TIU CHUN QUC GIA

TCVN 6122 : 2010

ISO 3961 : 2009
DU M NG VT V THC VT - XC NH TR S IT
Animal and vegetable fats and oils - Determination of iodine value
Li ni u
TCVN 6122 : 2010 thay th TCVN 6122 : 2007;
TCVN 6122 : 2010 hon ton tng ng vi ISO 3961 : 2009;
TCVN 6122 : 2010 do Ban k thut tiu chun quc gia TCVN/TC/F2 Du m ng vt v thc vt bin
son, Tng cc Tiu chun o lng Cht lng ngh, B Khoa hc v Cng ngh cng b.
DU M NG VT V THC VT - XC NH TR S IT
Animal and vegetable fats and oils - Determination of iodine value
1. Phm vi p dng
Tiu chun ny quy nh phng php xc nh tr s it (IV) ca du m ng vt v thc vt, sau y
gi l cht bo.
Ph lc A m t phng php tnh tr s it t cc d liu thnh phn axit bo. Phng php ny khng
p dng cho du c.
CH THCH Phng php trong Ph lc A da trn khuyn ngh thc hnh AOCS Cd 1c-85 [4].
2. Ti liu vin dn
Cc ti liu vin dn sau rt cn thit cho vic p dng tiu chun ny. i vi cc ti liu vin dn ghi
nm cng b th p dng phin bn c nu. i vi cc ti liu vin dn khng ghi nm cng b th p
dng phin bn mi nht, bao gm c cc sa i, b sung (nu c).
TCVN 6128 (ISO 661), Du m ng vt v thc vt - Chun b mu th.
TCVN 4851 (ISO 3696), Nc dng phn tch trong phng th nghim - Yu cu k thut v phng
php th.
3. Thut ng v nh ngha
Trong tiu chun ny s dng thut ng v nh ngha sau:
Tr s it (I V) [iodine value (IV)]
wi
Lng halogen tnh theo it, do phn mu th hp th chia cho khi lng phn mu th, iu kin
quy nh trong tiu chun ny.
CH THCH Tr s it c biu th bng s gam trn 100 g cht bo.
4. Nguyn tc
Ha tan phn mu th trong dung mi v cho thm thuc th Wijs. Sau mt thi gian quy nh, b sung
dung dch kali iodua v nc, chun it c gii phng bng dung dch natri thiosulfat.
CH THCH Ph lc A m t phng php tnh tr s it t cc d liu thnh phn axt bo. Tuy nhin,
phng php ny khng phi l phng php th nhanh. Phng php ny cho hai kt qu t cng mt
quy trnh phn tch. Phng php th tch mi l phng php chun.
5. Thuc th

Ch s dng cc thuc th loi tinh khit phn tch v s dng nc loi 3 ca TCVN 4851 (ISO 3696).
CNH BO - Ch v cc quy nh quc gia v x l cc cht c hi. Cn tun th cc bin
php an ton k thut, an ton i vi t chc v c nhn.
5.1 Dung dch kali iodua, nng khi lng p(Kl) = 100 g/l, khng cha iodat hoc it t do.
5.2 Dung dch h tinh bt: Trn 5 g tinh bt ha tan trong 30 ml nc, cho thm nc si vo dung dch
ny n 1 000 ml. un trong 3 min v sau ngui. Chun b dung dch h tinh bt mi trong ngy
lm vic.
5.3 Dung dch chun natri thiosulfat, dung dch chun c(Na2S2O3.5H2O) = 0,1 mol/l, c chun ha
khng qu 7 ngy trc khi s dng.
5.4 Dung mi, c chun b bng cch trn mt th tch xyclohexan vi mt th tch axit axetic bng
(50 ml + 50 ml).
5.5 Thuc th Wijs, cha it monoclorua trong axit axetic. T l I/Cl ca thuc th Wijs phi trong
khong 1,10 0,1.
C th s dng thuc th Wijs bn sn trn th trng. Phi ch tun th thi hn s dng ca thuc
th.
6. Thit b, dng c
S dng cc thit b, dng c ca phng th nghim thng thng v c th nh sau:
6.1 Tha cn bng thy tinh, ph hp vi phn mu th v cho c vo trong bnh (6.2).
6.2 Bnh nn, dung tch 500 ml, c nt thy tinh mi va kht v kh hon ton.
6.3 Cn phn tch, c chnh xc 0,001 g.
6.4 Bnh nh mc, dung tch 1000 ml, ph hp vi loi A ca TCVN 7153 (ISO 1042) [2].
6.5 Pipet, dung tch 25 ml loi t ng hoc ph hp vi loi A ca ISO 648 [1], c gn qu bp.
7. Ly mu
iu quan trng l mu gi n phng th nghim phi l mu i din v khng b h hng hoc thay
i trong sut qu trnh vn chuyn v bo qun.
Vic ly mu khng quy nh trong tiu chun ny, nn ly mu theo TCVN 2625 (ISO 5555) Du m
ng vt v thc vt - Ly mu [3].
8. Chun b mu th
Mu th c chun b theo TCVN 6128 (ISO 661).
9. Cch tin hnh
9.1 Mu th v chun b dung dch mu trng
9.1.1 Ty thuc vo tr s it d kin ca mu, cn vo tha cn thy tinh (6.1) cc lng mu th theo
Bng 1, chnh xc n 0,001 g.
Bng 1 - Khi lng phn mu th
Tr s it d kin

