguyn mu trng di nh sng ban
ngy).

6.2. tinh khit


Nc

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


- Phng php Karl Fischer.

nht tng i

Cho mt lng cn chnh xc mu th, tng ng vi 1 g


polyvinylpyrolidon khan, vo mt bnh nn 250 ml, v tnh
lng nc thm vo thu c dung dch 1%. hn
hp nhit phng, thnh thong lc, ti khi tan hon
ton, sau yn trong 1 gi na. Lc qua phu lc xp
kh c l lc th, sau cho 10 ml dch lc vo nht k
Cannon-Fenske, hoc loi tng ng, v t nht k
vo trong ni cch thy duy tr nhit 250,05oC. Sau
7

QCVN 4 - 13 : 2010/BYT
khi dung dch mu th v pipet trong ni cch thy
lm m trong 10 pht, ly dung dch bng cch ht ln rt
nh qua ng mao qun ti khi to thnh mt khum ca cht
lng t 3 ti 4 mm trn vch. Gim t t chn khng, v
khi mt khum ca cht lng t ti vch mc trn, bt u
tnh thi gian chy qua mao qun. Ghi chnh xc thi gian
khi mt khum ca cht lng t n vch mc di, v tnh
thi gian chy chnh xc ti 0,1 giy. Lp li php th ny
t nht 3 ln. Gi tr thu c phi khng lch qu 0,3 giy;
nu khng, xc nh li vi 10 ml dung dch mu th khc
sau khi ra ng o nht bng dung dch ra acid
sulfuric-dicromat. Tnh thi gian chy trung bnh ca dung
dch mu th, v sau , o thi gian chy trung bnh theo
cch tng t ca 10 ml nc lc trn cng ng o
nht. Tnh nht tng i bng cch chia thi gian chy
trung bnh ca dung dch mu th cho thi gian chy trung
bnh ca nc.
Tro ton phn

Aldehyd

Cn 10 g mu th.

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

Cho khong 10 g mu th, cn chnh xc v ha tan trong


300 ml nc, vo bnh y trn 1000 ml c cha 80 ml acid
sulfuric 25%, un hi lu trong khong 45 pht di mt
ng sinh hn lm lnh bng nc, v sau ct khong
100 ml vo bnh hng c 20 ml hydroxylamin hydroclorid 1
N trc c iu chnh ti pH 3,1. Chun hn
hp trong bnh cha bng natri hydroxyd 0,1 N ti pH 3,1,
dng my o pH. Tin hnh lm mt mu trng v hiu
chnh nu cn.
1 ml natri hydroxyd 0,1 N tng ng vi 4,405 mg
C2H4O.

Hm lng monomer

Ha tan khong 4 g mu th, cn chnh xc, vo 30 ml


nc trong bnh y trn 125 ml, thm 0,5 g natri acetat,
trn u v bt u chun bng iod 0,1 N. Khi mu ca
iod khng cn nht i na, thm 3,0 ml dung dch chun
, yn dung dch trong khong 5 ti 10 pht. Thm h
tinh bt (TT), v chun iod d bng natri thiosulfat 0,1 N.
Song song tin hnh lm mt mu trng, s dng cng th
tch iod 0,1 N, ly chnh xc, nh mu th.
1 ml iod 0,1 N tng ng vi 5,56 mg vinylpyrolidon.

Hydrazin

Cho 2,5 g ch phm th vo mt ng ly tm 50 ml, thm 25


ml dung dch salicylaldehyd 1/20 trong methanol, lc xoy,
v un nng trong cch thy 60oC trong 15 pht.
8

QCVN 4 - 13 : 2010/BYT
ngui, thm 2,0 ml toluen, y np ng ly tm, lc mnh
trong 2 pht, v ly tm. Trn bn mng sc k thch hp,
c ph lp hn hp silica gel dimethylsilan ha dy 0,25
mm, chm 10 L lp toluen trong pha trn trong ng ly tm
v 10 L dung dch chun salicylaldazin trong toluen cha
9,38 g/ml. vt chm kh, v khai trin trong h dung
mi methanol v nc (2:1) ti khi tuyn dung mi i c
ba phn t chiu di ca bn mng. Ly bn mng ra khi
bnh trin khai, nh du tuyn dung mi, v cho dung
mi bay hi. Pht hin vt trn bn mng di nh sng t
ngoi ti bc sng 365 nm: vt salicylaldazin pht quang
c gi tr Rf khong 0,3, v hunh quang ca bt k vt
salicylaldazin ca mu th khng c m hn vt thu
c ca dung dch chun salicylaldazin (hydrazin 1 ppm).
Dung dch chun Salicylaldazin: Ha tan 300 mg hydrazin
sulfat trong 5 ml dung dch salicylaldehyd 20% (tt/tt) trong
alcol isopropyl mi pha, lc u, v yn ti khi xut hin
ta mu vng. Chit hn hp hai ln, mi ln vi 15 ml
methylen clorid. Gp dch chit methylen clorid, v lm kh
trn natri sulfat khan. Gn dung dch methylen clorid, v c
ti kh. Kt tinh li cn salicylaldazin t hn hp toluen v
methanol m (60:40) bng cch lm lnh; lc v lm kh
tinh th trong chn khng. Tinh th c khong chy t
213oC ti 214oC.
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 ti JECFA monograph 1 - Vol.4 phn
cc phng php phn tch cng c.

