PHN TH NHT

M U

1. Tnh cp thit ca ti
Hin nay, hu ht cc loi thc phm nh vt quay, gi ch, chim rn hay ht da, mt ko, thm ch c
nc gii kht... tt c nhng loi thc n ph bin ny u c nhum mu thc phm. t lu,
ngi ta c thi quen lm nh th, bi nhum mu thc phm khng ch lm cho thc phm thm p
mt, m cn khin thc khch c cm gic ngon ming hn.
Tuy nhin, khng phi tt c cc loi thc phm c nhum mu u gy hi cho sc khe. nhn
bit c s c hi ca phm mu trong thc phm th khng th kim tra c bng mt thng,
thm ch i vi nhng ngi lm vic lu nm trong cc Vin kim nghim an ton v sinh thc
phm. kim tra thc phm no c nhum bng phm mu t nhin, thc phm no c nhum
bng phm mu cng nghip, v cc cht ph gia no c tc hi n sc khe ngi s dng th cn
phi qua bc kim nghim cht ch ti Vin kim nghim an ton v sinh thc phm. TS.L Th Hng
Ho cho rng: V tc hi ca mu cng nghip i vi ngi s dng, nu dng thc n c nhum
phm mu cng nghip s b ng c, nhng tn d ca cc cht ny c th s lm cho ngi s dng
b ung th. Tc hi ca vic s dng phm mu cng nghip trong ch bin thc n l r rng v ai
cng bit. Tuy nhin, v li ch trc mt, vn c nhiu ngi lm dng cc loi phm mu
cng nghip, thm ch c nhng sn phm nm trong danh sch cc ph gia b cm.
Theo TS.Ho, nhng sn phm kh nhum mu th thng c nhum bng phm mu cng nghip.
Do , ngi dn cn c bit ch khi mua cc lot ht hoc thc phm kh nhum mu. c bit,
khi mua cn la chn nhng sn phm c nhn mc, hn s dng v c ghi ch v cht ph gia.
Trong tnh hnh vic tm kim phng php hu hiu xc nh hm lng phm mu
trong thc phm l vn ht sc quan trng. Trong khun kh tiu lun ti trnh by cch xc nh
Tartrazine trong thc phm bng phng php ph hp th phn t UV-VIS.
2. Mc tiu
Trong tnh hnh hin nay, khi cc nh sn xut v chy theo li nhun m s dng nhng phm
mu thc phm ha hc c hi hay qu lm dng phm mu gy nhng nh hng xu n sc
khe ca ngi tiu dng . V vy tiu lun ny ra mt phng php xc nh Tartrazine l phng
php ph hp th phn t UV-VIS.
3. Phng php nghin cu
Phng php nghin cu l thuyt v phng php chuyn gia.
4. i tng v phm vi nghin cu

- Tartrazine trong thc phm

- Phng php ph hp th phn t UV-VIS

PHN TH HAI

NI DUNG

CHNG 1

TNG QUAN

1.1.Gii thiu v phm mu thc phm.

Phm mu l tn ch chung cho cc hp cht hu c c mu ( gc thin nhin v tng hp), rt a dng
v mu sc v chng loi. Chng c kh nng nhum mu, ngha l bt mu hay gn mu trc tip ln
cc vt liu khc.
Phm mu thc phm l mt nhm nhng cht c mu c dng lm ph gia thc phm, to ra
hoc ci thin mu sc ca thc phm, nhm lm tng tnh hp dn ca sn phm. Nhng phm mu l
cht ch lm tng cm quan v hon ton khng c gi tr dinh dng g khi n vo.
Nhng thc n c cha phm mu trong danh mc cho php s dng lm ph gia thc phm ca b y
t, di mc gii hn d lng cho php th khng gy nh hng cho sc khe ca ngi tiu dng.
Tuy nhin nu qu lm dng phm mu, hoc chy theo li nhun, s dng cc phm mu ngoi danh
mc cho php s gy c hi cho sc khe.
* Phn loi
Cc phm mu c chia lm hai loi chnh
1.1.1.Phm mu t nhin
L cc cht c chit xut ra hay c ch bin t cc nguyn liu hu c ( thc vt, ng vt)
sn c trong t nhin.
V d caroten t nhin c chit xut t cc loi qu c mu vng, curcumin c chit xut t c
ngh, mu caramen c ch bin t ng...
Nhm phm mu c ngun gc t nhin c nhc im l bn km, s dng vi lng ln
nn gi thnh sn phm cao.
1.1.2. Phm mu tng hp ha hc
L cc phm mu c to ra bng cc phn ng tng hp ha hc.
V d Amaranth(), Brilliant blue ( xanh), tartazine ( vng chanh)...
Cc phm mu tng hp thng t bn mu cao, vi mt lng nh cho mu t vi yu cu
t ra, nhng chng c th gy ng c nu dng khng nguyn cht hay dng qu liu lng cho
php.
1.2. Gii thiu v Tartrazine[1]
1.2.1. Tn khc, ch s
CI Food Yellow 4, FD&C Yellow No. 5; S CI (1975): 19140