Khi lng phn mu th

Th tch ca dung mi

wi

g/100g

ml

wi < 1,5

15,00

25

1,5 wi < 2,5

10,00

25

2,5 wi < 5

3,00

20

5 wi < 20

1,00

20

20 wi < 50

0,40

20

50 wi < 100

0,20

20

100 wi< 150

0,13

20

150 wi < 200

0,10

20

CH THCH Lng mu phi ln, sao cho thuc th Wijs d t 50 % n 60 % so vi

lng c thm vo ngha l 100 % n 150 % lng c hp th.
9.2 Tin hnh xc nh
9.2.1 t tha thy tinh cha phn mu th vo bnh nn dung tch 500 ml (6.2) v thm mt lng dung
mi (5.4) nh trong Bng 1. Dng pipet (6.5) thm 25,00 ml thuc th Wijs (5.5). y np v lc bnh ri
bnh ni ti.
CH THCH Tha vn trong bnh.
CNH BO - Khng c dng pipet ht bng ming ht thuc th Wijs.
9.2.2 Chun b mu th trng vi lng dung mi v thuc th nh trong 9.2.1 nhng khng c mu th.
9.2.3 i vi mu c tr s it thp hn 150, th bnh ni ti trong 1 h.
i vi mu c tr s it cao hn 150 v cc sn phm polyme ha v du cha axit bo ni i lin hp
(v d: du tru, du thu du kh nc) v loi du bt k c cha axit bo dng keto (v d: mt s
loi du hi ly hydro ha) v sn phm oxy ha n mc ng k th bnh ni ti trong 2 h.
9.2.4 n cui thi im phn ng (9.2.3), cho thm 20 ml dung dch kali ioua (5.1) v 150 ml nc.
Chun bng dung dch chun natri thiosulfat (5.3) cho n khi gn nh mt ht mu vng ca it.
Thm mt vi git dung dch h tinh bt (5.2) v tip tc chun cho n khi lc mnh bnh th mt mu
xanh. Ghi li th tch dung dch natri thiosulfat, V2, dng n kt thc chun . C th xc nh im
kt thc bng chun in th.
9.2.5 Tin hnh ng thi php xc nh mu trng (9.2.2). Trong php th trng 9.2.4, ghi li th tch
dung dch natri thiosulfat, V1, dng n kt thc chun .
10. Tnh ton
Tr s it, wi, tnh bng gam trn 100 g cht bo, theo cng thc sau y:
wi =

12,69 c V1 V2
m

trong
c l nng ca dung dch chun natri thiosulfat (5.3) dng, tnh bng mol trn lt (mol/l);
V1 l th tch dung dch chun natri thiosulfat dng trong php th trng, tnh bng mililit (ml);
V2 l th tch dung dch chun natri thiosulfat dng trong php xc nh, tnh bng mililit (ml);
m l khi lng phn mu th, tnh bng gam (g).
Lm trn kt qu theo Bng 2.
Bng 2 - Lm trn kt qu
Tr s it
wi
g/100 g

Lm trn n

wi < 20

0,1

20 wi < 60

0,5

wi 60

11. chm
11.1 Yu cu chung
Cc gi tr a ra ny c th khng p dng c cc gii nng v cc cht nn khc vi cc gi tr
nu.
11.1 lp li
Chnh lch tuyt i gia hai kt qu th ring r thu c khi s dng cng mt phng php, trn
cng vt liu th, trong cng phng th nghim, do cng mt ngi thao tc trong cng mt khong thi
gian ngn, khng c ln hn gi tr r nu trong Bng 3.
11.2 ti lp
Chnh lch tuyt i gia hai kt qu th ring r thu c khi s dng cng mt phng php, trn
cng vt liu th, trong cc phng th nghim khc nhau, do nhng ngi thao tc khc nhau v trn
cc thit b khc nhau, khng c ln hn gi tr R nu trong Bng 3.
Bng 3 - Gii hn lp li v ti lp
Tr s it

