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CNG HA X HI CH NGHA VIT NAM

QCVN 4-11: 2010/BYT

QUY CHUN K THUT QUC GIA


V PH GIA THC PHM CHT IU CHNH ACID
National technical regulation
on Food Additives Acidity regulators

H NI - 2010

Li ni u
QCVN 4-11:2010/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 28/2010/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 IU CHNH ACID
National technical regulation on Food Additives Acidity regulators
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 iu chnh acid 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 iu chnh acid 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 iu chnh acid: l ph gia thc phm c s dng vi mc ch
thay i hoc kim sot tnh acid hoc tnh kim 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 iu chnh acid
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 kali acetat.

1.2. Ph lc 2:

Yu cu k thut v phng php th i vi natri acetat

1.3. Ph lc 3:

Yu cu k thut v phng php th i vi natri diacetat

1.4. Ph lc 4:

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

1.5. Ph lc 5:

Yu cu k thut v phng php th i vi acid lactic

1.6. Ph lc 6:

Yu cu k thut v phng php th i vi acid malic

1.7. Ph lc 7:

Yu cu k thut v phng php th i vi acid fumaric

1.8. Ph lc 8:

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

1.9. Ph lc 9:

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

1.10. Ph lc 10: Yu cu k thut v phng php th i vi acid citric


1.11. Ph lc 11: Yu cu k thut v phng php th i vi natri
dihydrogen citrat
1.12. Ph lc 12: Yu cu k thut v phng php th i vi trinatri citrat
1.13. Ph lc 13: Yu cu k thut v phng php th i vi trikali citrat
1.14. Ph lc 14: Yu cu k thut v phng php th i vi acid tartric
1.15. Ph lc 15: Yu cu k thut v phng php th i vi dinatri tartrat
1.16. Ph lc 16: Yu cu k thut v phng php th i vi kali natri tartrat
1.17. Ph lc 17: Yu cu k thut v phng php th i vi mononatri
ortho-phosphat
1.18. Ph lc 18: Yu cu k thut v phng php th i vi acid orthophosphoric
1.19. Ph lc 19: Yu cu k thut v phng php th i vi trinatri orthophosphat
1.20. Ph lc 20: Yu cu k thut v phng php th i vi dicalci orthophosphat
1.21. Ph lc 21: Yu cu k thut v phng php th i vi calci malat
1.22. Ph lc 22: Yu cu k thut v phng php th i vi natri fumarat
1.23. Ph lc 23: Yu cu k thut v phng php th i vi magnesi
carbonat
1.24. Ph lc 24: Yu cu k thut v phng php th i vi nhm kali sulfat
1.25. Ph lc 25: Yu cu k thut v phng php th i vi natri hydroxyd
1.26. Ph lc 26: Yu cu k thut v phng php th i vi kali hydroxyd
1.27. Ph lc 27: Yu cu k thut v phng php th i vi calci hydroxyd

1.28. Ph lc 28: Yu cu k thut v phng php th i vi calci oxyd


1.29. Ph lc 29: Yu cu k thut v phng php th i vi natri nhm
phosphat, acid
1.30. Ph lc 30: Yu cu k thut v phng php th i vi natri nhm
phosphat, kim
1.31. Ph lc 31: Yu cu k thut v phng php th i vi glucono deltalacton
1.32. Ph lc 32: Yu cu k thut v phng php th i vi acid acetic
bng
1.33. Ph lc 33: Yu cu k thut v phng php th i vi acid adipic
1.34. Ph lc 34: Yu cu k thut v phng php th i vi monocalci
ortho-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 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 iu chnh acid 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 iu chnh acid
Vic kim tra cht lng, v sinh an ton i vi cc cht iu chnh acid
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 iu chnh acid 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 KALI ACETAT
1. Tn khc, ch s
INS 261
ADI khng gii hn
2. nh ngha
Tn ha hc

Kali acetat

M s C.A.S.

127-08-2

Cng thc ha hc

C2H3KO2

Cng thc cu to

CH3-COOK

Khi lng phn t

98,14

3. Cm quan

Tinh th tan, khng mu hoc bt tinh th mu trng,


khng mi hoc hi c mi acetic

4. Chc nng

Cht iu chnh acid, cht m, cht bo qun chng vi


sinh vt.

5. Yu cu k thut
5.1. nh tnh
tan

Rt d tan trong nc, d tan trong ethanol.

pH

7,5 9,0 (dung dch 1 trong 20).

Kali

Phi c phn ng c trng ca kali

Acetat

Phi c phn ng c trng ca acetat

5.2. tinh khit


Gim khi lng khi sy
kh

Khng c qu 8,0% (Sy ti 150 oC trong 2h)

Tnh kim

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

Natri

m tnh.

Ch

Khng c qu 2,0 mg/kg.

5.3. Hm lng
CH3-COOK

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

6. Phng php th
6.1. tinh khit
Tnh kim

Ho tan 1 g mu th trong 20 ml nc un si ngui


va chun b, thm 3 git dung dch phenolphatalein (TS).
Nu dung dch c mu hng th lm mt mu bng cch
cho thm dung dch acid hydrocloric 0,1 N, lng acid
hydrocloric 0,1 N s dng khng c qu 0,5 ml.

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
Cn 200 mg mu th c lm kh trc, chnh xc n
mg, ho tan trong 25 ml dung dch acid acetic bng. Cho
thm 2 git dung dch tm tinh th (TS) v chun vi dung
dch acid percloric 0,1 N trong acid acetic bng. Tin hnh
xc nh mu trng v hiu chun kt qu chun nu
cn.
Mi ml dung dch acid percloric 0,1N tng ng vi 9,814
mg C2H3KO2.

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

INS 262(i)
ADI khng gii hn

2. nh ngha
Tn ha hc

Natri acetat

M s C.A.S.

127-09-3

Cng thc ha hc

C2H3NaO2 . nH2O (n = 0 hoc 3)

Cng thc cu to

CH3COONa . nH2O (n = 0 hoc 3)

Khi lng phn t

Dng khan: 82,03; dng trihydrat: 136,08

3. Cm quan

Dng khan: bt d ht m hoc ht mu trng, khng mi


Dng trihydrat: tinh th trong sut, khng mu hoc bt, ht
tinh th, khng mi hoc c mi acetic nh. Ln hoa trong
khng kh kh, m.

4. Chc nng

Cht iu chnh acid.

5. Yu cu k thut
5.1. nh tnh
tan

Rt d tan trong nc, tan trong ethanol.

pH

8,0 9,5 (dung dch 1 trong 100)

Natri

Phi c phn ng c trng ca natri.

Acetat

Phi c phn ng c trng ca acetat.

Nhit

Dng khan: Khi lm nng dn dn mu th, u tin mu


th tan chy chm v si, sau b phn hu v gii phng
ra hi c mi aceton. Dung dch cn li c phn ng kim
vi giy qu.
Dng trihydrat: Khi lm nng dn dn mu th, mu th b
tan chy. Sau khi nc bc hi ht phn cn li l dng
bt. Tip tc gia nhit mnh, phn bt cn li b tan chy,
to thnh hn hp rn lng, sau phn hu v gii phng
ra hi c mi aceton. Dung dch cn li c phn ng kim
vi giy qu.

5.2. tinh khit


Gim khi lng khi sy
kh

Dng khan: khng c qu 2,0% (sy ti 120 oC trong


4h).
Dng trihydrat: gia 36,0 v 42,0% (sy ti 120 oC trong
4h).

Kali

m tnh.

Tnh acid v tnh kim

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

Ch

Khng c qu 2,0 mg/kg.

5.3. Hm lng
C2H3NaO4

Khng c thp hn 98,5% sau khi sy kh

6. Phng php th
6.1 tinh khit
Tnh acid v tnh kim

Dng khan: Ho tan 1,2 g mu th trong 20 ml nc ct


un si ngui mi chun b. Cho thm 2 git dung dch
phenolphtalein (TS) v gi dung dch ti 10 oC. Nu dung
dch khng c mu th cho thm dung dch natri hydroxyd
0,1 N n khi dung dch c mu hng, lng dung dch
natri hydroxyd 0,1 N s dng khng c qu 0,1 ml . Nu
dung dch c mu hng, cho thm dung dch acid
hydrocloric 0,1 N lm mt mu, lng dung dch acid
hydrocloric 0,1 N s dng khng c qu 0,1 ml.
Dng trihydrat: Cn 2 g mu th v tin hnh xc nh nh
i vi dng khan trn.

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

Cn 200 mg mu th, chnh xc n mg, ly t php th


Gim khi lng khi sy kh. Ho tan trong 40 ml dung
dch acid acetic bng, cho thm 2 git dung dch tm tinh th
(TS) v chun vi dung dch acid percloric 0,1 N trong
acid acetic bng. Tin hnh xc nh mu trng v hiu
chun nu cn thit. Mi ml dung dch acid percloric 0,1 N
tng ng vi 8,203 mg C2H3NaO4.

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

Sodium diacetate
INS 262(ii)
ADI= 0 - 15 mg/kg th trng

2. nh ngha
Tn ha hc

Natri hydrogen diacetat

M s C.A.S.

Natri acetat: 127-09-3. Acid acetic: 64-19-7

Cng thc ha hc

C4H7NaO4 . xH2O

Khi lng phn t

142,09 (dng khan)

3. Cm quan

Cht rn kt tinh d ht m, mu trng c mi acetic.

4. Chc nng

Cht iu chnh acid, cht chng nm, chng i thiu,


cht to phc kim loi.

5. Yu cu k thut
5.1. nh tnh
tan

D tan trong nc.

Th nung

Nung mu th. Cn cn li c tnh kim, cn ny khi c


acid ho s si bt.

Acetat

Phi c phn ng c trng ca acetat.

Natri

Phi c phn ng c trng ca natri.

5.2. tinh khit


Nc

Khng c qu 2,0% (Phng php Karl Fischer)

pH

4,5 - 5,0 (dung dch 1 trong 10).

Acid formic v cc tp
cht c th oxy ha

Vt (m t trong phn Phng php th).

Aldehyd

Khng c qu 0,2% (tnh theo propanal).

Ch

Khng c qu 2,0 mg/kg.

5.3. Hm lng

39,0 - 41,0% i vi acid acetic t do; 58,0 - 60,0% i vi


natri acetat

6. Phng php th
6.1 tinh khit
Acid formic v cc tp
cht c th oxy ha

Ha tan 2,5 g mu th trong 5 ml nc ct. Thm 2,5 ml


dung dch kali dicromat 0,1N v 6 ml acid sulfuric v
yn trong 1 pht. Thm 20 ml nc, lm ngui v 15 oC v
thm 1 ml dung dch kali iodid (TS). Xut hin ngay mu
vng nht hoc nu nht.

Aldehyd

Ha tan 5 g mu th trong 10 ml nc v tin hnh ct.


Ly 5 ml dch ct u tin, thm 10 ml dung dch thy ngn
(II) clorid (TS) v kim ha bng dung dch natri hydroxyd.
yn trong 5 pht, acid ha bng dung dch acid sulfuric
long (TS). Dung dch ch c php hi 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.

6.2. nh lng

Natri acetat:
Cn 0,5 g mu th, chnh xc n mg, ho tan vo 50 ml
acid acetic bng. Lm kh bn ngoi ca t hp in cc
calomel-thu tinh gn vi 1 pH k, nhng in cc vo trong
dung dch, t pH k v mc hiu chnh +mV, sau thm
acid percloric 0,1N, mi ln thm mt th tch tng i ln
cho n gn im tng ng (s dao ng ca kim c
th d nhn thy). Sau gim th tch acid percloric 0,1N
ca mi ln thm l 0,1 ml n khi sau mi ln thm dung
dch, in th gim r rt. Xy dng th biu din tng
quan gi th tch acid percloric 0,1N vi in th o c,
qua nh lng cht cn chun tng ng vi im
gia ca bc nhy th.
V x N x 0,1421
% Natri diacetat =
x 100
w
Trong :
V: th tch ca dung dch acid percloric, ml
N: chun chnh cc ca dung dch acid percloric
w: trng lng ca mu th, g
Acid acetic t do:
Cn 4 g mu th, chnh xc n mg, v ho tan trong 50 ml
dung dch nc ct pha long. Chun dung dch vi dung
dch natri hydroxyd N c s dng dung dch phenolphatalein
(TS) lm cht ch th.
V x N x 0,060
% Acid acetic t do=
x 100
w
Trong :
V: th tch ca dung dch natri hydroxyd, ml
N: chun chnh cc ca dung dch natri hydroxyd
w: trng lng ca mu th, g

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

INS 263
ADI khng gii hn.

2. nh ngha
Tn ha hc

Calci acetat

M s C.A.S.

62-54-4

Cng thc ha hc

Dng khan: C4H6CaO4


Dng hydrat ha: C4H6CaO4.H2O; C4H6CaO4.xH2O (x<1)

Cng thc cu to

Khi lng phn t

Dng khan: 158,17; dng monohydrat 176,18

3. Cm quan

Cht rn kt tinh cng knh, d ht m, mu trng; c th


c mi acid acetic nh. Dng monohydrat c th dng hnh
kim, ht hoc dng bt.

4. Chc nng

Cht iu chnh acid, cht chng nm, chng i thiu,


cht n nh, m.

5. Yu cu k thut
5.1. nh tnh
tan

D tan trong nc, khng tan trong ethanol.

Acetat

Phi c phn ng c trng ca acetat.

Calci

Phi c phn ng c trng ca calci.

5.2. tinh khit


Gim khi lng khi sy
kh

Khng c qu 11% (dng monohydrat - sy ti 155oC


n khi lng khng i).

pH

6 9 (dung dch 1/10)

Tp cht khng tan trong


nc

Khng c qu 0,3%.

Acid formic v cc tp
cht c th oxy ha

Vt (m t trong phn Phng php th).