INS: 102
ADI = 0 - 7,5 mg/kg th trng.
1.2.2. nh ngha
Ch yu gm Trinatri 5-hydroxy-1-(4-sulfonphenyl)-4-(4-sulfonphenylazo)-H-pyrazol-3carboxylat v cc cht mu ph cng vi NaCl v (hoc) Na2SO4 l cc thnh phn khng mu chnh.
C th chuyn thnh cht mu nhm (aluminium lake) tng ng, trong trng hp ny p dng quy
nh chung i vi cc loi cht mu nhm.
Tartrazine thng c dng trong cc sn phm nng, ng cc v cc sn phm ng cc, cc sn
phm sa, c v cc sn phm thy sn, tht v cc sn phm gia cm, cc sn phm c s dng trng,
nc tri cy, rau qu v cc sn phm u, nc gii kht, cc sn phm mt, cc loi bnh ko, thc
ung c cn, cc sn phm mui chua, nc st, cc sn phm trang tr thc phm, kem, cc loi mn
ngt, gia v, c xng khi, cc loi bnh snack, cc loi mn hm.
1.2.3.Cu to ha hc
* Tn ha hc: Trinatri 5-hydroxy-1-(4-sulfonphenyl)-4-(4-sulfonphenylazo)-H-pyrazol-3-carboxylat
* M s C.A.S: 1934-21-0
* Cng thc ha hc: C16H9N4Na3O9S2
*

Cng thc cu to:

* Khi lng phn t: 534,37 ( thuc nhm mu azo)

1.2.4.Thnh phn
+Hp cht mang mu phi khng thp hn 85%
+ Hp cht ph mang mu: Khng qu 1%
+ Hp cht hu c khng mang mu: Khng qu 0.5% bao gm 4-Hydrazinobenzensulfonic acid, 4aminobenzensulfonic acid, 5-oxo-1(4-sulfophenyl)-2-pyrazoline-3-tetrahydroxysuccinic acid
+Amine thm cha b sulfo ho khng qu 0.01% tnh theo aniline
+ Cc cht c th trch ly bng ete: Khng qu 0.2%
+Hnh dng: Dng b hay dng ht c mu cam sng
+ Chc nng: To mu