6.3. nh lng

Tin hnh theo ch dn trong phn Xc nh Nitrogen


Vol.4, s dng khong 1 g ch phm th, cn chnh xc.

QCVN 4 - 13 : 2010/BYT
Ph lc 2
YU CU K THUT V PHNG PHP TH I VI CALCI LACTAT
1. Tn khc, ch s

INS 327
ADI khng gii hn

2. nh ngha
Tn ha hc

Calci dilactat, calci dilactat dihydrat, mui calci ca acid 2hydroxypropanoic

M s C.A.S.

814-80-2

Cng thc phn t

C6H10CaO6.xH2O (x = 0 - 5)

Cng thc cu to

Khi lng phn t

218,22 (dng khan)

3. Cm quan

Bt tinh th hoc ht nh mu trng n kem, hu nh


khng mi. Dng pentahydrat i khi c th ln hoa.

4. Chc nng

Cht n nh, m, thc n cho men

5. Yu cu k thut
5.1. nh tnh
tan

Tan trong nc, khng tan trong ethanol.

Lactat

Phi c phn ng c trng ca lactat.

Calci

Phi c phn ng c trng ca calci.

5.2. tinh khit


Gim khi lng khi lm
kh

Khng c qu 30%

pH

Trong khong t 6,0 - 8,0 (Dung dch mu th 1/20).

acid

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

Mui magnesi v cc
mui kim

Khng c qu 1 %

Florid

Khng c qu 30 mg/kg

Ch

Khng c qu 2 mg/kg

5.3. Hm lng
C6H10CaO6

Khng thp hn 98,0% tnh theo cht kh.

10

QCVN 4 - 13 : 2010/BYT
6. Phng php th
6.1 nh tnh
Lactat

Th theo JECFA monograph 1 - Vol.4.

Calci

Th theo JECFA monograph 1 - Vol.4.

6.2 tinh khit


Gim khi lng khi lm
kh

- Th theo JECFA monograph 1 - Vol.4.


- Sy ti 120o trong 4 gi.

acid

Ha tan 1 g mu th trong 20 ml nc, thm 3 git dung


dch phenolphtalein (TS) v chun vi dung dch natri
hydroxyd 0,1 N. Th tch dung dch natri hydroxyd 0,1 N s
dng khng c qu 0,5 ml.

Mui magnesi v cc
mui kim

Cn 1 g mu th, ha tan trong 40 ml nc, thm 0,5 g


amoni clorid v thm khong 20 ml dung dch amoni oxalat
(TS). un trong b cch thy trong 1 gi, lm mt, thm
nc n 100 ml v lc. Ly 50 ml dch lc, thm 0,5 ml
acid sulfuric v cho bay hi hn hp n cn. Nung cn ti
khi lng khng i. ngui, cn v tnh hm lng %.
Khi lng cn khng c qu 5 mg.

Florid

- Th theo JECFA monograph 1 - Vol.4.

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 ti JECFA monograph 1 - Vol.4 phn
cc phng php phn tch cng c.

6.3. nh lng

Cn 350 mg (chnh xc n mg) mu th c lm kh


trc. Ha tan trong 150 ml nc c cha 2 ml dung dch
acid hydrocloric long (TS). Khuy u (tt nht khuy
bng my khuy t), trong khi khuy dng buret thm
khong 30 ml dung dch dinatri ethylendiamintetraacetat
0,05 M. Sau thm 15 ml natri hydroxyd (TS) v 300 mg
hn hp ch th xanh da tri hydroxy-naphtol, 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 10,91 mg C6H10CaO6.

11

QCVN 4 - 13 : 2010/BYT
Ph lc 3
YU CU K THUT V PHNG PHP TH
I VI KALI DIHYDROCITRAT
1. Tn khc, ch s

Monopotasium citrate; Potasium citrate monobasic


INS 332i
ADI khng gii hn

2. nh ngha
Tn ha hc

Kali dihydrogen citrat; Mui monokali ca acid 2-hydroxy1,2,3-propantricarboxylic

M s C.A.S.

866-83-1

Cng thc phn t

C6H7KO7

Cng thc cu to

Khi lng phn t

230,21

3. Cm quan

Tinh th trong hoc bt tinh th trng, khng mi.

4. Chc nng

Cht n nh, m, cht to phc kim loi, thc n cho


nm men.

5. Yu cu k thut
5.1. nh tnh
tan

D tan trong nc, rt t tan trong ethanol.

pH

Dung dch mu th 1/10 c pH trong khong 3,5 - 3,9.

Citrat

Phi c phn ng c trng ca citrat.

Kali

Phi c phn ng c trng ca kali.

5.2. tinh khit


Gim khi lng khi lm
kh

Khng c qu 0,5% (sy ti 105o trong 4 gi).

Oxalat

Khng c qu 0,04%.

Ch

Khng c qu 2,0 mg/kg.

5.3. Hm lng
C6H7NaO7

Khng thp hn 99,0% v khng c qu 101,0% tnh


theo ch phm khan.

6. Phng php th
6.1. nh tnh
Citrat

Th theo JECFA monograph 1 - Vol.4.


12

QCVN 4 - 13 : 2010/BYT
Kali

Th theo JECFA monograph 1 - Vol.4.

6.2 tinh khit


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 ti JECFA monograph 1 - Vol.4 phn
cc phng php phn tch cng c.

