CNG HA X HI CH NGHA VIT NAM

QCVN 3-3 : 2010/BYT

QUY CHUN K THUT QUC GIA

V CC CHT C S DNG B SUNG ST
VO THC PHM
National technical regulation
on substances may be added for iron fortification in food

H NI - 2010

Li ni u
QCVN 3-3:2010/BYT do Ban son tho quy chun k
thut quc gia v Thc phm b sung vi cht dinh dng
bin son, Cc An ton v sinh thc phm trnh duyt v
c ban hnh theo Thng t s 16/2010/TT-BYT
ngy 20 thng 5 nm 2010 ca B trng B Y t.

QUY CHUN K THUT QUC GIA

V CC CHT C S DNG B SUNG ST VO
THC PHM
National technical regulation
on substances may be added for iron fortification in food

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 c s dng vi mc
ch b sung st vo 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 b sung st vo 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. Cc cht b sung st vo thc phm: l cc cht c ch ng cho vo
thc phm vi mc ch b sung st.
3.2. Dc in quc t 2006 (The International Pharmacopoeia, 4th edition,
WHO 2006): Dc in quc t do T chc Y t th gii xy dng v xut bn ln
th 4, nm 2006.
3.3. JECFA monograph 1 - Vol. 4: JECFA monographs 1 - Combined
compendium - 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.
3.4. M s C.A.S (Chemical Abstracts Service): M s ng k ha cht ca
Hip hi Ha cht Hoa K.
3.5. TS (test solution): Dung dch thuc th.
3.6. AsTS (Test solution of suitable purity for use in the limit tests for arsenic):
Dung dch thuc th c tinh khit thch hp th gii hn arsen.

QCVN 3-3 : 2010/BYT

3.7. PbR: (Reagent of suitable purity for use in the limit tests for lead): Thuc
th c tinh khit thch hp th gii hn ch.
3.8. PbTS: (Test solution of suitable purity for use in the limit tests for lead):
Dung dch thuc th c tinh khit thch hp th gii hn ch.
3.9. R (Reagent): thuc th
3.10. VS (Volumetric solution): Dung dch chun .
3.11. ADI (Acceptable daily intake): Lng n vo hng ngy chp nhn c.
3.12. INS (International numbering system): H thng m s quc t i vi
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 b sung st vo thc
phm 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 natri st (III)

ethylendiamintetraacetat, trihydrat.

1.2.

Ph lc 2

Yu cu k thut v phng php th i vi st gluconat.

1.3.

Ph lc 3

Yu cu k thut v phng php th i vi st (II)

sulfat.

1.4.

Ph lc 4

Yu cu k thut v phng php th i vi st fumarat .

2. 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. Tt c cc cht b sung st vo thc phm 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 b sung st vo thc phm
Vic kim tra cht lng, v sinh an ton i vi cc cht b sung st vo thc
phm phi c thc hin theo cc quy nh ca php lut.

QCVN 3-3 : 2010/BYT

IV. TRCH NHIM CA T CHC, C NHN
1. T chc, c nhn phi cng b hp quy ph hp vi cc yu cu k thut
ti Quy chun ny, ng k bn cng b hp quy ti Cc An ton v sinh thc phm
v bo m cht lng, v sinh an ton theo ng ni dung cng b.
2. T chc, c nhn ch c nhp khu, xut khu, sn xut, bun bn v s dng
cc cht b sung st vo thc phm 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 3-3 : 2010/BYT

Ph lc 1
YU CU K THUT V PHNG PHP TH I VI
NATRI ST (III) ETHYLENDIAMINTETRAACETAT, TRIHYDRAT
1. Tn khc, ch s

Ferric sodium edetate, Sodium iron EDTA, Sodium

feredetate

2. nh ngha
Tn ha hc

Natri [[N, N'-ethandiylbis[N-(carboxymethyl) glycinato]]

(4-)] ferrat (1-);
Natri [(ethylendinitrilo) tetraacetato] ferrat (1-);
Natri st (III) ethylendiamintetraacetat

M s C.A.S.