+ Tnh tan: Tan c trong nc, tan t trong dung dch ethanol
+Tn tht khi sy 1350C: Khng qu 15%, vi chloride v sulfate tnh theo mui natri
+ Cht khng tan trong nc: Khng qu 0.2%
+ Quang ph hp thu: 426 nm
+ Ch: Khng qu 10 ppm
+ Arsen: Khng qu 3 ppm
+ Thu ngn: Khng qu 1 ppm
+ Cadmium: Khng qu 1ppm
+ Kim loi nng: Khng qu 40 ppm
1.2.5.Tnh cht
Tartrazine l cht mu bn, nhy vi nhng cht oxy ho mnh, d ht m. Tartrazin c s
dng ph bin trn khp th gii, bi v n l cht mu tng hp c gi thnh thp nht. Cc loi thc
phm c cha t l tartrazine khc nhau tu thuc vo nh sn xut hay gi thnh sn xut. Tuy nhin
ngy nay c xu hng hn ch s dng tartrazin v thay th bng nhng hp cht mu khng tng hp
nh annatto, mu malt, betacarotene.
Cht i khng vi Tartrazine l sulphur dioxide, acid ascorbic, sodium hydroxide v cc dung
dch kim khc.
Sn phm tartrazine thng mi dng bt, mu vng, ho tan tt trong nc. 1 lt nc 200C
c th ho tan c 150g tartrazine. Ngc li, tartrazine ho tan km trong cn. Mt lt ethanol ch
ho tan c 0.1g tartrazine. Trong mi trng kim, tartrazine s to nn mu .
Tartrazine gy ra cc phn ng d ng, c bit i vi nhng ngi khng s dng c thuc
aspirin. Theo FDA, tartrazine gy pht ban vi t l 0.01%. Tuy nhin, khng c nhng thng tin r
rng v mc ca nhng tc hi tartrazine vi tng c nhn c th. Nhiu nghin cu cn cho thy
tartrazine cn gy ra nhng ri lon, thay i tnh tnh ca tr em. Do , M yu cu phi cng b
cht mu ny trn cc sn phm thuc v thc phm v tng l mu cn phi c FDA cng nhn
trc khi em vo s dng. Tartrazine b cm s dng Na Uy, c v c. Hin nay, ngi ta ang
u tin s dng betacarotene to mu vng cho thc phm hu c v annatto cho thc phm v c)
Nh chng ta ghi nhn t trc, nhng nh hng ca vic s dng mu trong thc phm
c bit n t thi c i. Tuy nhin cc nghin cu mt cch c kim sot xem s tc ng ca
mu sc c nh hng n hng v v nh hng ln thc phm xem c c chp thun hay khng
th ch c tin hnh trong 70 nm qua. Hin nay, trong tnh hnh phm mu thc phm c s dng

trn lan, nn c nhng phng php thch hp xc nh mt s loi phm mu ph bin trong thc
phm. Trong tiu lun ny ti trnh by cch xc nh Tartrazine bng my UV-VIS.
1.3.Phng php ph hp th phn t UV-VIS
1.3.1. Tng quan[2]
Cc phn t iu kin bnh thng tn ti trng thi c bn bn vng c nng lng
thp.Khi chng c cung cp nng lng, v d nh c chm sng (photon) c nng lng thch hp
nm trong vng sng 190 - 800 nm chiu vo, phn t nhn nng lng, tr thnh trng thi kch thch.
Nng lng tng E(ts) ca chm sng m phn t nhn c cui cng bin thnh nhit nng
nhng c 3 dng chuyn ha:
E(ts) = E(e) + E(d) + E(q)
E(e) l dng chuyn mc cc electron: Trong phn t, cc in t tham gia vo lin kt trong cc lin
kt , , ngoi ra cn c cc i in t khng lin kt (n), s hp th nng lng ca chm sng v n
chuyn ln trng thi nng lng cao Em. Khi phn t cht b kch thch nh th, n c s chuyn mc
nng lng: * ; * ; n * hay n *
Ed v Eq: l nng lng quay v dao ng ca nguyn t trong phn t. N c hnh thnh khi phn
t ca cht nhn nng lng bi chm sng kch thch, tuy nhin do nng lng thp nn tc ng ca
n ch lm quay hoc dao ng cc nguyn t quanh v tr cn bng.
Sau khi cht hp th, ta o phn cn li ca chm sng chiu vo ban u to ra ph hp th
quang phn t ca cht. V th ph loi ny c gi l quang ph hp th phn t UV-VIS. Nh vy
ph hp th phn t UV-VIS l ph xut hin do s tng tc ca cc in t ha tr trong phn t hay
nhm phn t vi chm sng kch thch c bc sng nm trong vng UV-VIS.
*NH LUT BOUGHE - LAMBE BEER (nh lut Beer)
Chiu mt chm sng c bc sng xc nh i qua b lp dung dch. Do hp th, sau mi lp dung
dch, nh sng gim i n ln. Gi cng nh sng ban u l I o, sau khi i qua lp th nht l I1 ta
c: I1

In

I
Io
. Khi i qua lp th hai, nh sng gim i n 2 ln, ta c I 2 o2 , tip tc vi b lp ta c
n
n