6.3. nh lng

Cn khong 180 mg (chnh xc n mg) mu th sy


kh, ha tan trong 25 ml nc v chun vi dung dch
natri hydroxyd 0,1 N, xc nh im kt thc chun bng
o th .
Mi ml dung dch natri hydroxyd 0,1 N tng ng vi
11,511 mg C6H7NaO7.

13

QCVN 4 - 13 : 2010/BYT
Ph lc 4

d
i

YU CU K THUT V PHNG PHP TH


I VI DINATRI HYDROGEN PHOSPHAT
1. Tn khc, ch s

Disodium hydrogen phosphate; Disodium phosphate;


Dibasic sodium phosphate; Disodium acid phosphate;
secondary sodium phosphate; Dinatri orthophosphat
INS 339ii
MTDI=70mg/kg th trng tnh theo Phospho t cc ngun
thc phm

2. nh ngha
Tn ha hc

Dinatri hydrogen phosphat; Dinatri hydrogen


orthophosphat; Dinatri hydrogen monophosphat;

M s C.A.S.

7558-79-4

Cng thc ha hc

Dng khan: Na2HPO4


Dng hydrat: Na2HPO4.xH2O

Khi lng phn t

141,98 (dng khan)

3. Cm quan

Dng khan: Bt trng, khng mi, ho nc.


Dng dihydrat: Tinh th trng, khng mi.
Dng heptahydrat: Tinh th trng, khng mi c th ln hoa
hoc dng bt ht nh.
Dng dodecahydrat: Tinh th hoc bt mu trng, khng
mi, c th ln hoa.
Cht n nh, cht nh ha, m, cht to kt cu

4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan

D tan trong nc, khng tan trong ethanol.

pH

9,0-9,6 (dung dch 1/100).

Natri

Phi c phn ng c trng ca natri.

Phosphat

Phi c phn ng c trng ca phosphat.

Orthophosphat

Phi c phn ng c trng ca orthophosphat.

5.2. tinh khit


Gim khi lng khi sy
kh

Dng khan: Khng c qu 5,0% (40oC trong 3 gi, sau


105oC trong 5 gi)
Dng dihydrat: Khng c qu 22,0% (40oC trong 3 gi,
sau 105oC trong 5 gi)
Dng heptahydrat: Khng c qu 50,0% (40oC trong 3
gi, sau 105oC trong 5 gi)
Dng dodecahydrat: Khng c qu 61,0% (40oC trong 3
gi, sau 105oC trong 5 gi)
14

QCVN 4 - 13 : 2010/BYT
Cc cht khng tan trong
nc

Khng c qu 0,2%.

Florid

Khng c qu 50,0 mg/kg.

Arsen

Khng c qu 3,0 mg/kg.

Ch

Khng c qu 4,0 mg/kg.

5.3. Hm lng Na2HPO4 Khng c thp hn 98,0% sau khi sy kh.


6. Phng php th
6.1. nh tnh
Natri

Th theo JECFA monograph 1 - Vol.4

Phosphat

Th theo JECFA monograph 1 - Vol.4

Orthophosphat

Ha tan 0,1g mu trong 10ml nc ct. Acid ha nh dung


dch bng acid acetic long (TS), thm 1ml dung dch bc
nitrat (TS). Trong dung dch phi xut hin kt ta mu
vng

6.2. tinh khit


Florid

Th theo JECFA monograph 1 - Vol.4 - phng php I


hoc III.

Arsen

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

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 ti JECFA monograph 1 - Vol.4 phn
cc phng php phn tch cng c.

6.3. nh lng

Cn khong 6,5g mu th, chnh xc n mg, mu th


c lm kh trc, cho vo cc 250ml. Thm 50ml dung
dch acid hydrocloric 1N v 50ml nc ct, khuy u n
khi mu tan ht. Cho in cc ca pH k thch hp vo
dung dch v chun lng acid d bng dung dch natri
hydroxyd 1N n im un ti khong pH = 4, ghi li th
tch c trn buret, tnh ton th tch (A) acid hydrocloric 1N
mu th tiu th. Tip tc chun n im un ti
khong pH=8,8; ghi li th tch trn buret v tnh th tch
dung dch (B) natri hydroxyd 1N tiu tn chun
gia 2 im un (pH=4 n pH=8,8).
Nu (A) bng hoc nh hn (B), mi ml HCl 1N trong th
tch (A) tng ng vi 142,0mg Na2HPO4.
Nu (A) ln hn (B), mi ml natri hydroxyd 1N trong hiu
th tch 2(B)-(A) tng ng vi 142,0mg Na2HPO4.

15

QCVN 4 - 13 : 2010/BYT
Ph lc 5
YU CU K THUT V PHNG PHP TH
I VI DIKALI HYDROGEN PHOSPHAT
1. Tn khc, ch s

Dipotassium hydrogen phosphate; Dibasic potassium


phosphate; Dipotassium monophosphate; Dipotassium
phosphate; Dipotassium acid phosphate; Secondary
potassium phosphate
INS 340ii
MTDI = 70 mg/kg th trng tnh theo Phospho t cc ngun
thc phm

2. nh ngha
Tn ha hc

Dikali hydrogen phosphat; Dikali hydrogen orthophosphat;


Dikali hydrogen monophosphat

M s C.A.S.

7758-11-4

Cng thc ha hc

K2HPO4

Khi lng phn t

174,18

3. M t

Dng bt ht, tinh th hoc khi khng mu hoc c mu


trng; dng tan chy

4. Chc nng

Cht n nh, cht m, cht to phc kim loi, thc phm


cho nm men

5. Yu cu k thut
5.1. nh tnh
tan

D tan trong nc, khng tan trong ethanol.

pH

8,7-9,3 (dung dch 1/100).