Aldehyd

Vt (m t trong phn Phng php th).

Ch

Khng c qu 2,0 mg/kg.

5.3. Hm lng
C4H6CaO4

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

6. Phng php th
6.1 tinh khit
Tp cht khng tan trong
nc

Cn 10 g mu th, chnh xc n mg, ha tan trong 100


ml nc nng. Lc qua chn lc Gooch ( c cn b,
chnh xc n 0,2 mg), ra k chn bng nc ct. Sy
chn ti 105 oC trong 2 gi. ngui, cn v tnh hm
lng %. (Trng lng cn kh khng c qu 30 mg).

Acid formic v cc tp
cht c th oxy ha

Ha tan 1 g mu th trong 5 ml nc ct. Thm 2,5 ml


dung dch kali dicromat 0,1N v 6 ml acid sulfuric v
yn trong 1 pht. Thm 20 ml nc, lm ngui v 15 oC v
thm 1 ml dung dch kali iodid (TS). Xut hin ngay mu
vng nht hoc nu nht.

Aldehyd

Ha tan 2 g mu th trong 10 ml nc v tin hnh ct.


Ly 5 ml dch ct u tin, thm 10 ml dung dch thy ngn
(II) clorid (TS) v kim ha bng dung dch natri hydroxyd.
yn trong 5 pht, acid ha bng acid sulfuric long (TS).
Dung dch ch c php hi 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.

6.2. nh lng
1. Hm lng calci:
Cn 2,5 g mu th, chnh xc n mg, cho vo cc, ha tan
trong 5 ml dung dch acid hydrocloric long nng. ngui,
chuyn vo bnh nh mc 250 ml, pha long n vch
bng nc ct, lc u. Ly 50 ml dung dch ny vo cc
400 ml, thm 100 ml nc ct, 25 ml dung dch natri
hydroxyd (TS), 40 mg hn hp ch th murexid v 3 ml dung
dch xanh lc naphtol (TS) (c th s dng ch th thay th l
2,5g xanh lam hydroxynaphtol, trong trng hp ny khng
s dng dung dch xanh lc naphtol). Chun bng dung
dch dinatri ethylendiamin tetraacetat 0,05M n khi dung
dch c mu xanh m.
Mi ml dinatri ethylendiamin tetraacetat 0,05M tng ng
vi 7,909mg C4H6CaO4.
2. Hm lng acid:
Nhi n na ct sc k (ng knh 1,5 cm, cao 20cm)
bng nha trao i cation mnh (Amberlite IR120, Amberlite
IR100, Duolit C III, Dorvex 50, Lewatit KS, Ion exchanger I
Merck). Cho dung dch acid hydrocloric 0,1 N ln ct t trn
xung di, vi vi ct c kha n khi phn nha ngp
trong dung dch, yn 1-2 gi. Rt ht acid v ra ct

bng nc ct (khong 1 lt nc), th dch ra gii bng


cch ly 20 ml dch ra gii, nh 1 git dung dch natri
hydroxyd 0,02N v mt git dung dch phenolphtalein (TS),
n khi th dch ra gii khng cho mu hng th ngng qu
trnh ra ct. Cn (chnh xc n mg) 0,05g mu th trc
c sy kh 155 oC n khi lng khng i, cho
vo bnh thy tinh. Ha tan trong 15 ml nc ct v rt t t
ln u ct. Ra bnh v ra gii ct bng khong 200 ml
nc ct. Thu dch ra gii vo bnh nn. Thm hai git
dung dch phenolphtalein (TS) v chun vi dung dch
natri hydroxyd 0,1 N s dng microburet.
Mi ml dung dch natri hydroxyd 0,1 N tng ng vi
7,909 mg C4H6CaO4.

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

INS 270
ADI khng gii hn

2. nh ngha

Thu c bng cch ln men lactic ng hoc tng hp,


c th cha cc sn phm ngng t nh acid lactic, lactat,
dilactid. Ch phm thng mi thng l dung dch 5090%. Ngoi ra cn c ch phm dng rn cha khong
100-125% acid lactic c th chun c (ch : Acid
lactic d ht nc v khi c c bng cch un si hoc
chng ct to ra sn phm ngng t, khi pha long sn
phm ny vi nc v un nng n b thy phn thnh acid
lactic.

Tn ha hc

Acid lactic, Acid 2-hydroxypropanoic, Acid 2hydroxypropionic

M s C.A.S.

50-21-5 (L-:79-33-4; D-:10326-41-7; DL-:598-82-3

Cng thc phn t

C3H6O3

Cng thc cu to

O
H3C

OH
OH

Khi lng phn t

90,08

3. Cm quan

Dng lng, snh khng mu hoc dng bt, rn, c mu


trng n vng nht

4. Chc nng

Cht iu chnh acid

5. Yu cu k thut
5.1. nh tnh
tan

Dng lng: tan trong nc v trong ethanol


Dng rn: t tan trong nc, tan trong aceton

Acid

Phi c phn ng c trng ca acid.

Lactat

Phi c phn ng c trng ca lactat.

5.2. tinh khit


Tro sulfat

Khng c qu 0,1%
(Phng php I, cn 2 g mu th. Gi li tro th st).

Clorid

Khng c qu 0,2%.

Sulfat

Khng c qu 0,25%

St

Khng c qu 10,0 mg/kg

Cyanid

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

Acid citric, oxalic,


phosphoric hoc tartric

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

Cc ng

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

Cc hp cht d b than
ha

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

Ch

Khng c qu 2,0 mg/kg.

5.3. Hm lng C3H6O3

Khng thp hn 95,0% v khng c qu 105% so vi


nng ghi trn nhn. i vi th tinh khit, pha dung
dch acid lactic 40% trong nc, s dng nng ghi
trn nhn pha. Nu cn, un nng ha tan hon
ton. Nu nng ghi nhn < 40% th c th s dng trc
tip ch phm tin hnh th tinh khit m khng cn
pha long. Lng mu cn ly trong cc php th l lng
acid lactic tnh c t nng ghi trn nhn ca ch
phm, ngoi tr trong php th Cc ng v Cc hp
cht d b than ha, trong 2 php th ny thut ng mu
th dng ch dung dch acid lactic 40%. Gii hn ca
cc php th da trn lng acid lactic, tnh t nng ghi
trn nhn.

6. Phng php th
6.1 tinh khit
Clorid

Cn (chnh xc n mg) mt lng mu th tng ng


vi 50 g acid lactic, ha tan trong 50 ml nc, trung ha
bng dung dch natri hydroxyd 1/4 vi ch th l qu tm.
Thm 2 ml dung dch kali cromat (TS) v chun vi
dung dch bc nitrat 0,1 N cho n khi dung dch bt u
nht. Mi ml dung dch bc nitrat 0,1 N tng ng vi
3,545 mg clorid.

Sulfat

Cn (chnh xc n mg) mt lng mu th tng ng


vi 50 g acid lactic, cho vo cc c m 600 ml, ha tan
trong 200 ml nc, trung ho bng dung dch natri
hydroxyd 1/2 n khi pH khong 4,5 - 6,5 v hiu chnh pH
cui cng bng dung dch kim long. Lc nu cn, un
nng dch lc hoc dung dch trong n nhit ngay di
im si. Thm 10 ml dung dch bari clorid, khuy u v
un si hn hp trong 5 pht, yn trong thi gian ti
thiu 2 gi, tt nht l qua m. Thu kt ta sulfat vo
mt chn nung Gooch, ra ta n khi ht clorid, sy ta
v nung 600o n khi lng khng i. Cn cn bari
sulfat sau nung. Hm lng sulfat trong mu c tnh
bng cch ly khi lng cn bari sulfat sau nung nhn vi
0,412.

St

Ly phn cn chun b trong phn th tro sulfat, thm 2 ml


dung dch acid hydrocloric 1/2, cho bay hi n kh trn b

cch thy nc si. Ha tan cn trong 1 ml acid


hydrocloric, pha long n 40 ml bng nc. Thm 40 mg
tinh th amoni persulfat v 10 ml dung dch amoni
thiocyanat (TS). Tin hnh lm song song mu chng thay
mu th bng 2 ml dung dch st (20 g Fe). So snh mu
ca ng th v ng chng, mu ca ng th khng c
m hn mu ca ng chng
Cyanid

Cn 0,1 g mu th, thm 3 ml dung dch natri hydroxyd


20%, un nng trong b cch thy 10 pht. Sau khi lm
mt, thm 1 git dung dch phenolphtalein (TS) v thm
tng git dung dch acid acetic long (TS) n khi hn hp
khng cn mu hng. Thm 3 git dung dch acid acetic
long (TS) v pha long bng nc ti 40 ml. Thm 0,6
ml dung dch cloramin T (pha nh sau: hon tan 1 g
cloramin T, C7H7NaO2SCl.3H2O, v nc n 100 ml,
s dng dung dch ngay sau khi pha). Thm 10 ml dung
dch pyridin-pyrazolon (pha nh sau: ha tan 0,5 g 1phenyl-3-methyl-5-pyrazolon trong 100 ml nc nng 75o,
lm mt v nhit phng, trn vi 20 ml pyridin c cha
0,025 g bis-1-phenyl-3-methyl-5-pyrazolon, s dng dung
dch ngay sau khi pha), yn trong 25 pht. Dung dch
khng c c mu xanh (gii hn ~ 1 mg/kg).

Acid citric, oxalic,


phosphoric hoc tartric

Cn 1 g mu th, ho tan trong 10 ml nc, thm 40 ml


dung dch calci hydroxyd (TS), un si trong 2 pht. Dung
dch khng c c.

Cc ng

Thm 5 ml dung dch mu th vo trong 10 ml dung dch


ng (II) tartrat kim (TS), Khng c xut hin kt ta .

Cc hp cht d b than
ha

Thm t t, cn thn 5 ml dung dch mu th c nhit


15 o ln trn 5 ml dung dch acid sulfuric (TS) c gi ti
15o. Sau 15 pht, vng tip xc gia 2 lp dung dch khng
c c mu xm m.

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
Cn (chnh xc n mg) lng mu th tng ng vi 3
g acid lactic, chuyn vo bnh 250 ml, thm 50 ml dung dch
natri hydroxyd 1 N, lc u v un si trong 20 pht. Thm
dung dch phenolphtalein (TS), khi dung dch cn nng,
chun lng kim d vi acid sulfuric 1 N, tin hnh
lm 1 mu trng song song.
Mi ml dung dch natri hydroxyd 1N tng ng vi 90,08
mg C3H6O3.

Ph lc 6
YU CU K THUT V PHNG PHP TH I VI ACID MALIC
1. Tn khc, ch s

dl-Malic acid; acid 2-hydroxybutandioic


INS 296
ADI Khng gii hn

2. nh ngha
Tn ha hc

Acid dl-malic; acid 2-hydroxybutandioic; acid


hydroxysuccinic

M s C.A.S.

6915-15-7

Cng thc phn t

C4H6O5

Cng thc cu to

COOH
CHOH
CH2
COOH

Khi lng phn t

134,1

3. Cm quan

Bt tinh th hoc ht mu rng hoc gn nh trng

4. Chc nng

Cht iu chnh acid

5. Yu cu k thut
5.1. nh tnh
tan

Rt tan trong nc, d tan trong ethanol.

Khong nng chy

127o - 132o.

Malat

Phi c phn ng c trng ca malat (dch th l dung


dch mu th 1/20 c trung ha bng dung dch
amoniac (TS)).

5.2. tinh khit


Acid fumaric v acid
maleic

Acid fumaric khng c qu 1,0%


Acid maleic khng c qu 0,05%.

Ch

Khng c qu 2,0 mg/kg.

5.3. Hm lng C4H6O5

Khng thp hn 99,0%

6. Phng php th
6.1 tinh khit
Ch

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


nh bng k thut AAS/ICP-AES 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.

6.2. nh lng
Cn khong 2 g (chnh xc n mg) mu th, ha tan trong
40 ml nc mi un si, ngui, thm 2 git dung dch
phenolphtalein (TS) v chun vi dung dch natri
hydroxyd 1 N n khi dung dch bt u c mu hng nht
bn trong 30 giy.
Mi ml dung dch natri hydroxyd 1 N tng ng vi
67,04 mg C4H6O5.

Ph lc 7
YU CU K THUT V PHNG PHP TH I VI ACID FUMARIC
1. Tn khc, ch s

INS 297
ADI khng gii hn

2. nh ngha
Tn ha hc

Acid trans-butendioic, acid trans-1,2-ethylen-dicarboxylic

M s C.A.S.

110-17-8

Cng thc ha hc

C4H4O4

Cng thc cu to

COOH
C
C

HOOC

Khi lng phn t

116,07

3. Cm quan

Bt hoc ht tinh th trng, khng mi.

4. Chc nng

Cht iu chnh acid, cht to mi.

5. Yu cu k thut
5.1. nh tnh
tan

Tan trong ethanol; kh tan trong nc v trong diethyl


ether.

pH

2,0-2,5 (dung dch 1 trong 30).

Acid 1,2 dicarboxylic

Phi c phn ng c trng ca Acid 1,2 dicarboxylic.

Lin kt i

Phi c phn ng c trng ca lin kt i.

5.2. tinh khit


Gim khi lng khi sy
kh

Khng c qu 0,5%. (120 oC, trong 4 gi).

Khong nhit nng


chy

286oC 302 oC (ng mao qun kn, lm nng nhanh).

Tro sulfat

Khng c qu 0,1%. (Th 2 g mu th - Phng php


1).

Acid maleic

Khng c qu 0,1%.

Ch

Khng c qu 2,0 mg/kg.