Io
I
I hay o n b
b
I
n

Hnh 1.1
a)Cuvet cha dung dch hp th
quang
b) Hai cuvet cng cha mt lng
cht mu c quan st t trn xung

Ly logarit hai v, ta c: log

s, ta c:

Io
I
= b.log n = k b. i lng log o ta gi l hp th quang A, k l h
I
I

A= k.b

Ly hai lng cht mu bng nhau, cng loi, ha tan trong cuvet, c th quan st dung dch t trn
xung. cng loi, dung dch mt c chiu cao h1, dung dch 2 c chiu cao h2; h1>h2. Nh vy, nng
dung dch 1 nh hn dung dch 2, ta c: K C1b1 = K C2 b2
Tin hnh vi nng dung dch C1 nh hn C2n ln, tuy nhin s lp cht mu li tng n ln nn tch
s K.C.b khng i.
Khi thay dung dch th hai bng cht mu khc, sao cho hai dung dch 1 v 2 c cng nng , v s
lp cht mu, C1= C2 v b1= b2. Tuy nhin, lc ny K1 khc K2 cho nn hp th quang khc nhau, ta
c phng trnh:
K1C b K2 C b

(2.2)

Nh vy hp th quang ca mt cht mu ph thuc vo:

Bn cht ca cht mu vi h s K tng ng
Nng cht mu, C
Chiu dy lp hp th, b
Kt hp c (2.1) v (2.2), h s k trong 2.1 l hng s ph thuc c hai yu t: nng v bn cht ca
cht, ta c phng trnh:

A=bC

* TNH CHT CA H S HP TH PHN T,

Trong biu thc A = bC, nu C c biu din bng mol/l v b tnh bng cm th l h s hp th
phn t gam. Biu thc trn cho thy c gi tr bng A khi dung dch c nng bng 1M o vi
cuvt c b dy b = 1cm.
H s hp th phn t gam c trng cho bn cht hp th nh sng v khng ph thuc vo th
tch dung dch, b dy lp dung dch v ch ph thuc vo ca dng sng ti (I0). Do i lng

thng c coi l tiu chun khch quan quan trng nht nh gi nhy ca php nh lng
trc quang, =f().
Th nguyn ca :
=

Ta c:

A
bC

(2.4)

= b(cm).C(M/l) = l /cm-1M
* TNH CHT CA HP TH QUANG A V H QU
a) Ph hp th quang A ph thuc bc sng ca nh sng ti.
Chiu chm sng c bc sng khc nhau i qua dung dch hp th, hp th ca dung dch ph
thuc nhiu vo bc sng (thay i bc sng).
e
ema
x

l (n
m)

l ma
x

Hnh 1.2

Ph hp th quang ph
thuc bc sng
Chiu cc chm sng c bc sng thay i mt cch lin tc t bc sng di n bc sng ngn
hn (hoc ngc li), cn gi l qut ph, ta thu c ph hp th l nhng di lin tc, c nhng cc
i hp th, cc v tr max khc nhau tu thuc cht phn tch (hnh 2.1).
b) hp th quang A ph thuc nng cht
Lp dy chun cht hp th quang c nng khc nhau trong iu kin ph hp v chiu chm sng
c bc sng c nh ng vi cc i ca ph hp th cht mu qua dung dch, ta thu c mt dy s
liu v hp th quang ca cc dung dch, v vo th, ta thu c ng chun biu din s ph
thuc hp th quang vo nng cht, A=f(C).
A

Ax

Cx

Hnh2.2. ng chun biu din s ph thuc A vo nng C.

d) hp th quang A c tnh cht cng tnh
Nu dung dch c nhiu cht hp th, hp th quang ca dung dch mt bc sng nht nh l
tng cc hp th quang thnh phn (hnh 2.3):
A= 1C1b + 2 C2 b ++ nCnb

* Bit v Amax ring c th xc nh ng thi nng hai cht trong dd

Hai cht P v Q c hai cc i hp th ti hai bc sng 1max v 2max
o hp th quang ti hai bc sng trn, thu c hai i lng hp th A 1 v A2, trong A1 v A2
u l tng ca cc i lng hp th thnh phn ti mi bc sng
Th d 1.1: P v Q to phc vi thuc th X, to thnh PX v QX c hai cc i hp th 400nm v
500 nm, tng ng vi mi nguyn t nh sau:
400 nm