Kali

Phi c phn ng c trng ca kali.

Phosphat

Phi c phn ng c trng ca phosphat.

Orthophosphat

Phi c phn ng c trng ca orthophosphat.

5.2. tinh khit


Gim khi lng khi sy
kh

Khng c qu 5% (105oC trong 4 gi).

Cc cht khng tan trong


nc

Khng c qu 0,2%.

Fluorid

Khng c qu 10,0 mg/kg.

Arsen

Khng c qu 3,0 mg/kg

Ch

Khng c qu 4,0 mg/kg.

16

QCVN 4 - 13 : 2010/BYT
5.3. Hm lng K2HPO4

Khng c thp hn 98,0% sau khi sy kh

6. Phng php th
6.1. nh tnh
Kali

Th theo JECFA monograph 1 - Vol.4

Phosphat

Th theo JECFA monograph 1 - Vol.4

Orthophosphat

Ha tan 0,1 g mu th trong 10 ml nc ct, acid ha nh


dung dch bng acid acetic long (TS) v thm 1 ml bc
nitrat (TS). Trong dung dch phi xut hin kt ta mu
vng

6.2. tinh khit


Fluorid

Cn 5 g mu th cho vo mt bnh cu ct 250 ml, thm 25


ml nc, 50 ml acid percloric, 5 git dung dch bc nitrat (1
trong 2) v vi vin bi thy tinh. Ni bnh cu vi 1 ng sinh
hn c gn nhit k v mt ng mao qun sc kh, u
nhit k v ng mao qun phi ngp trong dung dch cha
trong bnh. Gn mt phu nh git cha nc hoc b sinh
hi nc vo ng mao qun. t bnh trn aming c l
sao cho 1/3 y bnh tip xc vi ngn la. Tin hnh ct
n khi nhit trong bnh t 1350C. Thm nc t phu
vo bnh hoc cho hi nc qua bnh duy tr nhit
trong bnh lun t 1350C -1400C. Tip tc ct n khi thu
c 225-240 ml dch ct sau pha long dch ct thu
c vi nc n 250 ml, lc u. Ly 50 ml dung
dch ny cho vo mt ng Nessler 100 ml. Trong mt ng
Nessler tng t khc ly 50 ml nc lm mu chng.
Thm vo mi ng 0,1 ml dung dch natri alizarinsulfonat (1
trong 1000) lc v 1 ml dung dch hydroxylamin (1 trong
4000) mi pha, lc u. Thm tng git dung dch natri
hydroxyd 0,05 N vo ng cha dch ct, va thm va
khuy, n khi mu ng cha dch ct ging vi mu ng
chng, l mu hng nht. Sau thm vo mi ng chnh
xc 1 ml dung dch acid hydrocloric 0,1 N v lc u. S
dng buret chia vch 0,05 ml thm t t va dung dch
thori nitrat (1 trong 4000) vo ng cha dch ct sau khi
lc u mu ca dung dch chuyn v mu hng nht. Ghi
th tch dung dch thori nitrat (1 trong 4000) s dng,
thm chnh xc cng lng dung dch thori nitrat (1 trong
4000) nh vy vo ng chng, lc u. Dng buret thm
dung dch natri fluorid (TS) (10 g F / ml) vo ng chng
cho mu hai ng ging nhau sau khi pha long v cng th
tch. Lc u, yn cho bt kh thot ht trc khi so
mu. Kim tra im tng ng bng cch thm 1-2 git
dung dch natri fluorid (TS) vo ng chng. S thay i
mu r rt s xy ra. Ghi li th tch dung dch natri fluorid
(TS) s dng. Th tch dung dch natri flourid dng cho
ng chng phi khng qu 1 ml.

17

QCVN 4 - 13 : 2010/BYT
Arsen

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

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 ti JECFA monograph 1 - Vol.4 phn
cc phng php phn tch cng c.

6.3. nh lng
Cn khong 6,5 g (chnh xc n mg ) mu th, c
lm kh trc, cho vo cc 250 ml. Thm 50 ml dung dch
acid hydrocloric 1 N v 50 ml nc ct, khuy u n khi
mu tan ht. Cho in cc ca pH k thch hp vo dung
dch v chun lng acid d bng dung dch natri
hydroxyd 1 N n im un ti pH~4, ghi li th tch c
trn buret, tnh th tch (A) acid hydrocloric 1 N mu th
s dng. Tip tc chun bng dung dch natri hydroxyd
1 N n im un ti pH~8,8; ghi li th tch trn buret v
tnh th tch dung dch (B) natri hydroxyd 1N s dng
chun gia 2 im un (pH~4 n pH~8,8).
Nu (A) (B), mi ml acid hydrocloric 1 N trong th tch (A)
tng ng vi 174,2 mg K2HPO4.
Nu (A)>(B), mi ml natri hydroxyd 1 N trong hiu th tch
2(B)-(A) tng ng vi 174,2 mg K2HPO4.

18

QCVN 4 - 13 : 2010/BYT
Ph lc 6
YU CU K THUT V PHNG PHP TH
I VI TRICALCI PHOSPHAT
1. Tn khc, ch s

Calcium phosphate, tribasic; Calcium phosphate kt ta;


INS 341iii
MTDI = 70 mg/kg th trng tnh theo phospho t cc ngun
thc phm

2. nh ngha

Bao gm hn hp vi cc t l khc nhau ca cc mui


calci phosphat, thnh phn gn ng l 10CaO.3P2O5.H2O.
Ch phm thng mi cn c phn loi theo ch s
chun .