5.3. Hm lng C4H4O4

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

6. Phng php th
6.1 nh tnh
Acid 1,2 dicarboxylic

Ly 50 g mu th vo trong ng nghim, thm 2-3 mg


resorcinol v 1 ml acid sulfuric, lc u, un nng 130 oC
trong 5 pht v ngui. Pha long vi nc ct cho 5
ml v nh tng git dung dch natri hydroxyd (2 trong 5)
kim ha dung dch, ngui v pha long vi nc ct
n 10 ml. Khi soi di n t ngoi dung dch c hunh
quang xanh lam nh lc.

Lin kt i

Thm 10 ml nc ct vo 0,5 g mu th, un si ha


tan. Thm 2 hoc 3 git dung dch brom (TS) vo dung dch
nng. Mu ca dung dch brom s mt.

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.

6.3. nh lng
Cn 1g mu th, chnh xc n mg, chuyn vo bnh nn
250 ml, thm 50 ml methanol, ho tan mu bng cch lm
m nh trn b cch thu. ngui, thm dung dch
phenolphtalein (TS) v chun vi dung dch natri
hydroxyd 0,5 N cho n khi xut hin mu hng bn trong
t nht 30 giy. Tin hnh xc nh mu trng v hiu
chun nu cn.
Mi ml dung dch natri hydroxyd 0,5 N tng ng vi
29,02 mg C4H4O4.

Ph lc 8
YU CU K THUT V PHNG PHP TH I VI NATRI LACTAT
1. Tn khc, ch s

INS 325
ADI khng gii hn

2. nh ngha
Tn ha hc

Natri lactat, Natri 2-hydroxypropanoat

M s C.A.S.

72-17-3

Cng thc phn t

C3H5NaO3

Cng thc cu to

Khi lng phn t

112,06 (dng khan)

3. Cm quan

Dng lng, trong, khng mu, khng mi hoc c mi c


trng nh

4. Chc nng

Cht iu chnh acid, cht chng oxy ha, cht lm m

5. Yu cu k thut
5.1. nh tnh
Nung

Nung tro ha mu th. Tro c tnh kim v si bt khi thm acid.

Phn ng mu

Cho 2 ml mu th ln trn 5 ml dung dch catechol 1/100


trong acid sulfuric. Vng tip xc gia 2 dung dch phi c
mu m.

Lactat

Phi c phn ng c trng ca lactat.

Natri

Phi c phn ng c trng ca natri.

5.2. tinh khit


Tnh acid

t yu cu

pH

Dung dch mu th 1/5 c pH trong khong 6,5 -7,5.

Ch

Khng c qu 2,0 mg/kg.

5.3. Hm lng
C3H5NaO3

Khng thp hn 95,0% v khng c qu 110,0% so vi


lng ghi trn nhn. Yu cu ny da trn dung dch natri
lactat 60,0% (kl/kl) trong nc.

6. Phng php th
6.1 tinh khit
Tnh acid

trung ha 1 g mu th vi ch th l dung dch


phenolphtalein (TS) khng s dng qu 0,5 ml dung dch
natri hydroxyd 0,1 N.

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
Cn 0,6 g (chnh xc n mg) mu cho vo mt cc nh v
cho bay hi n kh. Thm vo cn cn li 60 ml hn hp
anhydrid acetic/acid acetic bng (1/5), khuy u n khi
cn tan hon ton. Thm dung dch tm tinh th (TS) v
chun vi dung dch acid percloric 0,1 N n im kt
thc dung dch c mu xanh.
Mi ml dung dch acid percloric 0,1 N tng ng vi
11,21 mg C3H5NaO3.

Ph lc 9
YU CU K THUT V PHNG PHP TH I VI KALI LACTAT
1. Tn khc, ch s

INS 326
ADI khng gii hn

2. nh ngha
Tn ha hc

Kali lactat, Kali 2-hydroxypropanoat

M s C.A.S.

996-31-6

Cng thc phn t

C3H5KO3

Cng thc cu to

O
CH3
O

OH

Khi lng phn t

128,17 (dng khan)

3. Cm quan

Dng lng, hi nht, trong, khng mi hoc c mi c


trng nh

4. Chc nng

Cht iu chnh acid, cht h tr chng oxy ha

5. Yu cu k thut
5.1. nh tnh
Nung

Nung tro ha mu th. Tro c tnh kim v si bt khi thm


acid.

Phn ng mu

Cho 2 ml mu th ln trn 5 ml dung dch catechol 1/100


trong acid sulfuric. Vng tip xc gia 2 dung dch phi c
mu m.

Lactat

Phi c phn ng c trng ca lactat.

Kali

Phi c phn ng c trng ca kali.

5.2. tinh khit


Tnh acid

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

Cc hp cht kh

Mu th khng c c phn ng kh i vi dung dch


Fehling.

Ch

Khng c qu 2,0 mg/kg.

5.3. Hm lng C3H5KO3

Khng thp hn 95,0% v khng c qu 110,0% so vi


lng ghi trn nhn. Yu cu ny da trn dung dch natri
lactat 60,0% (kl/kl) trong nc.

6. Phng php th
6.1 tinh khit
Tnh 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 0,2 ml.

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
Cn 0,6 g (chnh xc n mg) mu cho vo mt cc nh v
cho bay hi n kh. Thm vo cn cn li 60 ml hn hp
anhydrid acetic/acid acetic bng (1/5), khuy u n khi
cn tan hon ton. Thm dung dch tm tinh th (TS) v
chun vi dung dch acid percloric 0,1 N n im kt
thc dung dch c mu xanh. Tin hnh lm mu trng
song song v hiu chnh kt qu nu cn.
Mi ml dung dch acid percloric 0,1 N tng ng vi
12,82 mg C3H5KO3.

Ph lc 10
YU CU K THUT V PHNG PHP TH I VI ACID CITRIC
1. Tn khc, ch s

INS 330
ADI khng gii hn

2. nh ngha

Acid citric c th c sn xut t cc ngun nh chanh


hoc nc da hay ln men t dung dch ng hoc cc
mi trng thch hp s dng chng Candida spp. hoc
chng Aspegillus niger khng c c tnh.

Tn ha hc

Acid 2-hydroxy-1,2,3-propantricarboxylic

M s C.A.S.

Dng khan: 77-92-9


Dng monohydrat: 5949-29-1

Cng thc phn t

Dng khan: C6H8O7


Dng monohydrat: C6H8O7.H2O

Cng thc cu to

CH2
HO

C
CH2

COOH
COOH

CH2
HO

COOH

Dng khan

C
CH2

COOH
COOH

.HO
2

COOH

Dng monohydrat

Khi lng phn t

Dng khan: 192,13


Dng monohydrat: 210,14

3. Cm quan

Tinh th rn mu trng hoc khng mu, khng mi. Dng


monohydrat c th ln hoa trong khng kh kh.

4. Chc nng

Cht iu chnh acid, cht to phc kim loi, cht h tr


chng oxy ha, hng liu

5. Yu cu k thut
5.1. nh tnh
tan

D tan trong ethanol, rt tan trong nc, t tan trong ether.

Citrat

Phi c phn ng c trng ca citrat.

5.2. tinh khit


Hm lng nc

Dng khan: Khng c qu 0,5%


Dng monohydrat: Khng c thp hn 7,5% v khng
c qu 8,8%. (Phng php Karl-Fischer).

Tro sulfat

Khng c qu 0,05%.

Oxalat

Khng c qu 100,0 mg/kg.

Sulfat

Khng c qu 150,0 mg/kg.

Cc hp cht d than ha t yu cu (m t trong phn Phng php th).


Ch

Khng c qu 0,5 mg/kg.

5.3. Hm lng C6H8O7

Khng thp hn 99,5% v khng c qu 100,5% tnh


theo ch phm khan.

6. Phng php th
6.1 tinh khit
Oxalat

Th theo hng dn ti JECFA monograph 1 - Vol.4 chuyn lun th gii hn Oxalat dng 1 g mu th. o
hp th quang ti 520 nm, s dng cuvet 10 mm. hp
th quang ca dch th o c phi nh hn 0,023 n v
o hp th.

Sulfat

Th theo hng dn ti JECFA monograph 1 - Vol.4 chuyn lun th gii hn Sulfat: dng 20 g mu th v 6 ml
dung dch acid sulfuric lm chun.

Cc hp cht d than ha un nng 1 g mu th ovi 10 ml acid sulfuric 98% trong b


cch thy nhit 90 trong 60 pht. Mu ca dung dch
khng c m hn mu ca dung dch i chng
Matching fluid K (25o) ( hp th quang khi o ti bc
sng 470 nm, s dng cuvet 10 mm khng c qu 0,5
n v hp 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
Cn khong 2,5 g (chnh xc n mg) mu th, cho vo
mt bnh cn b. Ha tan trong 40 ml nc v chun
vi dung dch natri hydroxyd 1 N, dng ch th l dung dch
phenolphtalein (TS).
Mi ml dung dch natri hydroxyd 1 N tng ng vi
64,04 mg C6H8O7.

Ph lc 11
YU CU K THUT V PHNG PHP TH I VI NATRI DIHYDROGEN
CITRAT
1. Tn khc, ch s

Monosodium citrate; Sodium citrate monobasic


INS 331i
ADI khng gii hn

2. nh ngha
Tn ha hc

Mononatri citrat; Mui natri ca acid 2-hydroxy-1,2,3propantricarboxylic

Cng thc phn t

C6H7NaO7

Cng thc cu to

Khi lng phn t

214,11

3. Cm quan

Tinh th mu trng hoc bt tinh th khng mi.

4. Chc nng

m, cht to phc kim loi, cht iu chnh acid.

5. Yu cu k thut
5.1. nh tnh
tan

D tan trong nc, thc t khng tan trong ethanol.

pH

Dung dch mu th 1/10 c pH trong khong 3,4 - 3,8.

Citrat

Phi c phn ng c trng ca citrat.

Natri

Phi c phn ng c trng ca natri.

5.2. tinh khit


Gim khi lng khi lm
kh

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

Oxalat

t yu cu.

Ch

Khng c qu 2,0 mg/kg.

5.3. Hm lng
C6H7NaO7

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

6. Phng php th
6.1 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.
6.2. nh lng
Cn khong 180 mg (chnh xc n mg) mu th, 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
10,706 mg C6H7NaO7.

Ph lc 12
YU CU K THUT V PHNG PHP TH I VI TRINATRI CITRAT
1. Tn khc, ch s

Trisodium citrate; Sodium citrate;


INS 331iii
ADI khng gii hn

2. nh ngha
Tn ha hc

Trinatri citrat; Mui trinatri ca acid 2-hydroxy-1,2,3propantricarboxylic; Mui trinatri ca acid -hydroxy
tricarballynic.

M s C.A.S.

68-04-2

Cng thc phn t

Dng khan: C6H5Na3O7


Dng hydrat: C6H5Na3O7.xH2O

Cng thc cu to

CH2

COO

+
3Na

HO

COO
_

CH2

COO

Khi lng phn t

258,07 (dng khan)

3. Cm quan

Tinh th khng mu hoc bt tinh th mu trng, khng


mi. Dng hydrat ha bao gm dihydrat v
pentahemihydrat.

4. Chc nng

Cht iu chnh acid, m, cht to phc kim loi, cht


n nh nh tng.

5. Yu cu k thut
5.1. nh tnh
tan

D tan trong nc, thc t khng tan trong ethanol.

Citrat

Phi c phn ng c trng ca citrat.

Natri

Phi c phn ng c trng ca natri.

5.2. tinh khit


Gim khi lng khi lm
kh

Dng khan: Khng c qu 1,0%


Dng dihydrat: Khng c qu 13,0%
Dng pentahemihydrat: Khng c qu 30,0%
(sy ti 180o n khi lng khng i).

Tnh kim

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 mg/kg.

5.3. Hm lng
C6H5Na3O7

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


kh.

6. Phng php th
6.1 nh tnh
Citrat

Ly 5 ml dung dch mu th 1/10, thm 1 ml dung dch calci


clorid (TS) v 3 git dung dch xanh bromothymol (TS), acid
ha nh bng dung dch acid hydrocloric long (TS). Thm
dung dch natri hydroxyd (TS) n khi dung dch chuyn
thnh mu xanh da tri trong, sau un si dung dch
trong 3 pht, lc nh trong khi un. Trong dung dch xut
hin kt ta trng, kt ta ny khng tan trong dung dch
natri hydroxyd (TS) nhng tan trong dung dch acid acetic
(TS).
Ly 10 ml dung dch mu th 1/10, thm 1 ml dung dch
thy ngn (II) sulfat (TS). un si hn hp v thm vi git
dung dch kali permanganat (TS). Trong dung dch xut
hin kt ta trng.

Natri

Ly 5 ml dung dch mu th 1/20, acid ha bng dung dch


acid acetic (TS) v thm 1 ml dung dch uranyl km acetat
(TS). Sau vi pht trong dung dch xut hin kt ta mu
vng.

6.2 tinh khit


Tnh kim

Dung dch mu th 1/20 phi c tnh kim khi th bng


qu. Thm 0,2 ml dung dch acid sulfuric 0,1 N v 1 git
dung dch phenolphtalein (TS) vo 10 ml dung dch mu
th, dung dch khng c c mu hng.

Oxalat

Ly 10 ml dung dch mu th 1/10, thm 5 git dung dch


acid acetic long (TS) v 2 ml dung dch calci clorid (TS).
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, cho vo
cc 250 ml. Thm 100 ml acid acetic bng, khuy n khi
tan hon ton v chun vi dung dch acid percloric 0,1
N, s dng ch th l dung dch tm tinh th (TS). Tin hnh
lm mt mu trng song song v hiu chnh kt qu nu
cn.
Mi ml dung dch acid percloric 0,1 N tng ng vi
8,602 mg C6H5Na3O7.