500 nm

ca phc PX

1.104 l /cm-1M1

1.103 l /cm-1M1

ca phc QX

1.103 l /cm-1M1

1.104 l /cm-1M1

Ho tan hon ton 0,10g mu, thm cht che v thuc th ri nh mc n 100 ml. o hp th
quang (A) hai bc sng 400 nm v 500 nm, c cc s liu sau:
A400 = 1.104 CP +

1.103 CQ = 0,500

(2.5)

A500 = 1.103 CP +

1.104 CQ = 0,300

(2.6)

Tnh hm lng P, Q trong mu bit MP = 65, MQ = 60.

Gii: Nhn hai v ca phng trnh (2.6) vi 10 ta c
1.104 CP + 1.103 CQ

0,500

1.104 CP + 10.104 CQ

3,00

Ly 2 tr 1 ta c 9,9.104CQ =

2.50

2,50

%Q =

Tnh c CQ = 9,9.10 4 =2,525.10-5M

%P =

CP = 4,75.10-5M/l

2,525.10 5.60.100.
0,00152%
1000 x0,1

4,75.10 5.65.100.
0,00308%
1000 x 0,1

*MI LIN H GIA TRUYN QUA T V HP TH A

I

1
truyn qua c nh ngha, T I ; A log
T
o

I
I

-logT = log.C.b

hay T 10 Cb

* Mi lin h gia hp th quang (A) v truyn qua (T)

Th d 1.2: Mt mu dung dch cha trong cuvet 1cm o truyn qua t 80% nh sng mt bc
sng nht nh. Nu hp th quang ca cht ny cng bc sng l 2,0 th nng cht l bao
nhiu.
Gii: truyn qua l 0,8 hay phn trm truyn qua t 80% nn T=0,8. Theo nh ngha: log T = .b.C hay log 1/T = .b.C, vy theo u bi ta c
Log 1/T = 2,0 cm-1mol-1 .l .1 cm.C
Log 1/0,8 = log 1,25 = 2 mol-1 l.C
C = 0,10/2,0 = 0,05M/l
* NHNG SAI LCH CA NH LUT BEER
- Nhng du hiu
hp th quang A l hm bc nht ca bc sng, nng C v chiu dy lp dung dch o b:
A = f(, C, b). Khi c nh iu kin o v bc sng, v chiu dy lp dung dch (thng o vi
cuvet 1cm) th A=f(C), y l s ph thuc tuyn tnh (hnh 2.2). Khi s ph thuc ny khng tuyn
tnh iu c ngha l c s sai lch. y l du hiu th nht v s sai lch khi nh lut Beer.
Du hiu th hai l ph hp th ca dung dch cht hp th quang nhng nng khc nhau phi c
cc i cng mt bc sng (cc iu kin khc nh pH, thnh phn dung ging nhau). Cc dung
dch c thnh phn ging nhau tr cht hp th quang c thnh phn khc nhau nhng cc i hp th
lch nhau th y cng l du hiu ca s khng tun theo nh lut Beer.
- Nhng nguyn nhn sai lch ca nh lut Beer
a) Do nh sng khng n sc
Khi nh sng khng n sc chiu qua cht hp th quang, c ngha dng sng ti c nhiu tia sng vi
cc bc sng khc nhau, cht phn tch ch hp th mt s tia sng nht nh, t l hp th khng

10

ng u. Khi tng nng cht phn tch, mt s tia sng c th b hp th hon ton trong khi
mt s tia sng vn b hp th t, thm ch khng hp th. Kt qu l thu c ng biu din khng
tng tuyn tnh v hp th quang theo nng (do cc tia sng khng b hp th c cng i ra
(I) khng gim khi tng nng )
b) Cht hp th quang c thnh phn thay i
1. Cht hp th quang khng bn, thnh phn thay i khi pha long dung dch
Gi l phn ly ca phc mu MX, phng trnh phn ly nh sau:
MX

(1-)C
[M][X]

K = [MX]