15708-41-5

Cng thc phn t

C10H12FeN2NaO8.3H2O

Cng thc cu to

OOC CH2

OOC CH2

CH2 COO
NCH2CH2N
CH2 COO

Na ,

3+

Fe

Khi lng phn t

Dng trihydrat: 421,09.

3. Cm quan

Ch phm c dng bt mu vng nht, tng i bn v

khng b bin i trong qu trnh bo qun.

4. Chc nng

Cht dinh dng b sung.

5. Yu cu k thut
5.1. nh tnh
tan

Tan trong nc.

St (III)

Phi c phn ng c trng ca st (III).

Natri

Phi c phn ng c trng ca natri.

5.2. tinh khit

pH

3,5 - 5,5 (dung dch 1 trong 100).

Cht khng tan trong

nc

Khng c qu 0,1%.

Acid nitrilotriacetic

Khng c qu 0,1%.

Ch

Khng c qu 1,0 mg/kg.

Arsen

Khng c qu 1,0 mg/kg.

5.3. Hm lng

Hm lng st khng c thp hn 12,5% v khng

c qu 13,5% tnh theo ch phm dng trihydrat.
Hm lng EDTA khng c thp hn 65,5% v
khng c qu 70,5% tnh theo ch phm dng
trihydrat.
4

QCVN 3-3 : 2010/BYT

6. Phng php th
Cc yu cu k thut c th theo hng dn trong JECFA monograph 1 - Vol. 4,
ngoi tr cc php th c hng dn ring trong ph lc ny ; c th s dng
cc phng php th khc tng ng.
6.1. tinh khit
Cht khng tan trong
nc

Cn 5 g mu th, cho vo 100 ml nc ct. Khuy u

n khi tan hon ton. t giy lc (c l ti a 1 m)
vo mt chn lc Gooch (3,5 - 4,0 cm). t chn lc vo
b ht chn khng, ra phu bng nc. Sy chn lc
ti 175oC trong 15 pht, ngui trong bnh ht m, cn
phu. Lc dung dch qua chn v ra 3 ln, mi ln vi
10 ml nc ct. Sy chn lc ti 110oC trong 1 gi.
ngui trong bnh ht m v cn phu. Tnh hm lng
cn (%).

Acid nitrilotriacetic

Pha ng: Thm 10 ml dung dch tetrabutylamoni

hydroxyd trong methanol (1 trong 4) vo 200 ml nc
ct, chnh pH v 7,5 0,1 bng acid phosphoric 1 M.
Chuyn hn hp vo bnh nh mc 1000 ml, thm 90
ml methanol, pha long bng nc ct n th tch,
lc u, lc qua mng (kch thc l lc 0,5 m hoc
mn hn), ui kh.
Dung dch mu trng amoni hydroxyd: Ly 0,5 ml amoni
hydroxyd, cho vo bnh nh mc 10 ml. Pha long bng
nc ct n th tch.
Dung dch chun gc: Cn chnh xc khong 100 mg
acid nitrilotriacetic cho vo bnh nh mc 100 ml, thm
0,5 ml amoni hydroxyd, lc u. Pha long n th
tch, lc u.
Pha chun: Cn 1,0 g mu, cho vo bnh nh mc 100
ml. Thm 100 l dung dch chun gc, pha long bng
nc ct n th tch, lc u. Rung siu m ha
tan ht, nu cn (dung dch A).
Pha mu th: Cn 1,0 g mu, cho vo bnh nh mc
100 ml. Thm 100 l dung dch mu trng amoni
hydroxyd, pha long bng nc ct n th tch, lc
u. Rung siu m ha tan ht, nu cn (Dung dch
B).
H sc k (Xem m t h thng HPLC trong chuyn lun
General Methods, JECFA monograph 1 - vol.4): H sc
k c ghp ni vi detector UV c th o c ti
bc sng 254 nm; Ct 4,6 mm 15 cm cha silica gn
vi octylsilan c ht 5 - 10 m (Ct Zorbax hoc tng
ng). Tc dng 2 ml/pht. Tin hnh chy sc k
dung dch A 3 ln, ghi li pic p ng theo hng dn
trong phn tin hnh th. lch chun tng i
khng c qu 2,0% v h s phn gii gia acid
nitrilotriacetic v natri st EDTA khng c thp hn
5