Ph lc 13
YU CU K THUT V PHNG PHP TH I VI TRIKALI CITRAT
1. Tn khc, ch s

Potasium citrate;
INS 332ii
ADI khng gii hn

2. nh ngha
Tn ha hc

Trikali citrat; Mui trikali ca acid 2-hydroxy-1,2,3propantricarboxylic; Mui trikali ca acid -hydroxy
tricarballynic.

M s C.A.S.

866-84-2

Cng thc phn t

C6H5K3O7.H2O

Cng thc cu to

CH2

COO

COO

HO

3K

.HO
2

CH2

COO

Khi lng phn t

324,42

3. Cm quan

Tinh th trong, khng mu d chy ra, hoc bt dng ht


mu trng, khng mi.

4. Chc nng

Cht iu chnh acid, m, cht to phc kim loi, cht


n nh.

5. Yu cu k thut
5.1. nh tnh
tan

Rt d tan trong nc, thc t khng tan trong ethanol.

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 6,0% (sy ti 180oC trong 4 gi).

Tnh kim

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 C6H5K3O7 Khng thp hn 99,0% tnh theo ch phm c lm


kh.

6. Phng php th
6.1 nh tnh
Citrat

Ly 5 ml dung dch mu th 1/10, thm 1 ml dung dch


calci clorid (TS) v 3 git dung dch xanh bromothymol
(TS), acid ha nh bng dung dch acid hydrocloric long
(TS). Thm dung dch natri hydroxyd (TS) n khi dung
dch chuyn thnh mu xanh da tri trong, sau un si
dung dch trong 3 pht, lc nh trong khi un. Trong dung
dch xut hin kt ta trng, kt ta ny khng tan trong
dung dch natri hydroxyd (TS) nhng tan trong dung dch
acid acetic (TS).
Ly 10 ml dung dch mu th 1/10, thm 1 ml dung dch
thy ngn (II) sulfat (TS). un si hn hp v thm vi
git dung dch kali permanganat (TS). Trong dung dch
xut hin kt ta trng.

Kali

Trong mi trng acid hydrocloric, dung dch mu th s


to kt ta tinh th mu vng vi dung dch platin clorid
(TS), acid ha bng dung dch acid acetic (TS) v thm 1
ml dung dch uranyl km acetat (TS). Kt ta ny khi nung
s cn li kali clorid v platin.

6.2. tinh khit


Tnh kim

Dung dch mu th 1/20 phi c tnh kim khi th bng


qu. Thm 0,2 ml dung dch acid sulfuric 0,1 N v 1 git
dung dch phenolphtalein (TS) vo 10 ml dung dch mu
th, dung dch khng c c mu hng.

Oxalat

Ly 10 ml dung dch mu th 1/10, thm 5 git dung dch


acid acetic long (TS) v 2 ml dung dch calci clorid (TS).
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 250 mg (chnh xc n mg) mu th c
lm kh. Thm 40 ml acid acetic bng, un nh ha
tan hon ton. ngui v nhit phng thm 2 git
dung dch tm tinh th (TS) v chun vi dung dch acid
percloric 0,1 N. Tin hnh lm mt mu trng song song
v hiu chnh kt qu nu cn.
Mi ml dung dch acid percloric 0,1 N tng ng vi
10,21 mg C6H5K3O7.

Ph lc 14
YU CU K THUT V PHNG PHP TH I VI ACID TARTRIC
1. Tn khc, ch s

L(+)-tartaric acid
INS 334
ADI = 0 - 30 mg/kg th trng

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

Acid L(+)-tartaric; Acid L-2,3-dihydroxybutanedioic; Acid L2,3-dihydroxysuccinic


87-69-4

Cng thc phn t

C4H6O6

Cng thc cu to

COOH
H

OH

HO

COOH

Khi lng phn t

150,09

3. Cm quan

Tinh th khng mu, trong m hoc bt tinh th, ht nh


mu trng; khng mi.

4. Chc nng

Cht h tr chng oxy ha, cht iu chnh acid, cht


to phc kim loi, hng liu.

5. Yu cu k thut
5.1. nh tnh
tan

Rt d tan trong nc v d tan trong ethanol.

quay cc ring

Dung dch mu th 1/10 hu tuyn.

Tartrat

Phi c phn ng c trng ca tartrat.

5.2. tinh khit


Gim khi lng khi lm
kh
Gc quay cc ring

Khng c qu 0,5% (trn P2O5 trong 3 gi).


D
20 =

trong khong t +11,5o n + 13,5o.

Tro sulfat

Khng c qu 0,1 %.

Sulfat

Khng c qu 0,05%.

Oxalat

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

Ch

Khng c qu 2,0 mg/kg.

5.3. Hm lng C4H6O6

Khng thp hn 99,5% tnh theo ch phm lm kh.

6. Phng php th
6.1 tinh khit
Tro sulfat

Phng php I, cn 2 g mu.

Sulfat

Th 0,4 g mu, phi t yu cu trong chuyn lun th gii


hn sulfat, s dng 0,2 mg ion sulfat (SO42-) lm mu
chng.

Oxalat

Trung ha 10 ml dung dch mu th 1/10 bng dung dch


amoniac (TS) , thm 10 ml calci sulfat (TS), 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.

6.2 nh lng
Cn khong 2 g (chnh xc n mg) mu th c lm
kh, ha tan trong 40 ml nc, thm dung dch
phenolphtalein (TS) v chun vi dung dch natri
hydroxyd 1 N n khi dung dch bt u c mu hng nht
bn trong 30 giy.
Mi ml dung dch natri hydroxyd 1 N tng ng vi
75,04 mg C4H6O6.

Ph lc 15
YU CU K THUT V PHNG PHP TH I VI DINATRI TARTRAT
1. Tn khc, ch s

Sodium tartrate; Sodium dextro-tartrate; Natri L(+)-tartrat


INS 335ii
ADI = 0 - 30 mg/kg th trng

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

Dinatri L-tartrat; Dinatri (+)-tartrat; Mui dinatri ca acid L(+)


-2,3-dihydroxybutandioic.
868-18-8

Cng thc phn t

C4H4Na2O6.2H2O

Cng thc cu to

COO
H

OH

HO

+
2 Na 2 H2O

COO

Khi lng phn t

230,8

3. Cm quan

Tinh th trong, khng mu, khng mi.

4. Chc nng

Cht iu chnh acid, cht to phc kim loi v cht n


nh cho cc sn phm tht v ch bin xc xch.

5. Yu cu k thut
5.1. nh tnh
tan

1 g ch phm tan trong 3 ml nc, khng tan trong ethanol.

Natri

Phi c phn ng c trng ca natri.

Tartrat

Phi c phn ng c trng ca tartrat.

5.2. tinh khit


Gim khi lng khi lm
kh

Khng c qu 17,0% v khng thp hn 14,0%. (sy ti


150oC trong 3 gi).

pH

Dung dch mu th 1/10 c pH trong khong 7,0 - 7,5.

Oxalat

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

Ch

Khng c qu 2,0 mg/kg.

5.3. Hm lng
C4H4Na2O6

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

6. Phng php th
6.1 tinh khit
Oxalat

Thm 5 git dung dch acid acetic long (TS) v 2 ml calci


clorid (TS) vo 10 ml dung dch mu th 10%, 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.

6.2. nh lng
Cn khong 1,5 g (chnh xc n mg) mu th c
sy kh vo mt chn nung bng s cn b. u tin
nung nh n khi ch phm b than ha hon ton, trnh
cho ch phn b than ha lun tip xc vi ngn la.
ngui , t chn nung vo mt cc thy tinh, dng a thy
tinh dm nh khi cn than ha. nguyn chn nung v
a trong cc, thm vo cc thy tinh 50 ml nc, 50 ml
dung dch acid sulfuric 0,5 N. y cc v un si trong 30
pht. Lc v ra cn bng nc nng n khi dch ra
trung tnh khi th bng qu, ngui. Gp dch lc v dch
ra. Thm dung dch da cam methyl (TS) v chun acid
d bng dung dch natri hydroxyd 0,5 N.
Mi ml dung dch acid sulfuric 0,5 N tng ng vi
0,0097 g C4H4Na2O6.
Ngoi ra c th tin hnh nh lng theo cch sau:
Cn 0,45 g (chnh xc n mg) mu th c lm kh
trc, cho vo cc 250 ml, thm 100 ml acid acetic bng v
khuy u hn hp bng my khuy t n khi mu tan
hon ton. Chun dung dch vi dung dch acid percloric
0,1 N trong acid acetic bng, xc nh im tng ng
bng o th, khi gn n im tng ng chun
chm li, mi ln ch thm 0,2 ml thuc th.
Mi ml dung dch natri acid percloric 0,1 N trong acid acetic
bng tng ng vi 0,0097 g C4H4Na2O6.

Ph lc 16
YU CU K THUT V PHNG PHP TH I VI KALI NATRI TARTRAT
1. Tn khc, ch s

Potassium sodium tartrate; Potassium sodium dextrotartrate; Mui Rochelle, Mui Seignette
INS 337
ADI = 0 - 30 mg/kg th trng

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

Kali natri L-tartrat; Kali natri (+)-tartrat; Mui kali natri ca


acid L-2,3-dihydroxybutandioic.
304-59-6

Cng thc phn t

C4H4NaKO6.4H2O

Cng thc cu to

COO K+
H

OH

HO

H
_

.4HO
2

COO Na

Khi lng phn t

282,23

3. Cm quan

Tinh th khng mu hoc bt tinh th mu trng.

4. Chc nng

Cht iu chnh acid, cht to phc kim loi v cht n


nh cho cc sn phm tht v ch bin xc xch v phomt.

5. Yu cu k thut
5.1. nh tnh
tan

1g ch phm tan trong 1 ml nc, khng tan trong ethanol.

Kali

Phi c phn ng c trng ca kali.

Natri

Phi c phn ng c trng ca natri.

Tartrat

Phi c phn ng c trng ca tartrat.

5.2. tinh khit


Gim khi lng khi lm
kh

Khng c qu 26,0% v khng thp hn 21,0%


(sy ti 150o trong 3 gi).

pH

Dung dch mu th 1/10 c pH trong khong 6,5 - 7,5.

Oxalat

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

Ch

Khng c qu 2,0 mg/kg.

5.3. Hm lng
C4H4NaKO6

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

6. Phng php th
6.1 tinh khit
Oxalat

Thm 3 git dung dch acid acetic long (TS) v 2 ml calci


clorid (TS) vo 10 ml dung dch mu th 10%, 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.

6.2. nh lng
Cn khong 1,5 g (chnh xc n mg) mu th c
sy kh vo mt chn nung bng s cn b. u tin
nung nh n khi ch phm b than ha hon ton, trnh
cho ch phn b than ha lun tip xc vi ngn la. Nhit
cui cng khng c cao qu nhit nng .
ngui , t chn nung vo mt cc thy tinh, dng a thy
tinh dm nh khi cn than ha. nguyn chn nung v
a trong cc, thm vo cc thy tinh 50 ml nc, 50 ml
dung dch acid sulfuric 0,5 N. y cc v un si trong 30
pht. Lc v ra cn bng nc nng n khi dch ra
trung tnh khi th bng qu, ngui. Gp dch lc v dch
ra. Thm dung dch da cam methyl (TS) v chun acid
d bng dung dch natri hydroxyd 0,5 N.
Mi ml dung dch acid sulfuric 0,5 N tng ng vi
0,05254 g C4H4NaKO6.

Ph lc 17
YU CU K THUT V PHNG PHP TH
I VI ACID PHOSPHORIC
1. Tn khc, ch s

Phosphoric acid, orthophosphoric acid


INS 338
MTDI=70 mg/kg th trng tnh theo phospho t cc ngun
thc phm

2. nh ngha
Tn ha hc

Acid phosphoric; acid ortho-phosphoric

M s C.A.S.

7664-38-20

Cng thc ha hc

H3PO4

Khi lng phn t

98,00

3. Cm quan

Trong, khng mu, khng mi, dng dung dch snh

4. Chc nng

Cht iu chnh acid, cht to phc kim loi, cht h tr


chng oxy ho

5. Yu cu k thut
5.1. nh tnh
tan

C th trn vi nc v ethanol.

Acid

Acid mnh, ngay c khi nng rt long.

Phosphat

Phi c phn ng c trng ca phosphat.

5.2. tinh khit


Cc nitrat

Khng c qu 5,0 mg/kg.

Cc acid d bay hi

Khng c qu 10,0 mg/kg tnh theo acid acetic.

Clorid

Khng c qu 200,0 mg/kg tnh theo clor.

Sulfat

Khng c qu 0,15 %.

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 H3PO4

Khng thp hn 75,0 %, v khng thp hn mc thp nht


hoc trong gii hn m nh phn phi cng b.

6. Phng php th
6.1 nh tnh
Phosphat

Trung ho vi ml dung dch acid phosphoric v thm dung


dch acid nitric long (TS). Sau cho thm ng th tch

dung dch nhm molybdat (TS) v lm m hn hp. S xut


hin kt ta mu mu hong yn, ta ny tan trong dung
dch amoniac long (TS).
6.2. tinh khit
Cc nitrat

Pha long 3,48 g mu th bng nc ct n 10 ml v cho


thm 5 mg natri clorid, 0,1ml dung dch indigo carmin (TS)
v 10 ml dung dch acid sulfuric. Trong vng 5 pht, mu
xanh da tri s khng bin mt hon ton.

Cc acid d bay hi

Pha long 60,05 g mu th vi 75 ml nc un si


ngui trong bnh chng ct c by hi, ct ly 50 ml dch
ct. Thm dung dch phenolphtalein (TS) vo dch ct ri
chun vi dung dch natri hydroxyd 0,1 N. Th tch dung
dch natri hydroxyd 0,1 N dng trung ho khng c
qu 0,1 ml.

