Cng ho x hi ch ngha Vit Nam

Tiu chun Vit nam

hp rau qu
Phng php xc nh hm lng axit benzoic

TCVN 4714-89
ST SEV 4879-84

H Ni

TCVN 4714 - 1989

C quan bin son:

Trung tm nghin cu hp
Tng cng ty xut nhp khu rau qu
B Nng nghip v Cng nghip thc phm

C quan ngh ban hnh:

B Nng nghip v Cng nghip thc phm
C quan trnh duyt
Tng cc Tiu chun - o lng - Cht lng
U ban Khoa hc v K thut Nh nc
C quan xt duyt v ban hnh:
U ban Khoa hc v K thut Nh nc
Quyt nh ban hnh s 107/Q ngy 28 thng 02 nm 1989

Tiu chun Vit nam

hp rau qu
Phng php xc nh hm lng
axit benzoic
Canned fruits and vegetables. Determination of
benzoic acid content.

Nhm m
TCVN 4714-89
(ST SEV 4879-84)
C hiu lc t
01/01/1990

TCVN 4714 - 1989

iu 1 ca tiu chun ny ph hp vi ST SEV 4879-84.

1. Phng php so mu (phng php trng ti)

1.1. Ni dung phng php
Chit axit benzoic t mu bng ete etylic, nitro ho vi axit m-dinitrobenzoic,
kh ti axit m-diaminobenzoic. Dng hydroxylamin clorua to phc cht c mu,
o cng bc sng 532 nm.
1.2. Ly mu theo TCVN 4409-87. Chun b mu theo TCVN 4413-87.
1.3. Dng c, ho cht
My so mu quang in,
Cn phn tch chnh xc n 0,0001 g,
T sy,
Bp cch thu,
Bnh chit chia , dung tch 250 ml,
Bnh nh mc, dung tch 10 v 100 ml,
B ct,
Micro pipet chia , dung tch 2 ml,
Natri hydroxyt dung dch 4g/l v 40g/l,
Axit benzoic (C6H5COOH), dung dch tiu chun 1 mg/1ml:
Cn 100mg axit benzoic chnh xc n 0,0002 g, chuyn vo bnh nh
mc dung tch 100 ml, thm 25 ml NaOH 4g/l, thm nc n vch mc, lc
u.
Axit sunfuric c d = 1,84 v dung dch 25%,
Hn hp nitro ho: ho tan 25g KNO3 vo 250 ml HNO3 c.
Kali feroxyanua K4Fe (CN)6.3H2O dung dch 150 g/l (dung dch Care 1)
Km sunfat (ZnSO4. 7H2O) dung dch 300 g/l dung dch Care II,
Amonihydroxyt c d = 0,91,
Phenolphtalein 0,1%,
Hydroxylamin clorua 20g/l,
Ete etylic.
1.4 Tin hnh th
1.4.1. Xy dng ng chun
Dng micro pipet cho vo 5 ng nghim ln lt 0,6-0,8-1,0-1,2-1,4 ml dung dch
axit benzoic tiu chun, c kh cc dung dch trong ng nghim, trn ni cch

TCVN 4714 - 1989

thu, chuyn vo t sy, sy 105 oC trong 15 pht. Ly ra, lm ngui n
nhit phng.
Dng pipet cho vo mi ng nghim 1 ml dung dch nitro ho v un trn bp
cch thu si trong 30 pht (khuy u dung dch trong ng nghim trong 5
pht u tin). Ly cc ng nghim ra, ngm trong nc nhit 20oC trong
15 pht, thm vo mi ng nghim 10 ml NH 4OH (mi ln thm 0,5 ml cho n
ht 10 ml). yn trong 15 pht, thm 2 ml dung dch hydroxylamin clorua ri
t cc ng nghim vo bp cch thu 60 oC trong 5 pht. Lm ngui cc
ng nghim. dung dch t ng nghim vo cuvt dy 10 mm v o mt
quang bc sng 532 nm hoc vi knh lc mu xanh. Dung dch so snh
l dung dch c y cc ho cht tng ng nhng khng c axit benzoic.
V ng chun t trc tung l mt quang v trc honh l nng axit
benzzoic (mg/ml).
1.4.2. Tin hnh o mu
1.4.2.1. i vi mu dng lng
Ht 10 ml mu vo phu chit c chia , thm 2 ml H 2SO4 25% v 25 ml ete
etylic. Lc trong 5 pht, yn cho phn lp. Tch lp nc vo phu chit khc
v li chit mt ln na.
Gp cc phn ete vo mt phu chit khc, thm 2 ml NaOH 40 g/l v 1 git
phenolphtalein, lc trong 5 pht. Tch dung dch kim vo bnh mc dung
tch 10 ml. Chit 2 ln na, mi ln dng 2 ml NaOH 4 g/l trng bnh chit.
Gp dch kim chit c vo bnh mc trn, thm nc n vch mc, lc
u.
Ly 1 ml dch chit kim chuyn vo ng nghim v tin hnh o mu theo
iu 1.4.1
1.4.2.2. i vi mu dng rn, c
Cn 10g mu, chnh xc n 0,001 g, chuyn ton b vo bnh cu y
bng, trng cc cn v thnh bnh bng t nc ct. Kim ho dung dch bng
NaOH 40g/l vi ch th phenolphtalein. un hn hp trn bp cch thu si trong
30 pht, lm ngui, chuyn ton b sang bnh mc dung tch 100 ml, thm 2
ml dung dch Care 1 v v 2 ml dung dch Care II, khuy u, thm nc n
vch mc, lc u, lng, lc.
Ht 50 ml dch lc vo phu chit c chia , thm 5 ml dung dch axit
sunfuric, 50 ml ete etylic, lc trong 5 pht phn lp, chit phn ete sang
mt phu chit khc, tip tc chit tch mt ln na. Gp cc phn ete chit
li v tip tc tin hnh nh trong iu 1.4.2.1.