QCVN 3-3 : 2010/BYT

4,0.
Tin hnh th: Bm vo my sc k khong 50 L dung
dch A v dung dch B, ghi li sc k , o mc p
ng ca cc pic chnh. Thi gian lu i vi acid
nitrilotriacetic khong 3,5 pht v natri st EDTA khong
11,9 pht. Mc p ng ca pic acid nitrilotriacetic
trong sc k ca dung dch B khng c qu s
chnh lch gia mc p ng ca pic acid
nitrilotriacetic trong sc k ca dung dch A so vi
trong sc k ca dung dch B.
Ch

Xc nh bng k thut hp th nguyn t thch hp cho

hm lng qui 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.

Arsen

Th 3 g mu theo chuyn lun th gii hn Arsen,

phng php II trong JECFA monograph 1 - Vol. 4.

6.2. nh lng

- St
Cn khong 0,5 g mu (chnh xc n mg), ha tan
trong 40 ml nc ct trong bnh nn nt mi. Thm
khong 20 ml acid hydrocloric c, lc u, thm 3 g kali
iodid sau yn trong 5 pht. Chun iod c gii
phng bng dung dch natri thiosulfat 0,1 M ( chun
ha nng ), dng ch th l dung dch h tinh bt.
Trnh lc mnh trong qu trnh chun . Tin hnh lm
song song mu trng, khng c mu th.
% Fe = [(Ts - Tb) M 0,05585 100] / W
trong :
Tb l th tch dung dch natri thiosulfat mu trng (ml)
Ts l th tch dung dch natri thiosulfat mu th (ml)
0,05585 l trng lng phn t ca st 10-3
M l nng phn t gam chnh xc ca dung dch natri
thiosulfat
W l khi lng chnh xc ca mu th (g).
- EDTA
Ha cht, thuc th:
Dung dch calci acetat 0,25 M ( chun ha nng
): Cn 44,0 g calci acetat monohydrat (tinh khit thuc
th), cho vo bnh nh mc 1000 ml, thm nc ct
ha tan hon ton, pha long n th tch. Cn chnh
xc 3 phn 2,0 n 2,1 g EDTA (tinh khit thuc th)
(lng cn chnh xc l W EDTA), cho vo 3 bnh nn 250
ml, thm vo mi bnh 150 ml nc ct v iu chnh pH
v 11 12 (th bng giy o pH) bng dung dch natri
hydroxyd 50%.

QCVN 3-3 : 2010/BYT

Thm khong 30 mg ch th xanh hydroxynaphtol v
chun vi dung dch calci acetat n im tng
ng mu r, th tch dung dch calci acetat s
dng l V (ml).
Nng (M) = (W EDTA 1000) / (V 292,24)
Triethanolamin (tinh khit thuc th) ;
Ch th xanh hydroxynaphtol ;
Dung dch natri hydroxyd 50%;
Tin hnh th:
Cn chnh xc khong 0,8 - 1,0 g mu th (khi lng
cn chnh xc l ms, tnh bng g), cho vo cc 250 ml.
Thm 75 ml nc ct ha tan hon ton. Chnh pH
hn hp n 9,0 bng cch thm nh git
triethanolamin. Sau chnh pH v 12,5 - 13,0 bng
cch thm dung dch natri hydroxyd 50%. Dung dch phi
trong v khng mu. Thm khong 30 mg ch th xanh
hydroxynaphtol v chun bng dung dch calci acetat
(nng chnh xc xc nh trn, M) n im
tng ng c mu r. Th tch calci acetat s
dng l V1 (ml).
% EDTA = (V1

292,24) / (10

m s)

QCVN 3-3 : 2010/BYT

Ph lc 2
YU CU K THUT V PHNG PHP TH I VI ST (II) GLUCONAT
1. Tn khc, ch s

INS 579

2. nh ngha
Tn ha hc

St (II) D-gluconat dihydrat; St (II) gluconat

M s C.A.S.

299-29-6

Cng thc phn t

C12H22FeO14.2H2O

Cng thc cu to

OH OH H OH
HOCH2

COO

Fe2+

H H OH H
2

Khi lng phn t

482,17

3. Cm quan

Dng ht hoc bt mu xanh xm, hoc vng xanh; c

mi nh ging mi ng chy.