Clorid

Cn 1,78 g mu th, tin hnh th theo hng dn phn


th gii hn clor, s dng 1,0 ml dung dch acid hydrocloric
0,01 N lm mu chng.

Sulfat

Cn 1,25 g mu th, mu th phi ph hp vi cc yu


cu nu trong chuyn lun th gii hn sulfat.

Arsen

Dung dch gm 1,5 g mu th trong 35 ml nc ct phi


ph hp vi cc yu cu nu trong chuyn lun th gii
hn arsen (phng php II), s dng hn hp gm 3 ml
dung dch arsen chun (3 g As) v 1,5 g dung dch acid
phosphoric (TS) lm mu chng. (th theo hng dn ti
JECFA monograph 1 - Vol.4).

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 1,00 g mu th cho vo bnh thu tinh nt mi, pha
long vi 100 ml nc ct, thm 0,5 ml dung dch
thymolphtalein (TS) v chun bng dung dch natri
hydroxyd 1 N.
Mi ml dung dch natri hydroxyd 1N tng ng vi 0,049
g H3PO4.

Ph lc 18
YU CU K THUT V PHNG PHP TH
I VI mono-NATRI ortho-PHOSPHAT
1. Tn khc, ch s

Mononatri orthophosphat; Sodium dihydrogen phosphate;


Monobasic sodium phosphate; Monosodium
monophosphate; Sodium acid phosphate; Sodium
biphosphate.
INS 339i
MTDI=70mg/kg th trng tnh theo Phospho t cc ngun
thc phm.

2. nh ngha
Tn ha hc

Natri dihydrogen phosphat; mono-natri hydrogen orthophosphat; mono-natri dihydrogen mono-phosphat;

M s C.A.S.

7558-80-7

Cng thc ha hc

Dng khan: NaH2PO4


Dng monohydrat: NaH2PO4.H2O
Dng dihydrat: NaH2PO4.2H2O

Khi lng phn t

Dng khan: 119,98


Dng monohydrat: 138,00
Dng dihydrat: 156,01
Dng bt d tan, tinh th hoc dng ht, khng mi mu
trng.
Cht iu chnh acid, cht to phc kim loi

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

D tan trong nc, khng tan trong ethanol, ether hoc


cloroform.

pH

4,2 - 4,6 (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 ortho-phosphat (m t


trong phn Phng php th).

5.2. tinh khit


Gim khi lng khi sy
kh

Dng khan: Khng c qu 2,0% (60 oC trong 1 gi, sau


105 oC trong 4 gi)
Dng monohydrat: Khng c qu 15,0% (60 oC trong 1
gi, sau 105 oC trong 4 gi)
Dng dihydrat: Khng c qu 25,0% (60 oC trong 1 gi,
sau 105 oC trong 4 gi)

Acid t do v dinatri

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

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 NaH2PO4 Khng c thp hn 97,0% sau khi sy kh


6. Phng php th
6.1 nh tnh
orthophosphat

Thm dung dch bc nitrat (TS) vo dung dch mu th 1%;


trong dung dch phi xut hin kt ta mu vng, ta ny
tan trong dung dch acid nitric long (TS).

6.2 tinh khit


Acid t do v dinatri

trung ha dch th (gm 2 g mu th trong 40 ml nc


ct), s dng khng qu 0,3 ml dung dch natri hydroxyd 1
N hoc dung dch acid sulfuric 1 N, s dng ch th l dung
dch da cam methyl (TS).

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
Cn 0,7 g mu th sy kh, chnh xc n mg, cho vo
cc 250 ml, thm 50 ml dung dch acid hydrocloric 0,1 N v
khuy u n khi mu tan ht. Cho in cc ca pH k
thch hp vo dung dch v dng buret cho t t dung dch
natri hydroxyd 0,1 N vo, va thm va khuy u, cho ti
khi pH = 3,3. Tip tc cho thm 0,5ml hoc 1 ml dung dch
natri hydroxyd (ty theo chia vch ca buret). Lp bng
d liu thc nghim theo mu:
V (ml)

pH

pH

2 pH

(1)

(2)

(3)

(4)

Trong :
V (ml): Th tch dung dch natri hydroxyd 0,1N c trn
buret.
pH: Hiu s chnh lch pH gia 2 ln thm dung dch
natri hydroxyd 0,1N lin tip.

2 pH: Hiu s chnh lch gia pH sau so vi gi tr


pH lin trc, du ca gi tr 2 pH c th dng hoc m
ty thuc gi tr pH sau ln hn (hoc nh hn) so vi
gi tr pH lin trc.
im tng ng ca qu trnh chun c xc nh
ti bc thm 0,5 ml natri hydroxyd 0,1N cho gi tr pH
ln nht. Xc nh gi tr chnh xc ca im tng ng
= gi tr th tch cn trn ca bc thm th tch natri
hydroxyd 0,1N c im tng ng + 0,5 b/B
Trong :
- b l gi tr 2 pH cui cng mang du (+).
- B l tng tr tuyt i ca 2 pH cui cng mang du (+)
v 2 pH u tin mang du (-).
Xc nh 2 im tng ng ca qu trnh chun ti
gia pH 3,3 v pH 6 (k hiu l F); gia pH 8,5 v pH 10
(k hiu l T). Th tch dung dch natri hydroxyd 0,1N dng
trong chun l gi tr F - T. Mi ml dung dch natri
hydroxyd 0,1N tng ng vi 12,0 mg NaH2PO4.

Ph lc 19
YU CU K THUT V PHNG PHP TH
I VI TRINATRI ortho-PHOSPHAT
1. Tn khc, ch s

Trisodium phosphate; Tribasic sodium phosphate; Sodium


phosphate.
INS 339iii
MTDI=70mg/kg th trng tnh theo Phospho t cc ngun
thc phm

2. nh ngha
Tn ha hc

Trinatri orthophosphat; Trinatri phosphat; Trinatri


monophosphat

M s C.A.S.

7601-54-9

Cng thc ha hc

Dng khan: Na3PO4


Dng hydrat: Na3PO4.xH2O

Khi lng phn t

163,94 (dng khan)

3. Cm quan

Dng tinh th, ht hoc bt tinh th trng, khng mi; dng


hydrat sn c gm hemi v monohydrat, hexahydrat,
octahydrat,
decahydrat
v
dodecahydrat;
dng
dodecahydrat bao gm 1/4 mol dung dch natri hydroxyd.

4. Chc nng

Cht iu chnh acid, m, cht to phc kim loi, cht


n nh nh tng

5. Yu cu k thut
5.1. nh tnh
tan

D tan trong nc, khng tan trong ethanol.

pH

11,5-12,5 (dung dch 1/100).

Natri

Phi c phn ng c trng ca natri (m t trong phn


Phng php th).

Phosphat

Phi c phn ng c trng ca phosphat (m t trong


phn Phng php th).

Orthophosphat

Phi c phn ng c trng ca orthophosphat (m t


trong phn Phng php th).

5.2. tinh khit


Gim khi lng khi nung

Cc cht khng tan trong


nc

Dng khan: Khng c qu 2% (120 oC trong 2 gi, sau


800oC trong 30 pht)
Dng monohydrat: Khng c qu 11% (120 oC trong 2
gi, sau 800 oC trong 30 pht)
Dng dodecahydrat: 45 - 58% (120 oC trong 2 gi, sau
800 oC trong 30 pht)
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 10,0 mg/kg.

5.3. Hm lng Na3PO4

Dng khan, hemihydrat v monohydrat: khng thp hn


97,0% tnh theo ch phm khan.
Dng dodecahydrat: khng thp hn 92,0% tnh theo ch
phm sau khi nung.

6. Phng php th
6.1 nh tnh
Natri

Thm 1 ml dung dch acid acetic (TS) v 1 ml dung dch


km uranyl acetat (TS) vo 5 ml dung dch mu th (dung
dch 1/20). Trong hn hp dung dch phi xut hin kt ta
dng tinh th mu vng trong vng vi pht.

Phosphat

Thm 1 ml dung dch acid nitric c v 5 ml dung dch


nhm molybdat (TS) vo 5 ml dung dch mu th (dung
dch 1/100) v lm m. Trong dung dch phi xut hin kt
ta vng nht.

Orthophosphat

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


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

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.

6.3. nh lng
Cn mu, chnh xc n mg, khi lng mu tng
ng vi khong 5,5 6 g Na3PO4, ha tan vo 40 ml
nc ct trong cc 400 ml, thm 100 ml dung dch acid
hydrocloric 1N. Sc dng khng kh kh carbon dioxyd
qua dung dch, chnh cho dng kh to bt nh, thi gian
sc khong 30 pht ui ht carbon dioxyd, y nh
ming cc ngn nga mt dch trong khi sc kh. Ra
np v thnh cc bng nc ct v cho in cc ca pH
k thch hp vo dung dch. Chun dung dch bng
dung dch natri hydroxyd 1 N n im un ti pH ~ 4, tnh
th tch (A) acid hydrocloric 1 N tiu th. Bo v dung
dch trnh hp th carbon dioxyd t khng kh v tip tc
chun vi dung dch natri hydroxyd 1 N n im un
ti pH ~ 8,8. Tnh th tch dung dch (B) natri hydroxyd 1 N
tiu tn khi chun .

Nu (A) 2(B), mi ml natri hydroxyd 1 N trong th tch (B)


tng ng vi 163,9 mg Na3PO4.
Nu (A) < 2(B), mi ml natri hydroxyd 1 N trong hiu th
tch (A)-(B) tng ng vi 163,9 mg Na3PO4.

Ph lc 20
YU CU K THUT V PHNG PHP TH
I VI DICALCI ortho-PHOSPHAT
1. Tn khc, ch s

Calcium mono hydrogen phosphate; Dibasic calcium


phosphate; Dicalcium phosphate,
INS 341ii
MTDI=70mg/kg th trng tnh theo Phospho t cc ngun
thc phm

2. nh ngha
Tn ha hc

Calci monohydrophosphat, Calcium hydrogen


orthophosphat, Secondary calcium phosphat;

M s C.A.S.

Dng khan: 7757-93-9

Cng thc ha hc

Dng khan: CaHPO4


Dng dihydrat: CaHPO4.2H2O

Khi lng phn t

Dng khan: 136,06


Dng dihydrat: 172,09

3. Cm quan

Dng tinh th hoc ht, bt mu trng.

4. Chc nng

Cht iu chnh acid, thc n cho men.

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.

Phosphat

Phi c phn ng c trng ca phosphat.

5.2. tinh khit


Gim khi lng khi sy
kh

Dng khan: Khng c qu 2% (200 oC, trong 3 gi)


Dng dihydrat: Khng thp hn 18% v khng c qu
22% (200 oC trong 3 gi)

Florid

Khng c qu 50,0 mg/kg.

Arsen

Khng c qu 3,0 mg/kg.

Ch

Khng c qu 4,0 mg/kg (Xc nh bng k thut hp


th nguyn t thch hp cho hm lng quy nh).

5.3. Hm lng CaHPO4

Khng c thp hn 98,0% v khng c qu 102,0%


tnh theo ch phm sau khi sy kh.

6. Phng php th
6.1. nh lng

Cn 0,3 g (chnh xc n mg) mu th c sy kh


trong 3 gi 200o, ho tan trong 10 ml dung dch acid
hydrocloric (TS). Thm 120 ml nc v vi git dung dch

da cam methyl (TS) v un si trong 5 pht, duy tr lin tc


th tch v pH ca dung dch trong qu trnh un si bng
cch cho thm dung dch acid hydrocloric hoc nc nu
cn thit. Thm 2 git dung dch methyl (TS) v 30 ml
dung dch amoni oxalat (TS), sau thm tng git (va
thm va khuy) hn hp ng th tch dung dch amoniac
6 N v nc n khi dung dch bt u c mu hng.
hn hp trong b cch thy nc si trong 30 pht, lm
ngui ti nhit phng v ch kt ta lng xung, lc b
phn dch qua phu lc thy tinh xp, ht chn khng nh
nu cn. Ra ta trong cc vi khong 30 ml dung dch ra
lnh (di 20o), c pha bng cch ly 10 ml dung dch
amoni oxalat (TS) pha long vi nc n 1000 ml.
kt tu lng xung, gn phn dch pha trn qua phu lc,
lm nh vy thm 3 ln. Dng dch ra, chuyn ton b
phn kt ta vo phu lc, ra cc v thnh phu bng
nc lnh (di 20o) 2 ln X 10 ml. t phu lc thy tinh
xp ln trn cc, thm 100 ml nc v 50 ml dung dch
acid sulfuric long lnh (1 trong 6). Dng buret cho 35 ml
kali permanganat 0,1N vo dung dch. Khuy u n khi
dung dch mt mu. un nng n khong 70o v chun
tip bng dung dch kali permanganat 0,1N.
Mi ml dung dch kali permanganat 0,1N tng ng vi
6,803 mg CaHPO4.

Ph lc 21
YU CU K THUT V PHNG PHP TH I VI CALCI MALAT
1. Tn khc, ch s

Calcium dl-Malate; Monocalcium dl-malate


INS 352ii
ADI Khng gii hn

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

Monocalcium dl-malat Mui monocalci ca acid 2hydroxybutandioic.


17482-42-7

Cng thc phn t

C4H4CaO5

Cng thc cu to

O
2+

HO

Ca
O

Khi lng phn t

172,14

3. Cm quan

Bt trng hoc khng mu

4. Chc nng

Cht iu chnh acid, m

5. Yu cu k thut
5.1. nh tnh
tan

t tan trong nc, khng tan trong ethanol.

Malat

Phi c phn ng c trng ca malat.

Calci

Phi c phn ng c trng ca calci.

5.2. tinh khit


Gim khi lng khi lm
kh

Khng c qu 2,0%.
(Sy ti 110oC trong 3 gi).

Florid

Khng c qu 30,0 mg/kg (phng php I hoc III).