3. Cm quan

Dng bt mu trng, khng mi, bn trong khng kh.

4. Chc nng

Cht n nh, cht chng ng vn, m.

5. Yu cu k thut
5.1. nh tnh
tan

Kh tan trong nc, khng tan trong ethanol, tan trong acid
hydrocloric long v acid nitric long.

Calci

Phi c phn ng c trng ca calci.

Phosphat

Phi c phn ng c trng ca phosphat.

5.2. tinh khit


Gim khi lng khi nung

Khng c qu 10% sau khi nung n khi lng khng


i ti 825 oC.

Fluorid

Khng c qu 50 mg/kg.

Ch

Khng c qu 4 mg/kg.

5.3. Hm lng
Ca3(PO4)2

Khng c thp hn tng ng 90% Ca3(PO4)2 tnh


theo ch phm sau khi nung.

6. Phng php th
6.1. nh tnh
Calci

Ha tan khong 100 mg mu th bng cch un nng vi 5


ml dung dch acid hydrocloric long (TS) v 5 ml nc.
Thm nh git dung dch amoniac (TS) vo hn hp, va
thm va lc u, sau thm 5 ml dung dch amoni
oxalat (TS). Trong dung dch xut hin kt ta trng.

Phosphat

Ha tan mu th trong acid nitric d, un nng hn hp,


thm dung dch amoni molybdat (TS). Trong dung dch xut
hin kt ta mu vng.

6.2 tinh khit


Fluorid

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


19

QCVN 4 - 13 : 2010/BYT
hoc III
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.

6.3. nh lng
Cn 200 mg (chnh xc n 0,1 mg) mu th, ho tan trong
hn hp gm 10ml dung dch acid nitric long (TS) v 25 ml
nc. Lc nu cn, ra kt ta, thm dung dch amoniac
(TS) vo dch lc va to kt ta nh. Sau ha
tan kt ta bng cch thm 1 ml dung dch acid nitric long
(TS). Chnh nhit v 50o, thm 75 ml dung dch amoni
molybdat (TS). Gi nhit ti 50o trong 30 pht, thnh
thong khuy. Gn ra ta 1 hoc hai ln, mi ln vi 30
n 40 ml nc. Chuyn ta sang mt phu lc v ra ta
bng dung dch kali nitrat (1/100) n khi dch ra khng
cn acid khi th bng giy qu. Chuyn ta, giy lc vo
mt bnh kt ta, thm 40 ml natri hydroxyd 1N, lc u n
khi kt ta tan han ton, thm 3 git dung dch
phenolphtalein (TS), sau chun kim d bng acid
sulfuric 1N.
Mi ml dung dch natri hydroxyd 1N tng ng vi 6,743
mg Ca3(PO4)2.

20

QCVN 4 - 13 : 2010/BYT
Ph lc 7
YU CU K THUT V PHNG PHP TH
I VI AMONI POLYPHOSPHAT
1. Tn khc, ch s

INS 452v
MTDI = 70 mg/kg th trng, tnh theo phospho t cc ngun
thc phm

2. nh ngha
Tn ha hc

Amoni polyphosphat

M s C.A.S.

6833-79-9

Cng thc ho hc

Hn hp d th cc mui amoni ca acid polyphosphoric c


trng ngng mch thng c cng thc chung: Hn+2PnO3n+1

3. Cm quan

Dng dung dch lng

4. Chc nng

Cht n nh, to phc kim loi, cht nh ho

5. Yu cu k thut
5.1. nh tnh
tan

Tan hon ton trong nc

pH

4,0 9,0 (dung dch 1%)

Amoni

Phi c phn ng c trng ca amoni.

Phosphat

Phi c phn ng c trng ca phosphat.

5.2. tinh khit


Phosphat mch vng

Khng vt qu 8,0% tnh theo P2O5

Fluorid

Khng vt qu 10,0 mg/kg

Arsen

Khng vt qu 3,0 mg/kg

Ch

Khng vt qu 4,0 mg/kg.

5.3. Hm lng

Khng c thp hn 55,0% v khng c qu 75,0% tnh


theo P2O5 trn ch phm khan

6. Phng php th
6.1 nh tnh
Amoni

Th theo JECFA monograph 1 - Vol.4

Phosphat

- Trn u 0,5 g mu vi 10 ml acid HNO3 v 50 ml nc, un


si trong 30 pht v ngui.
- Th theo JECFA monograph 1 - Vol.4

6.2 tinh khit


21

QCVN 4 - 13 : 2010/BYT
Phosphat mch vng

Th theo JECFA monograph 1 - Vol.4

Fluorid

Th theo JECFA monograph 1 - Vol.4

Arsen

Th theo JECFA monograph 1 - Vol.4

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.

6.3 nh lng
Tin hnh nh ch dn Xc nh photphat tnh theo P2O5 ,
Phng php I, Vol. 4.

22

QCVN 4 - 13 : 2010/BYT
Ph lc 8
YU CU K THUT V PHNG PHP TH
I VI NATRI HYDROGEN CARBONAT
1. Tn khc, ch s

Sodium hydrogen carbonate; bt n; soa bicarbonat; natri


bicarbonat
INS 500(ii)
ADI khng gii hn

2. nh ngha
Tn ha hc

Natri hydrogen carbonat, natri acid carbonat

M s C.A.S.