4. Chc nng

- Cht dinh dng b sung: B sung st.

- Ph gia thc phm: to mu, cht n nh.

5. Yu cu k thut
5.1. nh tnh
tan

Tan trong nc khi un nh, thc t khng tan trong

ethanol.

Mui st (II)

Phi c phn ng c trng ca mui st (II).

Gluconat

Phi c phn ng c trng ca gluconat.

5.2. tinh khit

Gim khi lng khi lm
kh

Khng thp hn 6,5% v khng c qu 10,0%. Sy

ti 105 oC trong 16 gi.

Cc ng kh

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

St (III)

Khng c qu 2,0%.

Ch

Khng c qu 2,0 mg/kg.

5.3. Hm lng

Khng thp hn 95,0% tnh theo ch phm lm kh.

6. Phng php th
Cc yu cu k thut c th theo hng dn trong JECFA monograph 1 - Vol.
4, ngoi tr cc php th c hng dn ring trong ph lc ny; c th s dng
cc phng php th khc tng ng.

QCVN 3-3 : 2010/BYT

6.1. tinh khit
Cc ng kh

Ha tan 0,5 g mu th trong 10 ml nc, lm m v

kim ha dung dch bng 1 ml dung dch amoniac (TS).
Sc kh hydro sulfid vo dung dch kt ta st v
yn trong 30 pht tu ng li. Lc v ra kt ta 2
ln, mi ln vi 5 ml nc. Gp dch ra v dch lc,
acid ha bng acid hydrocloric, thm d 2ml dung dch
acid hydrocloric long (TS). un si dung dch n khi
hi bay ra khng lm en giy tm ch acetat, tip tc
un si, nu cn, n khi th tch dch ch cn khong
10 ml. ngui, thm 5 ml dung dch natri carbonat
(TS) v 20 ml nc, lc v iu chnh th tch dch lc
v 100 ml. Ly 5 ml dch lc thm 2 ml dung dch
ng II tartrat kim (TS) v un si trong 1 pht. Sau 1
pht khng c xut hin kt ta mu .

St (III)

Cn 5 g (chnh xc n mg) mu th, ha tan trong

bnh 250 ml c nt mi cha sn hn hp gm 100 ml
nc v 10 ml acid hydrocloric. Thm 3 g kali iodid, lc
u v yn trong ch ti 5 pht. Chun iod c
gii phng vi dung dch natri thiosulfat 0,1 N, s dng
ch th l dung dch h tinh bt (TS).
Mi ml dung dch natri thiosulfat 0,1 N tng ng vi
5,585 mg st (III).

Ch

Xc nh bng k thut hp th nguyn t thch hp

cho hm lng qui 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 lm

kh, ha tan trong bnh 300 ml c nt mi cha sn
hn hp gm 75 ml nc v 15 ml dung dch acid
sulfuric long (TS), thm 250 g bt km. y bnh bng
nt gn vi van Bunsen, yn ti nhit phng
trong 20 pht, sau lc qua chn lc Gooch cha
giy lc x thy tinh ph mt lp mng bt km. Ra
chn lc v cn trong chn bng 10 ml dung dch acid
sulfuric long (TS), tip theo vi 10 ml nc. Thm
dung dch orthophenanthrolin (TS) v chun ngay
dch lc trong bnh vi dung dch ceri (IV) sulfat 0,1 N.
Tin hnh lm mu trng song song v hiu chnh kt
qu nu cn.
Mi ml dung dch ceri (IV) sulfat 0,1 N tng ng vi
44,61 mg C12H22FeO14.

QCVN 3-3 : 2010/BYT

Ph lc 3
YU CU K THUT V PHNG PHP TH I VI ST (II) SULFAT
1. nh ngha
Tn ha hc

St (II) sulfat heptahydrat

M s C.A.S.

7720-78-7

Cng thc phn t

FeSO4.7H2O

Khi lng phn t

278,02

2. Cm quan

C dng tinh th, bt tinh th hoc dng ht khng mi,

mu xanh nht.
Tinh th c th b mt nc trong iu kin khng kh
kh. Trong khng kh m d b oxi ha thnh st (III)
sulfat c mu vng nu.