Acid maleic

Khng c qu 0,05%.

Ch

Khng c qu 2,0 mg/kg. (Xc nh bng k thut


AAS/ICP-AES thch hp cho hm lng quy nh).

5.3. Hm lng
C4H4CaO5

Khng c thp hn 97,5%

6. Phng php th
6.1. nh lng

Cn khong 0,4 g (chnh xc n mg) mu th c


sy kh ti 110o trong 3 gi, ha tan trong hn hp gm 10

ml nc v 2 ml dung dch acid hydrocloric long (TS), sau


pha long bng nc n 100 ml. Khuy u bng
my khuy t, trong khi khuy, dng buret 50 ml 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 hydroxynaphtol v tip tc chun
n khi dung dch c mu xanh da tri.
Mi ml dung dinatri ethylendiamintetraacetat 0,05 M tng
ng vi 8,607 mg C4H4CaO5.

Ph lc 22
YU CU K THUT V PHNG PHP TH I VI NATRI FUMARAT
1. Tn khc, ch s

Monosodium fumarate,
INS 365
ADI khng gii hn

2. nh ngha
Tn ha hc

Mononatri fumarat, acid mononatri trans-butendioic,


mononatri trans-1,2-ethylendicarboxylat; acid mononatri
trans-1,2-ethylendicarboxylic

M s C.A.S.

7704-73-6

Cng thc ha hc

C4H3NaO4

Cng thc cu to

Khi lng phn t

138,06

3. Cm quan

Bt tinh th trng, khng mi.

4. Chc nng

Tc nhn m, cht iu chnh acid, cht tr hng.

5. Yu cu k thut
5.1. nh tnh
tan

Tan trong nc.

pH

3 - 4 (dung dch 1 trong 30).

Acid 1,2 dicarboxylic

Phi c phn ng c trng ca acid 1,2 dicarboxylic (m


t trong phn Phng php th).

Lin kt i

Phi c phn ng c trng ca lin kt i (m t trong


phn Phng php th).

Natri

Phi c phn ng c trng ca natri.

5.2. tinh khit


Gim khi lng khi sy
kh

Khng c qu 0,5%.( 120 oC, trong 4 gi).

Sulfat

Khng c qu 0,01%.

Acid maleic

Khng c qu 0,05%.

Ch

Khng c qu 2,0 mg/kg (Xc nh bng k thut hp


th nguyn t thch hp cho hm lng quy nh)

5.3. Hm lng C4H3NaO4 Khng c thp hn 98,0% v khng c qu 102,0%


tnh theo ch phm kh.

6. Phng php th
6.1 nh tnh
Acid 1,2 dicarboxylic

Ly 50 mg mu th vo trong ng nghim, thm 2-3mg


resorcinol v 1 ml acid sulfuric, lc u, un nng 130oC
trong 5 pht v ngui. Pha long vi nc ct cho 5
ml v nh tng git dung dch natri hydroxyd (2 trong 5)
kim ha dung dch, ngui v pha long vi nc ct
n 10 ml. Khi soi di n t ngoi dung dch c hunh
quang xanh lam nh lc.

Lin kt i

Thm 10 ml nc ct vo 0,5 g mu th, un si ha


tan. Thm 2 hoc 3 git dung dch brom (TS) vo dung dch
nng. Mu ca dung dch brom s mt.

6.2 tinh khit


Sulfat

Thm 30 ml nc ct vo 1 g mu, lc u, thm 1 git


dung dch phenolphtalein (TS), thm tng git dung dch
amoniac (TS) n khi dung dch c mu hng nht. Thm 1
ml dung dch acid hydrocloric long (TS). Tin hnh th
theo hng dn trong chuyn lun Th gii hn tp cht.
Dung dch ny tng ng vi khng qu 0,2 ml acid
sulfuric 0,01 N.

6.3. nh lng
Cn 0,3 g chnh xc n mg, mu th c lm kh,
ha tan trong 30 ml nc ct. Chun vi dung dch natri
hydroxyd 0,1N, s dng ch th l 2 git dung dch
phenolphtalein (TS).
Mi ml dung dch natri hydroxyd 0,1N tng ng vi 13,81
mg C4H3NaO4.

Ph lc 23
YU CU K THUT V PHNG PHP TH I VI MAGNESI CARBONAT
1. Tn khc, ch s

Magnesium carbonate
INS 504(i)
ADI Khng gii hn

2. nh ngha

L dng magnesi carbonat hydrat kim hoc magnesi


carbonat hydrat, hoc l hn hp ca 2 dng trn.

Tn ha hc

Magnesi carbonat

M s C.A.S.

546-93-0

Cng thc ha hc

MgCO3

Khi lng phn t


3. Cm quan

Khi mu trng sng, khng mi, d v hoc bt trng

4. Chc nng

Cht chng ng vn, khng ty trng, cht iu chnh


acid

5. Yu cu k thut
5.1. nh tnh
tan

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

Magnesi

Phi c phn ng c trng ca magnesi.

Carbonat

Phi c phn ng c trng ca carbonat.

5.2. tinh khit


Cc cht khng tan trong
acid

Khng c qu 0,05%.

Cc cht tan trong nc

Khng c qu 1,0%.

Calci

Khng c qu 0,4%.

Ch

Khng c qu 2,0 mg/kg (Xc nh bng k thut hp


th nguyn t thch hp vi hm lng qui nh).

5.3. Hm lng Mg

Khng c thp hn 24,0% v khng c qu 26,4%

6. Phng php th
6.1 tinh khit
Cc cht khng tan trong
acid

Cn 5 g mu th, chnh xc n mg, trn ln vi 75 ml


nc. Thm tng phn nh acid hydroclorid, va cho va
khuy n khi mu th khng ho tan thm c na, un
si trong 5 pht. Nu cn cn khng tan, tin hnh lc, ri
ra cn bng nc n khi sch clorid. Nung cn,
ngui, cn v tnh kt qu (%).

Cc cht tan trong nc

Cn 2 g mu th, chnh xc n mg. Thm 100 ml nc


mi un si ngui. un si hn hp, va un va
khuy, sau ngui v lc. Ly 50 ml dch lc em c
cn trn bp cch thu, sau sy cn 120o trong 3 gi.
ngui, cn v tnh hm lng % (Khi lng cn thu
c khng c qu 10mg).

Calci

Cn 1 g mu th, chnh xc n 0,1 mg, ho tan trong hn


hp 3ml acid sulfuric v 22 ml nc. Thm 5 ml ethanol v
hn hp qua m. Nu tinh th magnesi sulfat hnh
thnh, un nng hn hp ti khong 50 oC ho tan. Lc
kt ta bng phu lc s c nung kh v cn b. Ra
kt ta vi ln bng hn hp ethanol v dung dch acid
sulfuric long (TS) theo t l 2:1 (tt:tt). Nung phu lc s
trong ngn la , ngui v cn. Khi lng calci sulfat
thu c, nhn vi h s 0,294 c gi tr tng ng
vi lng calci trong mu th.

6.2. nh lng
Cn 1 g mu th, chnh xc n 0,1 mg, chuyn vo bnh
nn 250ml. Thm 50 ml acid sulfuric 1N, khuy cho tan
mu. Chun acid d bng dung dch natri hydroxyd 1N
dng ch th l dung dch da cam methyl (TS). Hiu gia th
tch acid sulfuric 1 N tiu tn tr i lng acid sulfuric 1 N
tng ng vi lng Ca c trong mu (20,04 mg Ca tng
ng vi 1 ml acid sulfuric 1 N) chnh l th tch acid sulfuric
1N tiu tn trung ha magnesi carbonat.
Mi ml acid sulfuric 1 N tng ng vi 12,16 mg Mg.

Ph lc 24
YU CU K THUT V PHNG PHP TH I VI NHM KALI SULFAT
1. Tn khc, ch s

Aluminium potassium sulfate; Potassium alum; Potashalum;


Burnt alum (khan)
INS 522 (dng dodecahydrat)
PTWI = 1 mg/kg th trng

2. nh ngha
Tn ha hc

Nhm kali sulfat dodecahydrat; Nhm kali sulfat khan.

M s C.A.S.

Dng khan: 10043-67-1


Dng dodecahydrat: 7784-24-9

Cng thc ha hc

AlK(SO4)2.xH2O (x = 0 hoc 12)

Khi lng phn t

Dng khan: 258,21


Dng dodecahydrat: 474,38

3. Cm quan

Tinh th ln, trong sut, hoc mnh tinh th, hoc bt tinh
th khng mi.

4. Chc nng

Cht iu chnh acid, lm rn chc, cht to xp.

5. Yu cu k thut
5.1. nh tnh
tan

D tan trong nc, khng tan trong ethanol.

pH

Dung dch mu th 10% c pH trong khong 3,0 - 4,0.

Nhm

Phi c phn ng c trng ca nhm.

Kali

Phi c phn ng c trng ca kali.

Sulfat

Phi c phn ng c trng ca sulfat.

5.2. tinh khit


Cc mui amoni

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. (Phng php II, cn 0,2 g


mu).

Ch

Khng c qu 5,0 mg/kg


(Xc nh bng k thut hp th nguyn t thch hp cho
hm lng quy nh).

5.3. Hm lng AlK(SO4)2 Dng khan: Khng thp hn 96,5%.


Dng dodecahydrat: Khng thp hn 99,5%.

6. Phng php th
6.1. tinh khit
Cc mui amoni

un nng 1 g mu vi 10 ml dung dch natri hydroxyd (TS)


trn b cch thy nc si trong 1 pht. Khng nhn thy
c mi amoniac.

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 c trong a platin v x l theo hng dn trong
phn "Tin hnh th" bt u t giai on "Nung trong thi
gian ngn ti 600oC ...".
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 600o, 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 vo 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...".
6.2. nh lng
a) Dng Dodecahydrat
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, 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 c mu
hng nht. 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 23,72 mg AlK(SO4)2.12H2O.
b) Dng khan
Cn khong 0,8 g (chnh xc n mg) bt mu th nhm
kali sulfat c sy kh trc ti 200o trong 4 gi.
Thm 50 ml nc, ha tan bng cch un nng trong b
cch thy v lc u, lc v ra k phn khng tan bng
nc. Gp dch ra v dch lc, thm nc n 200 ml.
Ly 25 ml dung dch ny, thm 50 ml dung dch EDTA 0,01
M, un si. Lm mt, thm 7 ml dung dch natri acetat 14%
v 85 ml cn tuyt i. Chun EDTA d bng dung dch
km sulfat 0,01 M vi ch th l 3 git dung dch da cam
xylenol (TS) n khi dung dch chuyn t mu vng sang
mu .
Mi ml dung dch EDTA 0,01 M tng ng vi 2,5821
mg AlK(SO4)2.

Ph lc 25
YU CU K THUT V PHNG PHP TH I VI NATRI HYDROXYD
1. Tn khc, ch s

Sodium hydroxyde; xt n da; kim; natri hydrat


INS 524
ADI=khng gii hn

2. nh ngha
Tn ha hc

Natri hydroxyd

M s C.A.S.

1310-73-2

Cng thc ha hc

NaOH

Khi lng phn t

40,00

3. Cm quan

Dng vin, vy, hnh que, khi d chy mu trng, trng


ng hoc cc dng khc.

4. Chc nng

Cht iu chnh acid.

5. Yu cu k thut
5.1. nh tnh
tan

Rt d tan trong nc; d tan trong ethanol.

Kim

Dung dch mu th 1 trong 100 c phn ng kim mnh.

Natri

Phi c phn ng c trng ca natri.

5.2. tinh khit


Cc hp cht khng tan
trong nc

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

Carbonat

Khng c qu 3,0% tnh theo natri carbonat.


Mi ml dung dch acid sulfuric 1 N dng chun dung
dch t im tng ng nhn bit bng ch th
phenolphtalein n im tng ng nhn bit bng ch
th da cam methyl (m t trong phn nh lng) tng
ng vi 106 mg Na2CO3.

Ch

Khng c qu 2,0 mg/kg (Xc nh bng k thut hp


th nguyn t thch hp cho hm lng quy nh).

5.3. Hm lng NaOH

Khng c thp hn 95,0% tng lng kim tnh theo


NaOH.

6. Phng php th
6.1 tinh khit
Cc hp cht khng tan
trong nc

Ho tan hon ton 1 g mu th trong 20 ml nc ct s


to thnh mt dung dch trong v khng mu.

6.2. nh lng
Cn 1,5 g mu th, chnh xc n mg, ho tan trong 40 ml
nc va mi un si ngui, lm ngui n 150C, cho
thm dung dch phenolphtalein (TS) v chun vi dung
dch acid sulfuric 1N. Khi dung dch mt mu hng, ghi li
th tch acid nu cn, cho thm dung dch da cam methyl
(TS) v tip tc chun cho n khi c mu hng. Ghi
chp li tng th tch dung dch acid chun .
Mi ml dung dch acid sulfuric 0,1 N tng ng vi 40,0
mg tng lng kim, tnh theo NaOH.

Ph lc 26
YU CU K THUT V PHNG PHP TH I VI KALI HYDROXYD
1. Tn khc, ch s

Potassium hydroxyde; potash n da; kali hydrat


INS 525
ADI=khng gii hn

2. nh ngha
Tn ha hc

Kali hydroxyd

M s C.A.S.

1310-58-3

Cng thc ha hc

KOH

Khi lng phn t

56,11

3. Cm quan

Dng vin, vy, hnh que, khi d chy mu trng, trng


ng hoc cc dng khc.

4. Chc nng

Cht iu chnh acid.

5. Yu cu k thut
5.1. nh tnh
tan

Rt d tan trong nc; d tan trong ethanol.

Kim

Dung dch mu th 1 trong 100 c phn ng kim mnh.

Kali

Phi c phn ng c trng ca kali.