144-55-8

Cng thc ha hc

NaHCO3

Khi lng phn t

84,01

3. Cm quan

Khi tinh th hoc bt tinh th trng hoc khng mu

4. Chc nng

Cht n nh, cht kim ha, bt ni, m, cht to xp

5. Yu cu k thut
5.1. nh tnh
tan

Tan trong nc, khng tan trong ethanol.

pH

8,0 - 8,6 (dung dch mu th 1/100 trong nc lnh, khng


lc)

Natri

Phi c phn ng c trng ca natri.

Carbonat

Phi c phn ng c trng ca carbonat.

5.2. tinh khit


Gim khi lng khi lm
kh

Khng c qu 0,25% (Trn silicagel, trong 4 gi).

Cc cht khng tan trong


nc

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

Mui amoni

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

Ch

Khng c qu 2,0 mg/kg.

5.3. Hm lng NaHCO3

Khng c thp hn 99,0% sau khi sy kh.

6. Phng php th
6.1. nh tnh
Natri

Th theo JECFA monograph 1 - Vol.4.

Carbonat

Th theo JECFA monograph 1 - Vol.4.

23

QCVN 4 - 13 : 2010/BYT
6.2. tinh khit
Cc cht khng tan trong
nc

1 g mu th ho tan hon ton trong 20 ml nc phi thu


c dung dch trong.

Mui amoni

t nng 1 g mu th trong mt ng nghim. Khng c


c mi ammoniac.

Ch

- Th theo JECFA monograph 1 - Vol.4.


- Xc nh bng k thut quang ph hp th nguyn t
thch hp vi hm lng qui 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 3 g (chnh xc n mg) mu th sy kh, ha tan
trong nc, thm ch th l dung dch da cam methyl (TS)
v chun bng acid sunfuric 1 N.
Mi ml acid sulfuric 1 N tng ng vi 84,01 mg
NaHCO3.

24

QCVN 4 - 13 : 2010/BYT
Ph lc 9
YU CU K THUT V PHNG PHP TH
I VI KALI CARBONAT
1. Tn khc, ch s

INS 501(i)
ADI khng gii hn

2. nh ngha
Tn ha hc

Kali carbonat, mui kali ca acid carbonic

M s C.A.S.

584-08-7

Cng thc ha hc

Dng khan: K2CO3


Dng hydrat ha: K2CO3.1H2O

Khi lng phn t

138,21 (dng khan)

3. Cm quan

Bt d ht m, mu trng, khng mi. Dng hydrat ha


thng gp l tinh th hoc ht nh trng, trong.

4. Chc nng

Cht n nh, cht kim ha

5. Yu cu k thut
5.1. nh tnh
tan

Rt d tan trong nc, khng tan trong ethanol.

Kali

Phi c phn ng c trng ca kali.

Carbonat

Phi c phn ng c trng ca carbonat.

5.2. tinh khit

Ch

Dng khan: Khng c qu 5% (sy 180o trong 4 gi)


Dng hydrat ha : trong khong 10-18% (sy 180o trong
4 gi)
Khng c qu 2,0 mg/kg.

5.3. Hm lng K2CO3

Khng c thp hn 99,0% tnh theo cht kh

Gim khi lng khi sy


kh

6. Phng php th
6.1. nh tnh
Kali

Th theo JECFA monograph 1 - Vol.4.

Carbonat

Th theo JECFA monograph 1 - Vol.4.

6.2. tinh khit


Ch

- Th theo JECFA monograph 1 - Vol.4.


- Xc nh bng k thut quang ph hp th nguyn t
thch hp vi hm lng qui 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
25

QCVN 4 - 13 : 2010/BYT
cc phng php phn tch cng c.
6.3. nh lng
Cn 1 g (chnh xc n mg) mu th sy kh, ha tan
cn thn trong 50 ml acid sulfuric 1 N, thm ch th l dung
dch da cam methyl (TS) v chun acid d bng dung
dch natri hydroxyd 1N.
Mi ml dung dch acid sulfuric 1 N tng ng vi 69,11
mg K2CO3.

26

QCVN 4 - 13 : 2010/BYT
Ph lc 10
YU CU K THUT V PHNG PHP TH
I VI AMONI HYDROGEN CARBONAT
1. Tn khc, ch s

Amonium hydrogen carbonate; amoni bicarbonat


INS 503(ii)
ADI khng gii hn

2. nh ngha
Tn ha hc

Amoni hydrogcarbonat

M s C.A.S.

1066-33-7

Cng thc ha hc

CH5NO3

Cng thc cu to

NH4HCO3

Khi lng phn t

79,06

3. Cm quan

Tinh th trng hoc bt tinh th c mi ammoniac nh.

4. Chc nng

Cht n nh, bt ni.

5. Yu cu k thut
5.1. nh tnh
tan

D tan trong nc, khng tan trong ehtanol

pH

Khong 8,0 (dung dch 1/20).

Carbonat

Phi c phn ng c trng ca carbonat.

Amoni

Phi c phn ng c trng ca amoni.

Nhit

Khi b t nng, mu th ha hi m khng b than ha, hi


c tnh kim khi th bng giy qu m.

5.2. tinh khit


Cn khng bay hi

Khng c qu 500,0 mg/kg (S dng 4 g mu th trong


10 ml nc)

Clorid

Khng c qu 30,0 mg/kg (m t trong phn Phng


php th).