TCVN 4714 - 1989

1.5. Tnh kt qu
Hm lng axit benzoic trong mu lng (X1) tnh bng g/l theo cng thc:

n.V2
V1 .V3

Hm lng axit benzoic trong mu c (X2) tnh bng % theo cng thc:

n.V .V2
.10 1
m.V1 .V3

Trong :
n - Hm lng axit benzoic xc nh theo th chun, mg,
V - Th tch bnh mc ho long mu cn ban u, ml,
V1 - Th tch mu sn phm, ml,
V2 - Th tch bnh mc dch chit kim, ml,
V3 - Th tch dch chit kim ly xc nh, ml,
m - Khi lng mu cn, g.
Kt qu l trung bnh cng ca 2 ln xc nh song song tnh chnh xc n
0,001 g, chnh lch kt qu khng c ln hn 5% vi gi tr trung bnh.

2. Phng php chun

2.1 Ni dung phng php
Chit axit benzoic hoc natri benzoat t mu bng nc v t nc bng clorofooc,
sau chun bng kim.
2.2. Ly mu v chun b mu theo iu 1.2.
2.3 Dng c, ho cht
Bnh nh mc, dung tch 100, 250, 500 ml,
Phu chit c chia , 250 ml,
Bnh tam gic 100, 250 ml,
Km sunfat 30%,
Kali feroxyanua, dung dch 15%,
Axit clohydric 10%,
Natri hydroxyt 0,05 N v 10%,
Etanola 95%,
Clorofooc,
Phenolphtalein 0,1%.

TCVN 4714 - 1989

2.4 Tin hnh th
Cn 50 g mu chnh xc n 0,001 g, chuyn ton b vo bnh mc 250 ml,
dng NaOH 10% trung ho n trung tnh th bng giy o pH.
Thm 10 ml dung dch kali feroxyanua 15%, lc u thm 12 ml ZnSO 4 30%,
lc k, thm nc ct n vch mc, lc u, lng, lc.
Ht 50 ml dch lc, chuyn vo phu chit chia , trung ho bng HCl 10%,
th bng giy o pH, sau thm tip 5 ml HCl 10%.
Thm 30 ml clorofooc vo phu chit, lc trong 5 pht, phn lp, chit
phn dung dch nc sang mt phu chit khc, cho thm 15 ml clorofooc v
chit li 2 ln na.
Gp ton b clorofooc, c th cho vo b ct ct thu hi bt clorofooc
650C n cn li 1/4 th tch.
Chuyn phn cn cn li trong cc s v lm bc hi trn bp cch thu
50oC, ngui. Dng 50 ml etanola ho tan cn axit benzoic trong cc, thm 2
git phenolphtalein ri chun bng NaOH 0,05N.
2.5. Tnh kt qu
Hm lng axit benzoic hoc natri benzoat (X) tnh bng % theo cng thc:

V .K .V2 .100
m.V1

Trong :
V - th tch NaOH 0,05 N dng chun , ml,
V1 - th tch bnh nh mc pha mu, ml,
V2 - th tch dch lc mu ht chit, ml,
m - khi lng mu cn, g,
K - chun ca cht cn xc nh theo NaOH 0,05N vi
axit benzoic K = 0,0061 g
natri benzoat K = 0,0071 g.
Kt qu l trung bnh cng ca hai ln xc nh song song tnh chnh xc
n 0,001%. Chnh lch kt qu ca hai ln xc nh song song khng ln
hn 5% kt qu trung bnh.