3. Chc nng

Cht dinh dng b sung.

4. Yu cu k thut
4.1. nh tnh
tan

1 g mu th tan trong 1,5 ml nc 25 oC v 0,5 ml

nc si; Khng tan trong ethanol.

acid

Dung dch mu th 1 trong 10 phi c tnh acid khi th

vi qu.

St

Phi c phn ng c trng ca st.

Sulfat

Phi c phn ng c trng ca sulfat.

4.2. tinh khit

Ch

Khng c qu 2,0 mg/kg.

Thy ngn

Khng c qu 1,0 mg/kg.

4.3. Hm lng

Khng thp hn 99,5% v khng c qu 104,5%.

5. Phng php th
Cc yu cu k thut c th theo hng dn trong JECFA monograph 1 - Vol.
4, ngoi tr cc php th c hng dn ring trong ph lc ny; c th s dng
cc phng php th khc tng ng.
5.1. tinh khit
Ch

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 monograph1 - vol. 4,
phn cc phng php phn tch cng c.

10

QCVN 3-3 : 2010/BYT

Thy ngn

Dung dch chit Dithizon: Ha tan 30 mg Dithizon trong

1000 ml cloroform, thm 5 ml cn v lc u. Gi v
bo qun trong t lnh. Lc dung dch ny vi acid
nitric long (1 trong 100), lng acid ~1/2 lng dung
dch dithizon, tch lp v loi b lp acid, Dung dch
dithizon cn li c th s dng trong thi gian 1 thng.
Dung dch Dithizon long: Ch chun b ngay trc khi
s dng, ly 5 ml dung dch chit Dithizon pha long
vi 25 ml cloroform.
Dung dch Hydroxylamin hydroclorid: Ha tan 20 g
hydroxylamin hydroclorid trong nc c khong
65 ml dung dch. Cho dung dch ny vo phu chit,
thm vi git xanh thymol (TS), sau thm amoni
hydroxyd n khi dung dch c mu vng. Thm 10 ml
dung dch natri diethyldithiocarbamat (1 trong 25), lc
u v yn trong 5 pht. Chit dung dch nhiu ln,
mi ln vi khong 10-15 ml cloroform n khi ly 5 ml
dch chit cloroform th bng cch lc vi dung dch
ng sulfat long, lp cloroform khng c mu vng.
Thm dung dch acid hydrocloric 2,7 N n khi dch
chit c mu hng, thm 1 hoc 2 git xanh thymol
(TS), nu cn. Sau pha long n 100 ml bng
nc ct, lc u.
Dung dch thy ngn chun gc: Cn chnh xc 135,4
mg thy ngn (II) clorid, cho vo bnh nh mc 100 ml,
ha tan trong acid sulfuric 1 N. Pha long n th
tch bng acid sulfuric 1 N v lc u. Ly 5 ml dung
dch ny pha long n 500 ml bng acid sulfuric 1 N.
Mi ml dung dch ny cha tng ng 10 g Hg.
Dung dch thy ngn chun pha long: trong ngy s
dng, ly 10 ml dung dch thy ngn chun gc vo
bnh nh mc 100 ml, pha long n th tch bng
acid sulfuric 1 N, lc u. Mi ml dung dch ny cha
tng ng 1 g Hg.
Dung dch natri citrat: Ha tan 250 g natri citrat dihydrat
trong 1000 ml nc ct.
Dung dch mu th: Cn 3 g mu th, ho tan trong 30
ml acid nitric 1,7 N, un nng trn b cch thy nc
nng. Lm ngui v nhit phng trong b nc ,
khuy u v lc qua giy lc S No. 589 hoc tng
ng. Giy lc c ra trc bng acid nitric 1,7
N, sau trng bng nc ct. Thu dch lc v thm
vo 20 ml dung dch natri citrat v 1 ml dung dch
hydroxylamin hydroclorid.
Tin hnh th: Thao tc trong nh sng du. Pha dung
dch kim chng gm 3 ml dung dch thy ngn chun
pha long, 30 ml acid nitric 1,7 N v 5 ml natri citrat, 1
ml dung dch hydroxylamin hydroclorid. Dng pH k
chnh pH dung dch kim chng v dung dch mu th
v 1,8 bng dung dch amoni hydroxyd 6N, chuyn 2
11