5.2. tinh khit


Cc hp cht khng tan
trong nc

Ho tan hon ton 1 g mu th trong 20 ml nc ct s to


thnh mt dung dch trong v khng mu.

Carbonat

Khng c qu 3,5% tnh theo kali carbonat.


Mi ml dung dch acid sulfuric 1 N dng chun dung
dch t im tng ng nhn bit bng ch th
phenolphtalein n im tng ng nhn bit bng ch
th da cam methyl (m t trong phn nh lng) tng
ng vi 138,2 mg K2CO3

Ch

Khng c qu 2,0 mg/kg (Xc nh bng k thut hp


th nguyn t thch hp cho hm lng quy nh).

5.3. Hm lng KOH

Khng c thp hn 85,0% tng lng kim tnh theo


KOH.

6. Phng php th
6.1. nh lng

Cn 1,5 g mu th, chnh xc n mg, ho tan trong 40 ml


nc va mi un si ngui, lm ngui n 15 0C, cho
thm dung dch phenolphtalein (TS) v chun vi dung
dch acid sulfuric 1N. Khi dung dch mt mu hng, ghi li

th tch acid nu cn, cho thm dung dch da cam methyl


(TS) v tip tc chun cho n khi c mu hng. Ghi
chp li tng th tch dung dch acid chun
Mi ml dung dch acid sulfuric 0,1 N tng ng vi
56,11 mg tng lng kim, tnh theo KOH.

Ph lc 27
YU CU K THUT V PHNG PHP TH I VI CALCI HYDROXYD
1. Tn khc, ch s

Calcium hydroxyde; vi ti
INS 526
ADI=khng gii hn

2. nh ngha
Tn ha hc

Calci hydroxyd

M s C.A.S.

1305-62-0

Cng thc ha hc

Ca(OH)2

Khi lng phn t

74,09

3. Cm quan

Bt trng.

4. Chc nng

Cht iu chnh acid, tc nhn trung ha, m, cht lm


chc

5. Yu cu k thut
5.1. nh tnh
tan

Kh tan trong nc, khng tan trong ethanol, tan trong


glycerol.

Kim

Mu th c tnh kim vi giy qu t.

Calci

Phi c phn ng c trng ca calci.

5.2. tinh khit


Bari

Khng c qu 0,03%.

Magnesi v cc mui
kim

Khng c qu 6,0%.

Tro khng tan trong acid

Khng c qu 1,0%.

Florid

Khng c qu 50,0 mg/kg.

Ch

Khng c qu 2,0 mg/kg (Xc nh bng k thut hp


th nguyn t thch hp cho hm lng quy nh).

5.3. Hm lng Ca(OH)2

Khng c thp hn 92,0%

6. Phng php th
6.1 tinh khit
Bari

Trn 1,5 g mu th vi 10 ml nc ct, thm 15 ml acid


hydrocloric long (TS), pha long n 30 ml bng nc ct
v lc. Ly 20 ml dch lc, thm 2 g natri acetat, 1 ml acid
acetic long (TS) v 0,5 ml dung dch kali cromat (TS),
yn 15 pht. c ca dung dch ny khng c ln
hn c ca dung dch chng c pha bng cch ly

0,3 ml dung dch bari chun (1,779g bari clorid trong 1000
ml nc ct) thm nc ct cho 20 ml, thm 2 g natri
acetat, 1 ml acid acetic long (TS) v 0,5 ml dung dch kali
cromat (TS), yn 15 pht.
Magnesi v cc mui
kim

Ha tan 500 mg mu th vo hn hp gm 30 ml nc ct
v 10 ml acid hydrocloric long (TS) v un si trong 1
pht. Thm nhanh 40 ml dung dch acid oxalic (TS), khuy
mnh n khi kt tu hon ton. Thm ngay 2 git dung
dch methyl (TS), sau thm tng git dung dch
amoniac (TS) n khi hn hp va c tnh kim, ngui.
Chuyn dung dch vo ng ong 100 ml, pha long dung
dch n 100 ml bng nc ct, yn trong 4 gi hoc
qua m, sau lc gn phn nc trong pha trn qua
giy lc kh. Ly 50 ml dch lc trong vo mt bt platin,
thm 0,5 ml acid sulfuric v cho hn hp bay hi cch thy
n gn cn. Cho bay hi t t phn cn li trn ngn la
n kh, tip tc un cho n khi cc mui amoni phn hy
v bay hi hon ton. Cui cng nung phn cn cn li n
khi lng khng i. Khi lng cn khng c qu 15
mg.

Tro khng tan trong acid

Ha tan 2 g mu th trong 30 ml acid hydrocloric long (1


trong 3) v un si. Lc hn hp, ra bng nc nng v
nung. Khi lng cn cn li khng c qu 20 mg.

6.2. nh lng
Cn 1,5 g mu th, chnh xc n mg, cho vo cc thy
tinh, thm 30 ml acid hydrocloric long (TS). Khi mu tan
hon ton, chuyn dung dch vo bnh nh mc 500 ml,
trng sch cc thy tinh v gp nc ra cc vo bnh nh
mc, nh mc n vch bng nc ct, lc u. Ht ly
50 ml dung dch ny vo bnh nn c dung tch thch hp
v thm 50 ml nc ct, 15 ml ung dch natri hydroxyd
(TS), 40 mg hn hp ch th murexid (amoni purpurat) v 3
ml dung dch xanh lc naphtol (TS). 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 3,075 mg Ca(OH)2.

Ph lc 28
YU CU K THUT V PHNG PHP TH I VI CALCI OXYD
1. Tn khc, ch s

Calcium oxyde; vi
INS 529
ADI=0-6mg/kg th trng

2. nh ngha
Tn ha hc

Calci oxyd

M s C.A.S.

1305-78-8

Cng thc ha hc

CaO

Khi lng phn t

56,08

3. Cm quan

Dng ht, khi hoc bt khng mi, cng, mu trng n


trng xm nht.

4. Chc nng

Cht iu chnh acid, cht iu ho bt nho, thc n


cho men

5. Yu cu k thut
5.1. nh tnh
tan

Kh tan trong nc, khng tan trong ethanol, tan trong


glycerol. (ch : bo v mt khi thm nc vo mu th)

Phn ng vi nc

Tm t mu th vi nc, nhit c sinh ra. (ch : bo


v mt khi thm nc vo mu th).

Kim

Mu th c tnh kim vi giy qu t.

Calci

Phi c phn ng c trng ca calci.

5.2. tinh khit


Gim khi lng sau khi
nung

Khng c qu 10,0% (cn 1g, nung ti 8000C n khi


lng khng i)

Bari

Khng c qu 0,03%.

Magnesi v cc mui
kim

Khng c qu 3,6%.

Cht khng tan trong acid Khng c qu 1,0%.


Florid

Khng c qu 50,0 mg/kg (phng php I hoc III).

Ch

Khng c qu 2,0 mg/kg (Xc nh bng k thut hp


th nguyn t thch hp cho hm lng quy nh).

5.3. Hm lng CaO

Khng c thp hn 95,0% tnh theo ch phm sau nung.

6. Phng php th
6.1 tinh khit
Bari

Trn cn thn 1,5 g mu th vi 10 ml nc ct, thm 15


ml acid hydrocloric long (TS), pha long n 30 ml bng
nc ct v lc. Ly 20 ml dch lc, thm 2 g natri acetat, 1
ml dung dch acid acetic long (TS) v 0,5 ml dung dch
kali cromat (TS), yn 15 pht. c ca dung dch ny
khng c ln hn c ca dung dch chng c
chun b bng cch ly 0,3 ml dung dch bari chun (1,779
g bari clorid trong 1000 ml nc ct) thm nc ct cho
20 ml, thm 2 g natri acetat, 1 ml dung dch acid acetic
long (TS) v 0,5 ml dung dch kali cromat (TS), yn 15
pht.

Magnesi v cc mui
kim

Ha tan 500 mg mu th vo hn hp gm 30 ml nc ct
v 10 ml dung dch acid hydrocloric long (TS) v un si
trong 1 pht. Thm nhanh 40 ml dung dch acid oxalic
(TS), khuy mnh. Thm 2 git dung dch methyl (TS),
sau trung ha dung dch bng dung dch amoniac (TS)
n khi calci kt ta hon ton. un nng hn hp trn b
cch thy trong 1 gi, ngui, pha long n 100 ml
bng nc ct, trn u v lc. Ly 50 ml dch lc trong,
thm t t 0,5 ml acid sulfuric c v cho hn hp bay hi
n kh v nung n khi lng khng i trong chn nung
platin ( cn b).

Cht khng tan trong acid Ti 5 g mu, trn vi 100 ml nc ct v thm tng git
acid hydrocloric n va ho tan. un si hn hp,
ngui v thm acid hydrocloric (nu cn) to mi
trng acid, lc qua mt chn lc cn b, ra cn bng
nc ct n khi ht clorid. Sy 105 oC trong 1 gi,
ngui v cn.
6.2 nh lng
Nung 1 g mu th nhit ~800 oC n khi lng
khng i. Cn chnh xc lng cn v ha tan trong 20
ml dung dch acid hydrocloric long (TS). ngui dung
dch, pha long vi nc ct n 500 ml v trn u. Ht
ly 50 ml dung dch ny vo bnh nn c dung tch thch
hp v thm 50 ml nc ct, 15 ml dung dch natri
hydroxyd (TS), 40 mg hn hp ch th murexid v 3 ml
dung dch xanh lc naphtol (TS). 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 2,804 mg CaO.

Ph lc 29
YU CU K THUT V PHNG PHP TH
I VI NATRI NHM PHOSPHAT - ACID
1. Tn khc, ch s

Sodium aluminium phosphate, acidic; SALP


INS 541i
PTWI=1mg/kg th trng tnh theo nhm v cc mui nhm

2. nh ngha
Tn ha hc

Natri trialumini tetradecahydrogen octaphosphat tetrahydrat


hoc trinatri dialumini pentadecahydrogen octaphosphat

Cng thc ha hc

Na3Al2H15(PO4)8
NaAl3H14(PO4)8.4H2O

Khi lng phn t

Na3Al2H15(PO4)8 : 897,82
NaAl3H14(PO4)8.4H2O : 949,88

3. Cm quan

Bt mu trng, khng mi

4. Chc nng

Cht iu chnh acid, tc nhn lm n

5. Yu cu k thut
5.1. nh tnh
tan

Khng tan trong nc, tan trong acid hydrocloric.

pH

Acid i vi qu tm (th theo hng dn ti vol. 4).

Natri

Phi c phn ng c trng ca natri (Dch th l dung


dch mu th (1/10) trong acid hydrocloric long (1/2)).

Phosphat

Phi c phn ng c trng ca phosphat (Dch th l


dung dch mu th (1/10) trong acid hydrocloric long
(1/2)).

Nhm

Phi c phn ng c trng ca nhm (Dch th l dung


dch mu th (1/10) trong acid hydrocloric long (1/2)).

5.2. tinh khit


Gim khi lng khi sy
kh

Na3Al2H15(PO4)8: 19,5-21% (750-800 oC trong 2 gi)


NaAl3H14(PO4)8.4H2O: 15-16% (750-800 oC trong 2 gi)

Florid

Khng c qu 25,0 mg/kg.

Arsen

Khng c qu 3,0 mg/kg.

Ch

Khng c qu 2,0 mg/kg (Xc nh bng k thut hp


th nguyn t thch hp cho hm lng quy nh).
Na3Al2H15(PO4)8: Khng c thp hn 95,0%
NaAl3H14(PO4)8.4H2O: Khng c thp hn 95,0%

5.3. Hm lng

6. Phng php th
6.1. nh lng

Cn khong 2,5 g mu th c lm kh trc, chnh


xc n mg, cho vo bnh nh mc 250 ml. Thm 15 ml
acid hydrocloric v mt vin bi thy tinh, un nh trong
khong 5 pht. ngui v nh mc n vch bng nc
ct, lc u. Ly 10 ml, cho vo cc 250 ml, thm ch th l
dung dch phenolphtalein (TS) v trung ha bng dung dch
amoniac (TS). Thm dung dch acid hydrocloric long (1/2)
n khi ta va tan, sau pha long n 100 ml bng
nc ct v un n 70-80 oC. Thm 10 ml dung dch 8hydroxyquinolin (TS) v thm va dung dch amoni
acetat (TS) n khi to kt ta mu vng, sau thm d
30 ml. Gi hn hp ti 70 oC trong 30 pht. Lc hn hp
qua chn lc cn b, ra ta bng nc nng. Sy kh
ti 105 oC trong 2 gi v cn.
Mi mg ta thu c tng ng vi 0,689 mg
NaAl3H14(PO4)8.4H2O hoc 0,977 mg Na3Al2H15(PO4)8.

Ph lc 30
YU CU K THUT V PHNG PHP TH
I VI NATRI NHM PHOSPHAT KIM
1. Tn khc, ch s

Sodium aluminium phosphate, basic; Kasal


INS 541i
PTWI=1mg/kg th trng tnh theo nhm v cc mui nhm

2. nh ngha

L hn hp t nhin ca natri nhm phosphat kim (xp x


Na8Al2(OH)2(PO4)4) vi khong 30% dinatri hydrogen
phosphat

3. Cm quan

Bt mu trng, khng mi

4. Chc nng

Cht iu chnh acid, cht nh ha

5. Yu cu k thut
5.1. nh tnh
tan

Tan trong acid hydrocloric; phn natri phosphat tan trong


nc trong khi phn natri nhm phosphat t tan trong
nc.

Natri

Phi c phn ng c trng ca natri (Dch th l dung


dch mu th (1/10) trong acid hydrocloric long (1/2)).

Phosphat

Phi c phn ng c trng ca phosphat (Dch th l


dung dch mu th (1/10) trong acid hydrocloric long
(1/2)).