Sulfat

Khng c qu 70,0 mg/kg (m t trong phn Phng


php th).

Ch

Khng c qu 2,0 mg/kg (m t trong phn Phng


php th).

5.3. Hm lng NH4CO3

Khng c thp hn 99,0%

6. Phng php th

27

QCVN 4 - 13 : 2010/BYT
6.1. nh tnh
Carbonat

Th theo JECFA monograph 1 - Vol.4.

Amoni

Th theo JECFA monograph 1 - Vol.4.

6.2. tinh khit


Clorid

- Th theo JECFA monograph 1 - Vol.4.


- Ho tan 500 mg mu th trong 10ml nc nng, thm
khong 5mg natri carbonat, lm kh trn b cch thu. Th
cn thu c nh hng dn trong chuyn lun th gii
hn clorid. c ca dung dch thu c khng vt qu
c ca dung dch tin hnh nh trn i vi mu
-

chng c cha 15 g ion clorid (Cl ).


Sulfat

Ho tan 4g mu th trong 40ml nc. Thm 10mg natri


carbonat v 1ml hydrogen peroxyd 30% v lm kh trn b
cch thu. X l cn thu c theo hng dn trong
chuyn lun th gii hn sulfat. c ca dung dch thu
c khng qu c ca dung dch tin hnh nh trn
2-

i vi mu chng c cha 280 g ion sulfat (SO4 ).


Ch

- Th theo JECFA monograph 1 - Vol.4.


- Xc nh bng k thut quang ph hp th nguyn t
thch hp vi hm lng qui 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
Ly 10ml nc vo mt cc cn. Tin hnh xc nh b
(cc v nc). Thm vo cc 2g mu th (cn chnh xc
n mg). Chuyn ton b hn hp trong cc vo mt bnh
nn 250ml. Thm t t, va thm va lc 50ml acid
sulfuric 1N. Sau khi dung dch phn ng xong, trng ra
thnh bnh, thm ch th l dung dch da cam methyl (TS) v
chun acid d bng dung dch natri hydroxyd 1N.
Mi ml acid sulfuric 1N tng ng vi 79,06 mg
NH4HCO3.

28

QCVN 4 - 13 : 2010/BYT
Ph lc 11
YU CU K THUT V PHNG PHP TH
I VI KALI CLORID
1. Tn khc, ch s

Sylvite; Sylvine
INS 508
ADI khng gii hn

2. nh ngha
Tn ha hc

Kali clorid

M s C.A.S.

7447-40-7

Cng thc ha hc

KCl

Khi lng phn t

74,56

3. Cm quan

Tinh th khng mu hnh khi lp phng, lng tr hoc


thon di; hoc dng bt, ht nh mu trng; khng mi.

4. Chc nng

Cht n nh, gia v, cht to gel, thc n cho nm men.

5. Yu cu k thut
5.1. nh tnh
tan

D tan trong nc, khng tan trong ethanol.

Clorid

Phi c phn ng c trng ca clorid.

Kali

Phi c phn ng c trng ca kali.

5.2. tinh khit


Gim khi lng khi lm
kh
acid hoc kim

Khng c qu 1,0 % (105oC trong 2 gi).


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

29

QCVN 4 - 13 : 2010/BYT
Iodid hoc bromid

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

Natri

m tnh (m t trong phn Phng php th).

Ch

Khng c qu 2,0 mg/kg.

5.3. Hm lng KCl

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

6. Phng php th
6.1. nh tnh
Clorid

Th theo JECFA monograph 1 - Vol.4.

Kali

Th theo JECFA monograph 1 - Vol.4.

6.2. tinh khit


acid hoc kim

Cn 5 g mu th, ha tan trong 50 ml nc mi un si,


ngui, thm 3 git dung dch phenolphtalein (TS). Dung
dch khng c c mu hng. Sau thm 0,3 ml dung
dch natri hydroxyd 0,02 N, dung dch chuyn thnh mu
hng.

Iodid hoc bromid

Cn 2 g mu th, ha tan trong 6 ml nc, thm 1 ml


cloroform, sau thm nh git 5 ml hn hp gm dung
dch clor (TS) v nc (1:1 tt/tt), va thm va lc u.
Lp cloroform khng c c mu tm (khng bn) hoc
mu cam (bn).

Natri

Th theo JECFA monograph 1 - Vol.4.

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 ti JECFA monograph 1 - Vol.4 phn
cc phng php phn tch cng c.

6.3. nh lng
Cn khong 250 mg (chnh xc n mg) mu th lm
kh ha tan trong 50 ml nc trong mt bnh thy tinh nt
mi. Thm 50 ml dung dch bc nitrat 0,1 N, 3 ml acid nitric
v 5 ml nitrobenzen, va thm va lc mnh, thm 2 ml st
(III) amoni sulfat (TS). Chun lng bc nitrat d vi
dung dch amoni thiocyanat 0,1 N.
Mi ml dung dch bc nitrat 0,1 N tng ng vi 7,456
mg KCl.

30

QCVN 4 - 13 : 2010/BYT
Ph lc 12
YU CU K THUT V PHNG PHP TH
I VI KALI DIHYDROGEN PHOSPHAT
1. Tn khc, ch s

Potassium dihydrogen phosphate; Monobasic potassium


phosphate; Monopotassium monophosphate; Potassium
acid phosphate; Potassium biphosphate
INS 340i
MTDI=70mg/kg th trng tnh theo Phospho t cc ngun
thc phm

2. nh ngha
Tn ha hc

Kali dihydrogen phosphat; Monokali dihydrogen


orthophosphat; Monokali dihydrogen monophosphat

M s C.A.S.