QCVN 3-3 : 2010/BYT

dung dch vo 2 phu chit. Chit hai ln, mi ln vi 5
ml dung dch chit dithizon, tip theo chit vi 5 ml
cloroform. Loi b pha nc. Chuyn dch chit thu
c vo cc phu chit, gp dch chit dithizon v
dch chit cloroform, thm 10 ml acid hydrocloric long
(1 trong 2), lc u, tch lp v loi b lp
cloroform. Ra lp acid bng 3 ml cloroform, loi b
lp cloroform. Thm vo mi phu chit 0,1 ml dung
dch dinatri EDTA 0,05 M v 2 ml acid acetic 6 N, sau
thm t t 5 ml dung dch amoni hydroxyd. y nt
phu, lm mt di vi nc chy, lau kh thnh ngoi
ca phu. Qua ming phu, gn dung dch ra cc thy
tinh, ch trnh lm mt mu trong qu trnh gn.
Dng pH k chnh pH v 1,8 bng dung dch amoni
hydroxyd 6 N. Cho hn hp tr li phu chit, thm 5
ml dung dch dithizon long, lc u. Mu ca phu
mu th khng c m hn mu ca dung dch
trong phu kim chng.
5.2. nh lng

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

hp cha 25 ml acid sulfuric 2 N v 25 ml nc ct
mi un si, ngui. Thm dung dch
orthophenanthrolin TS v chun ngay vi dung dch
ceri sulfat 0,1 N. Tin hnh mu trng song song v
hiu chnh kt qu chun nu cn.
Mi ml ceri sulfat 0,1 N tng ng vi 27,80 mg
FeSO4.7H2O

12

QCVN 3-3 : 2010/BYT

Ph lc 4
YU CU K THUT V PHNG PHP TH I VI ST (II) FUMARAT
1. nh ngha
Tn ha hc

St (II) fumarat (1:1); St (2+) (E)-2-butendioat (1:1)

Ch s C.A.S.

141-01-5

Cng thc phn t

C4H2FeO4

Cng thc cu to

HC
O

CH O

Fe

Khi lng phn t

169,9

2. Cm quan

Dng bt mn mu nu hoc cam .

3. Chc nng

Cht b sung st

4. Yu cu k thut
4.1. nh tnh
tan

t tan trong nc, rt t tan trong ethanol (TS) (750 g/l).

Kt tu

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

Mui st (II)

Phi c phn ng trng ca mui st (II).

Hunh quang

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

4.2. tinh khit

Tng kim loi nng

Khng c qu 100,0 g/g.

Arsen

Khng c qu 5,0 g/g.

Ion st (III)

Khng c qu 20,0 mg/g.

Sulfat

Khng c qu 2,0 mg/g.

Gim khi lng khi sy

Khng c qu 10 mg/g. Sy ti 105 oC n khi lng

khng i.

4.3. Hm lng

Khng thp hn 93,0% v khng c qu 101,0%

C4H2FeO4 tnh theo ch phm sy kh.

5. Phng php th
Cc yu cu k thut c th theo hng dn trong Dc in quc t 2006,
ngoi tr cc php th c hng dn ring trong ph lc ny. c th s dng
cc phng php th khc tng ng.

13

QCVN 3-3 : 2010/BYT

5.1. nh tnh
Kt tu

Cn 0,4 g mu th, cho vo 10 ml acid hydrocloric 1 M

(VS), un nng tan hon ton, ngui (dch th).
Ly ring 1 ml dch th th phn ng mui st (II).
Thm vo phn dung dch cn li 15 ml natri hydroxyd 1
M (VS). Lc b kt ta sm mu. Thu phn dch lc v
thm 0,2 ml dung dch phenolphtalein/ethanol (TS) v
thm va acid hydrocloric 1 M (VS) n khi mt mu
hng. Ly 2 ml dung dch ny, thm 2 ml dung dch ng
(II) acetat 45 g/l (TS). Phi to kt ta tinh th mu trng.