Nhm

Phi c phn ng c trng ca nhm (Dch th l dung


dch mu th (1/10) trong acid hydrocloric long (1/2)).

5.2. tinh khit


o
Gim khi lng khi nung Khng c qu 9,0% (750-800 C trong 2 gi).

Florid

Khng c qu 25,0 mg/kg.

Arsen

Khng c qu 3,0 mg/kg.

Ch

Khng c qu 4,0 mg/kg (Xc nh bng k thut hp


th nguyn t thch hp cho hm lng quy nh).

5.3. Hm lng Al2O3

Khng c thp hn 9,5% v khng c qu 12,5%


Al2O3, tnh theo ch phm sau khi nung.

6. Phng php th
6.1. nh lng

Cn khong 2,5 g mu th, chnh xc n mg, cho vo


bnh nh mc 250 ml. Thm 15 ml acid hydrocloric v mt
vin bi thy tinh, un nh trong khong 5 pht. ngui v
nh mc n vch bng nc ct, lc u. Ly 10 ml, cho
vo cc 250 ml, thm ch th l dung dch phenolphtalein
(TS) v trung ha bng dung dch amoniac (TS). Thm
dung dch acid hydrocloric long (1/2) n khi ta va

tan, sau pha long n 100 ml bng nc ct v un


n 70-80 oC. Thm 10 ml dung dch 8-hydroxyquinolin
(TS) v thm va dung dch amoni acetat (TS) n khi
to kt ta mu vng, sau thm d 30 ml. Gi hn hp
ti 70 oC trong 30 pht. Lc hn hp qua chn lc cn
b, ra ta bng nc nng. Sy kh ti 105 oC trong 2 gi
v cn.
Mi mg ta thu c tng ng vi 0,111 mg Al2O3.

Ph lc 31
YU CU K THUT V PHNG PHP TH
I VI GLUCONO delta-LACTON
1. Tn khc, ch s

2. nh ngha

Glucono-delta-lacton; Gluconolacton; GDL; Deltagluconolacton


INS 575
ADI "khng gii hn"
Glucono delta lacton l ester ni phn t 1,5- ca acid Dgluconic. Trong mi trng nc n b thy phn thnh
hn hp cn bng gm acid D-gluconic (55-66%); delta- v
gamma-lacton.

Tn ha hc

D-glucon-1,5-lacton; Acid D-gluconic delta-lacton

M s C.A.S.

90-80-2

Cng thc phn t

C6H10O6

Cng thc cu to

CH2OH
H

H
OH

OH

OH

Khi lng phn t

178,14

3. Cm quan

Tinh th hoc bt tinh th khng mi, mu trng hoc gn


nh khng mu.

4. Chc nng

Cht iu chnh acid, cht to phc kim loi, cht to xp

5. Yu cu k thut
5.1. nh tnh
tan

D tan trong nc khi un nh, t tan trong ethanol.

Phn ng mu

Ly 1 ml dung dch mu th 1/50, thm 1 git dung dch st


(III) clorid (TS), dung dch c mu vng m.

Gluconat

Phi c phn ng c trng ca gluconat

5.2. tinh khit


o
Gim khi lng khi lm kh Khng c qu 1,0%. (sy ti 105 C, trong 2 gi).

Tro sulfat

Khng c qu 0,1% (cn 2 g mu th, Phng php I).

Cc hp cht kh

Khng c qu 0,5% (tnh theo D-glucose).

Ch

Khng c qu 2,0 mg/kg


(Xc nh bng k thut hp th nguyn t thch hp cho
hm lng quy nh).

5.3. Hm lng C6H10O6

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

6. Phng php th
6.1. tinh khit
Cc hp cht kh

Cn khong 10 g (chnh xc n mg) mu th, cho vo 1


cc 400 ml, ha tan mu trong 40 ml nc, thm dung dch
phenolphtalein (TS) v trung ho bng dung dch natri
hydroxyd 1/2. Pha long bng nc n 50 ml, thm 50
ml dung dch ng (II) tartrat kim (TS). un nng hn hp
trn mt li aming t trn n t Bunsen, kim sot
ngn la dung dch si sau 4 pht v dung dch si
trong chnh xc 2 pht. Lc qua chn lc Gooch, ra bng
3 ml nc hoc chia lm nhiu ln. t chn lc nm nga
trong cc 400 ml ban u. Thm vo chn lc 5 ml nc v
3 ml acid nitric, dng a thy tinh khuy u ha tan
hon ton ng (I) oxyd, ra chn lc bng vi ml nc,
thu dch ra vo cc. Thm vo cc lng dung dch
brom (TS) (5 hoc 10 ml) n khi dung dch trong cc bt
u c mu vng, pha long bng nc n 75 ml,
thm vi vin bi thy tinh v un hn hp trn n Bunsen
n khi ui ht brom, lm mt. Thm t t amoni
hydroxyd n khi dung dch bt u c mu xanh da tri,
hiu chnh pH v 4 bng acid acetic bng v pha long
bng nc n 100 ml. Thm 4 g kali iodid v chun
vi dung dch natri thiosulfat 0,1 N, khi gn n im tng
ng thm ch th l dung dch h tinh bt (TS). Th tch
dung dch natri thiosulfat 0,1 N s dng khng c qu
16,1 ml.

6.2. nh lng

Cn khong 0,6 g (chnh xc n mg) mu th lm kh,


ha tan trong 50 ml dung dch natri hydroxyd 0,1 N, yn
trong 20 pht. Thm 3 git dung dch phenolphtalein (TS)
v chun lng natri hydroxyd d vi dung dch acid
sulfuric 0,1 N. Tin hnh lm mu trng song song.
Mi ml dung dch natri hydroxyd 0,1 N tng ng vi
17,81 mg C6H10O6.

Ph lc 32
YU CU K THUT V PHNG PHP TH I VI ACID ACETIC BNG
1. Tn khc, ch s

INS 260
ADI khng gii hn i vi acid acetic v mui kali v natri
ca acid acetic

2. nh ngha
Tn ha hc

Acid acetic, acid ethanoic

M s C.A.S.

64-19-7

Cng thc ha hc

C2H4O2

Cng thc cu to

H3C

OH
O

Khi lng phn t

60,05

3. Cm quan

Cht lng khng mu, c mi cay c trng.

4. Chc nng

Cht iu chnh acid, cht to hng.

5. Yu cu k thut
5.1. nh tnh
tan

C th trn ln vi nc, ethanol, glycerol v diethyl ether.

Acid

Dung dch mu th trong nc 1/3 c tnh acid

Acetat

Phi c phn ng c trng ca acetat. Th i vi dung


dch mu th trong nc 1/3.

5.2. tinh khit


im ng c

Khng c thp hn 15,6 oC

Cn khng bay hi

Khng c qu 0,01% sau khi bay hi 20 g mu th v gi


nhit 100 oC trong 2 h.

Cc cht d b xy ho

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

Ch

Khng c qu 0,5 mg/kg (Xc nh bng k thut hp th


nguyn t thch hp cho hm lng quy nh).

5.3. Hm lng C2H4O2 Khng c thp hn 99,5%


6. Phng php th
6.1 tinh khit
Cc cht d b oxy ho

Pha long 2 ml dung dch mu th trong mt bnh thu tinh


nt mi bng 10 ml nc ct, cho thm 0,1 ml dung dch kali
permanganat 0,1N. Trong 30 pht, mu hng ca dung dch
khng c chuyn sang mu nu.

6.2. nh lng

Ly 2 ml mu th, chuyn vo bnh thu tinh nt mi cn


b. Thm 40 ml nc ct v dung dch phenolphthalein (TS)
ri chun bng dung dch natri hydroxyd 1N. Mi ml dung
dch natri hydroxyd 1N tng ng vi 60,05 mg C2H4O2.

Ph lc 33
YU CU K THUT V PHNG PHP TH I VI ACID ADIPIC
1. Tn khc, ch s

INS 355
ADI = 0 - 5 mg/kg th trng

2. nh ngha
Tn ha hc

Acid hexandioic; Acid 1,4-butandicarboxylic

M s C.A.S.

124-04-9

Cng thc phn t

C6H10O4

Cng thc cu to

O
HO
OH
O

Khi lng phn t

146,14

3. Cm quan

Tinh th hoc bt tinh th trng, khng mi.

4. Chc nng

Cht iu chnh acid, hng liu

5. Yu cu k thut
5.1. nh tnh
tan

t tan trong nc, rt d tan trong ethanol.

Khong nng chy

151,5oC - 154oC.

5.2. tinh khit


Nc

Khng c qu 0,2% (Phng php Karl Fischer).

Tro sulfat
Ch

Khng c qu 20,0 mg/kg


Khng c qu 2,0 mg/kg
(Xc nh bng k thut hp th nguyn t thch hp cho
hm lng quy nh).

5.3. Hm lng C6H10O4

Khng thp hn 99,6 % v khng qu 101,0%

6. Phng php th
6.1 tinh khit
Tro sulfat

Cn 100 g mu th vo mt a platin 125 ml cn b v


c lm sch trc bng cch un chy trong a 5 g
kali pyrosulfat hoc bisulfat, tip theo un si dung dch
acid sulfuric long (TS) v trng bng nc. un chy mu
hon ton bng n kh sau nung. Sau khi bt u qu
trnh nung, iu chnh gim nhit trnh mu b si, v
gi nhit n nh mu b than ha hon ton. Sau
nung trong l nhit ti 850oC trong 30 pht hoc n khi
carbon hon ton chy ht. ngui v cn.

6.2. nh lng
Cn 3 g (chnh xc n mg) mu th, cho vo bnh nn
250 ml, thm 50 ml methanol v ha tan bng cch un
nng nh trong b cch thy, ngui v thm dung dch
phenolphtalein (TS) v chun vi natri hydroxyd 1N.
Tin hnh lm mu trng song song v hiu chnh kt qu
chun nu cn.
Mi ml dung dch natri hydroxyd 1N tng ng vi 73,07
mg C6H10O4.

Ph lc 34
YU CU K THUT V PHNG PHP TH
I VI MONOCALCI ortho-PHOSPHAT
1. Tn khc, ch s

Calcium dihydrogen phosphate; Monobasic calcium


phosphate; Monocalcium orthophosphate, Monocalcium
phosphate; Calcium biphosphate; Acid calcium phosphate;
INS 341i
MTDI=70 mg/kg th trng tnh theo Phospho t cc ngun
thc phm

2. nh ngha
Tn ha hc

Calci dihydrogen phosphat

M s C.A.S.

Dng khan: 7758-23-8


Dng monohydrat: 10031-30-8

Cng thc ha hc

Dng khan: Ca(H2PO4)2


Dng monohydrat: Ca(H2PO4)2.H2O

Khi lng phn t

Dng khan: 234,05


Dng monohydrat: 252,07

3. Cm quan

Dng tinh th hoc ht mu trng, d ht m hoc dng ht


mn.

4. Chc nng

Cht iu chnh acid, m, cht lm rn chc, cht to


phc kim loi, bt n, cht iu ho dng nho, cht to
kt cu, thc phm cho men v cht dinh dng

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 calci.

Phosphat

Phi c phn ng c trng ca phosphat.

5.2. tinh khit


Gim khi lng khi sy
kh

Dng monohydrat: Khng c qu 1,0% (60oC trong 3


gi).

o
Gim khi lng khi nung Dng khan: gia 14,0 v 15,5% (800 C trong 3 pht).

Florid

Khng c qu 50 mg/kg. (th theo hng dn ti JECFA


monograph 1 - Vol.4 Dng khan: tin hnh xc nh theo
Phng php II; Dng monohydrat: tin hnh xc nh theo
phng php IV.)

Arsen

Khng c qu 3,0 mg/kg.

Ch

Khng c qu 4,0 mg/kg.

5.3. Hm lng Ca

Dng khan: Khng c thp hn 16,8% v khng c


qu 18,3%.
Dng monohydrat: Khng c thp hn 15,9% v khng
c qu 17,7%.

6. Phng php th
6.1 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.

6.2. nh lng

Cn mu th (chnh xc n mg) khi lng tng ng


vi khong 475 mg mui khan, ho tan trong 10 ml dung
dch acid hydrocloric (TS). Thm vi git dung dch da cam
methyl (TS) v un si trong 5 pht, duy tr lin tc th tch
v pH ca dung dch trong qu trnh un si bng cch cho
thm dung dch acid hydrocloric hoc nc ct nu cn
thit. Thm 2 git dung dch methyl (TS) v 30 ml dung
dch amoni oxalat (TS), sau thm tng git (va thm
va khuy) hn hp ng th tch dung dch amoniac 6 N
v nc n khi dung dch bt u c mu hng.
hn hp trong b cch thy nc si trong 30 pht, lm
ngui ti nhit phng v ch kt ta lng xung, lc b
phn dch qua phu lc thy tinh xp, ht chn khng nh
nu cn. Ra ta trong cc vi khong 30 ml dung dch ra
lnh (di 20o), c pha bng cch ly 10 ml dung dch
amoni oxalat (TS) pha long vi nc n 1000 ml.
kt tu lng xung, gn phn dch pha trn qua phu lc,
lm nh vy 3 ln. Dng dch ra, chuyn ton b phn kt
ta vo phu lc, ra cc v thnh phu bng nc lnh
(di 20o) 2 ln, mi ln vi 10 ml. t phu lc thy tinh
xp ln trn cc, thm 100 ml nc v 50 ml dung dch
acid sulfuric long lnh (1 trong 6). Dng buret cho 35 ml
kali permanganat 0,1 N vo dung dch. Khuy u n khi
dung dch mt mu. un nng n khong 70o v chun
tip bng dung dch kali permanganat 0,1 N.
Mi ml dung dch kali permanganat 0,1 N tng ng vi
2,004 mg Ca.

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