7778-77-0

Cng thc ha hc

KH2PO4

Khi lng phn t

136,09

3. Cm quan

Dng tinh th khng mu, khng mi, dng ht trng hoc


dng bt tinh th

4. Chc nng

Cht n nh, m, tc nhn trung ha, cht to phc kim


loi, thc n cho nm men

5. Yu cu k thut
5.1. nh tnh
tan

D tan trong nc, khng tan trong ethanol.

pH

4,2 - 4,7 (dung dch 1/100).

Kali

Phi c phn ng c trng ca kali.

Phosphat

Phi c phn ng c trng ca phosphat.

Orthophosphat

Phi c phn ng c trng ca orthophosphat.

5.2. tinh khit


Gim khi lng khi sy
kh

Khng c qu 2,0% (105oC trong 4 gi).

Cc cht khng tan trong


nc

Khng c qu 0,2%.

Florid

Khng c qu 10,0 mg/kg.

Arsen

Khng c qu 3,0 mg/kg.

Ch

Khng c qu 4,0 mg/kg.

5.3. Hm lng KH2PO4

Khng c thp hn 98,0% sau khi sy kh.


31

QCVN 4 - 13 : 2010/BYT
6. Phng php th
6.1. nh tnh
Kali

Th theo JECFA monograph 1 - Vol.4.

Phosphat

Th theo JECFA monograph 1 - Vol.4.

Orthophosphat

Thm dung dch bc nitrat (TS) vo 5ml dung dch mu th


(dung dch 1/100). Trong dung dch phi xut hin kt ta
mu vng.

6.2 tinh khit


Fluorid

Cn 5 g mu th cho vo mt bnh cu ct 250 ml, thm 25


ml nc, 50 ml acid percloric, 5 git dung dch bc nitrat (1
trong 2) v vi vin bi thy tinh. Ni bnh cu vi 1 sinh hn
c gn nhit k v mt ng mao qun sc kh, u nhit k
v ng mao qun phi ngp trong dung dch cha trong
bnh. Gn mt phu nh git cha nc hoc b sinh hi
nc vo ng mao qun. t bnh trn aming c l sao
cho 1/3 y bnh tip xc vi ngn la. Tin hnh ct n
khi nhit trong bnh t 135o. Thm nc t phu vo
bnh hoc cho hi nc qua bnh duy tr nhit trong
bnh lun t 135o-140o. Tip tc ct n khi thu c 225240 ml dch ct sau pha long dch ct thu c vi
nc n 250 ml, lc u. Ly 50 ml dung dch ny cho
vo mt ng Nessler 100 ml. Trong mt ng Nessler tng
t khc ly 50 ml nc lm mu chng. Thm vo mi ng
0,1 ml dung dch natri alizarinsulfonat (1 trong 1000) lc
v 1 ml dung dch hydroxylamin (1 trong 4000) mi pha, lc
u. Thm tng git dung dch natri hydroxyd 0,05 N vo
ng cha dch ct, va thm va khuy, n khi mu ng
cha dch ct ging vi mu ng chng l mu hng nht.
Sau thm vo mi ng chnh xc 1 ml dung dch acid
hydrocloric 0,1 N v lc u. S dng buret chia vch 0,05
ml thm t t va dung dch thori nitrat (1 trong 4000)
vo ng cha dch ct sau khi lc u mu ca dung
dch chuyn v mu hng nht. Ghi th tch dung dch thori
nitrat (1 trong 4000) s dng, thm chnh xc cng
lng dung dch thori nitrat (1 trong 4000) nh vy vo ng
chng, lc u. Dng buret thm dung dch natri fluorid
(TS) (10 g F / ml) vo ng chng cho mu hai ng
ging nhau sau khi pha long v cng th tch. Lc u,
yn cho bt kh thot ht trc khi so mu. Kim tra im
tng ng bng cch thm 1-2 git dung dch natri
fluorid (TS) vo ng chng. S thay i mu r rt s xy
ra. Ghi li th tch dung dch natri fluorid (TS) s dng.
Th tch dung dch natri florid (TS) s dng cho ng chng
khng c qu 1 ml.

Arsen

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

Ch

- Th theo JECFA monograph 1 - Vol.4


32

QCVN 4 - 13 : 2010/BYT
- 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.
6.3. nh lng
Cn khong 5,0 g (chnh xc n mg) mu th c
lm kh trc, cho vo cc 250 ml. Thm 100 ml nc ct
v 5 ml dung dch acid hydrocloric 1 N, khuy u n khi
mu tan ht. Cho in cc ca pH k thch hp vo dung
dch v chun t t (khuy u lin tc) lng acid d
bng dung dch natri hydroxyd 1 N, n im un ti pH~4.
Ghi li th tch c trn buret, tnh th tch (A) acid
hydrocloric 1 N s dng (nu cn). Tip tc chun
bng dung dch natri hydroxyd 1 N n im un ti
pH~8,8; ghi li th tch trn buret v tnh th tch dung dch
(B) natri hydroxyd 1N tiu tn chun gia 2 im
un (pH~4 n pH~8,8).
Mi ml natri hydroxyd 1 N ca hiu th tch (B)-(A) tng
ng vi 136,1 mg KH2PO4.

33

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