Mui st (II)

S dng dch th c chun b trong php th kt ta.

Ly 1 ml dung dch th, thm dung dch kali fericyanid 10
g/l (TS), phi to kt ta xanh lam sm, kt tu ny
khng tan trong acid hydrocloric 70 g/l (TS).

Hunh quang

Cn 0,5 g mu, trn vi 1 g resorcinol (R). Chuyn 0,5 g

hn hp v chn nung, thm khong 0,15 ml acid
sulfuric ~1760 g/l (TS) v un nh, trong chn to thnh
khi bn na mu sm. Cho khi na rn ny vo
lng ln nc ct to thnh dung dch mu vng cam,
dung dch ny khng to hunh quang.

5.2. tinh khit

Tng kim loi nng

Cn 1,0 g mu. Nung nh n khi sch carbon, ha tan

tro trong 5 ml acid hydrocloric ~ 420 g/l (TS), un nh
trn b cch thy ha tan hon tan, cho bay hi n
kh. Ha tan cn trong hn hp gm 15 ml acid
hydrocloric ~ 420 g/l (TS), 4 ml acid nitric ~ 1000 g/l (TS)
v 6 ml nc ct, un nh trong 1 pht, chit loi st 3
ln, mi ln vi 20ml ether (R). Nu lp acid vn cn
mu vng th chit thm 1 ln na vi 20 ml ether (R),
loi b dch chit. un nh dung dch lai ht ether.
Thm 1 g acid citric (PbR), kim ha dung dch bng
dung dch amoniac ~100 g/l (PbTS), thm 1 ml kali
cyanid (PbTS) v pha long n 40 ml vi nc ct;
Tin hnh xc nh tng kim loi nng theo Dc in
quc t 2006 (chuyn lun 2.2.3 Th gii hn tng kim
loi nng, Phng php A).

Arsen

Cn 0,2 g mu trn vi 1,5 g natri carbonat khan (R),

thm 10 ml dung dch brom (AsTS) v trn u. Cho bay
hi n kh trn b cch thy, nung nh, ngui cn
cn li, ha tan cn trong 20 ml dung dch brom trong
acid hydrocloric (AsTS) v 10 ml nc. Chuyn hn hp
vo bnh thy tinh nh, thm va thic clorid (AsTS)
loi mu vng. Ni bnh thy tinh vi sinh hn v ct
ly 22 ml dch ct. Tin hnh th vi dch ct theo
hng dn trong Dc in quc t 2006 (chuyn lun
2.2.5 Th gii hn arsen).

14

QCVN 3-3 : 2010/BYT

Ion st (III)

Cn 3 g (chnh xc n mg) mu th, ha tan trong hn

hp gm 100 ml nc ct v 10 ml acid hydrocloric ~
420 g/l (TS), un si n khi tan hon ton. Lm mt
nhanh hn hp, thm 3 g kali iodid R, y nt bnh, lc
u v yn trong ch ti 15 pht. Chun iod c
gii phng vi dung dch natri thiosulfat 0,1 M (VS), s
dng ch th l dung dch h tinh bt (TS), thm ch th khi
gn n im tng ng. Tin hnh song song mu
trng khng c mu th, hiu chnh kt qu chun .
Mi ml dung dch natri thiosulfat 0,1 M (VS) tng
ng vi 5,585 mg ion st (III).

Sulfat

Cn 0,15 g mu th, cho vo 8 ml acid hydrocloric ~70

g/l (TS) v 20 ml nc ct, un si. Lm mt bng nc
, lc b cn. Ly dch lc v tin hnh th theo hng
dn trong Dc in quc t 2006, chuyn lun 2.2.2
Th gii hn sulfat.

5.3. nh lng

Cn khong 0,3 g (chnh xc n mg) mu th, ha tan

trong 7,5 ml acid sulfuric ~100 g/l (TS), un nh.
ngui, thm 25 ml nc ct, chun ngay vi dung
dch ceri amoni sulfat 0,1 M (VS), ch th l 0,1 ml ophenanthrolin (TS).
Mi ml dung dch ceri amoni sulfat 0,1 M (VS) tng
ng vi 16,99 mg C4H2FeO4.

15