Gii hn lp li

Gii hn ti lp

wi

wi < 20

0,2

0,7

20 wi < 50

1,3

3,0

50 wi < 100

2,0

3,0

100 wi < 135

3,5

5,0

g/100 g

12. Bo co th nghim
Bo co th nghim phi ghi r:
a) mi thng tin cn thit cho vic nhn bit y v mu th;
b) phng php ly mu, nu bit;
c) phng php th s dng v vin dn tiu chun ny;
d) mi chi tit thao tc khng c quy nh trong tiu chun ny hoc nhng iu c coi l ty cng
nh cc s c bt k m c nh hng n kt qu th.
e) kt qu th nhn c v cc n v o biu th kt qu hoc nu p ng yu cu v lp li, th
ghi kt qu cui cng thu c.
Ph lc A
(Tham kho)
Tr s it tnh c
A.1 Yu cu chung
Ph lc ny m t phng php tnh tr s it ca du thc phm t cc thnh phn axit bo xc nh
c bng sc k kh cc metyl este ca cc axit bo. Phng php ny cng c th p dng cho cc

triglyxerit v cc axit bo t do v cc sn phm hydro ha ca chng. i vi cc loi du c hm

lng cht khng x phng ha ln hn 0,5 % (v d: du c) th khng cho kt qu chnh xc nn khng
th p dng c.
LU - Quy trnh xc nh tr s it ny khng phi l phng php th nhanh. Phng php
ny cho hai kt qu t mt php phn tch.
A.2 Cch tin hnh
A.2.1 Xc nh thnh phn axit bo ca du hoc ca hn hp axit bo.
A.2.2 Tnh tr s it i vi cc nhm thnh phn nh m t trong A.2.2.1 v A.2.2.2.
CH THCH Vic tnh ton cho s nh gi khng ng mc i vi cc vt liu c tr s it thp.
A.2.2.1 Triglyxerit
Tr s it ca cc triglyxerit, w1,1 tnh c theo cng thc sau:
w1,1 = (w16:1 x 0,950) + (w18:1 x 0,860) + (w18:2 x 1,732) + (w18:3 x 2,616) + (w20:1 x 0,785) + (w22:1 x 0,723)
A.2.2.2 Cc axit bo t do
Tr s it ca cc axit bo t do, w1,2 tnh c theo cng thc sau:
w1,2 = (w16:1 x 0,9976) + (w18:1 x 0,8986) + (w18:2 x 1,810) + (w18:3 x 2,735) + (w20:1 x 0,8175) + (w22:1 x
0,7497)
Trong :
w16:1 l phn trm khi lng axit hexadecenoic;
w18:1 l phn trm khi lng axit octadecenoic;
w18:2 l phn trm khi lng axit octadecadienoic;
w18:3 l phn trm khi lng axit octadecatrienoic;
w20:1 l phn trm khi lng axit eicosenoic;
w22:1 l phn trm khi lng axit docosenoic.
Cc tr s di trong dng nc:nene biu th s nguyn t cacbon trong phn t, nc, tip theo bng s cc
lin kt i, nene.
Cc tr s it tnh c bng php xc nh axit bo bng sc k kh ca cc vt liu lipid khng cha
triglyxerit, nh cc este ha tng phn ca glyxerol, sorbitol/sorbitan/isosorbit, polyoxyetylen
sorbitol/sorbitan/isosorbit hoc glyxerol, ch tnh c tr s it ca cc axit c s dng chun b
cc este khng tng phn. thu c tr s it thc ca cc este ha tng phn vi cc dch pha long
polyol axit khng bo, th cn s dng phng php xc nh tr s it s dng thuc th Wijs clo ha.
Cc tr s it ca cc este ha tng phn theo phng php Wijs thp hn cc tr s thu c bng sc
k kh v vic pha long c nh hng n polyol.
TH MC TI LIU THAM KHO
[1] TCVN 7151: 2002 (ISO 648: 1977), Dng c th nghim bng thy tinh. Pipet mt mc.
[2] TCVN 7153: 2002 (ISO 1042: 1998) Dng c th nghim bng thy tinh. Bnh nh mc.
[3] TCVN 2625: 2007 (ISO 5555: 2001) Du m ng vt v thc vt - Ly mu.
[4] AOCS Recommended Practices Cd 1c-85, Iodine value calculated from GLC.