= 2C

Pha long n ln n =

1
K = 2C =
1
K
=
C/n

nK
C

Hnh2.4
S ph thuc ca sai lch S
vo t l

Hng s phn ly K l

; S = n 1 =

K
(cha pha long)
C

(2.7)

K
.( n 1)
C

K
C

K
C
sai lch S t l thun vi

K v

n , t l nghch vi

C .(hnh 2.4).

trnh s phn ly ca phc MX, nng thuc th X cao, n = 1, S =0.

nh hng ca ion H+ (pH) ti s hnh thnh phc mu.
a s cc thuc th dng trong phn tch ph hp th phn t l nhng mui ca axit hay baz:
M + HX

MX + H+

Khi tng hoc gim nng H+, u lm cn bng to MX thay i.

Trng hp pH cao, kim loi M c th b thu phn v kt ta, mt khc X trng thi X -, nh vy,
phc c th trang thi a phi t (th d phc Fe(III)- salixilic pH 1-3 hnh thnh phc 1:1 FeSal +
c mu tm, khi tng pH ln 4, mt na phc c 2 phi t, FeSal 2- c mu ; n pH 9, phc chuyn
sang dng 3 phi t, FeSal3 c mu vng).
Trng hp nng H+ cao, pH thp, HX tn ti nhiu, MX cng hnh thnh t.
Ngi phn tch cn chn ra pH ph hp cho vic hnh thnh phc mu va m bo phc MX hnh
thnh tt, chnh xc v lp li cao.

11

2. nh hng ca cc cu t l
a) Cc cu t l l cation
K hiu cu t l l ion kim loi M, n cng tc dng vi thuc th X to hp cht mu MX tng t
MX. Nh vy, hp cht ny cng hp th quang, lm sai lch kt qu o v pha dng. trnh hin
tng ny, phi chn thuc th X c hng s bn vi M cao hn vi M (hng s bn ln hn 10 4 ln
th khng nh hng). Trng hp thuc th l anion ca axit yu, cn s dng nng H + lm
phng tin che.
Th d 1.3 Tnh pH cn thit xc nh Fe 3+ bng phng php quang ph hp th phn t UV-VIS
vi thuc th axit salixilic (H2Sal) 10-2M khi c mt Cu2+. Cho hng s phn ly H2Sal l 10-16, hng s
phn ly ca Fe(Sal)2+ l 10-16, ca Cu(Sal) l 1.10-12.
2+

Gii: Phn ly ca Fe(Sal) l Fe(Sal) =Fe

2+

Cu(Sal)=Cu +Sal

2-

3+

[Fe 3 ][Sal 2 ]
+Sal ; KPL=
=10-16
[Fe(Sal) 2 ]
2-

[Cu 2 ][Sal 2 ]
; KPL=
=10-12
[Cu(Sal)]

Khi 99% Fe3+ to phc tc l

K Pl
[Fe 3 ]
1

=
[Sal2-] = 100KPL Khi Cu2+ to phc 1% tc l

[Fe(Sal) ] 100 [Sal 2 ]

[Cu 2 ]
100

[Cu(Sal)]
1

K' PL
K' PL
2T y rt ra KPL = 10-4KPL hay ni cch khc l 2 hng
2 [Sal ] =
[Sal ]
100

s phn ly phi hn nhau 104 ln v [Sal2-] =

K PL .K' PL

= 10-14 . Mt khc: H2Sal = 2H+ + Sal2- ; KPL

[H ] 2 [Sal 2 ]
10 16
=
[H 2 Sal]

b) Cu t l l anion
Khi c cc anion (A) phn ng vi kim loi M cn phn tch, n lm cho phc mu MX hnh thnh
khng hon ton, i khi nu nng anion l ln, bn th phc MX khng hnh thnh. loi tr nh
hng ca cc anion c 3 kh nng chnh:
+ Chn thuc th X to phc tt vi M (c th p dng c k thut che, pH) phc MA khng
hnh thnh.
+ Thm vo dung dch cht chun mt lng anion l tng ng. Trng hp ny nh hng ca
cu t l n cht phn tch v cht chun l nh nhau, kt qu o c so snh vi nng cht c
trong mu chun, t tnh ra nng ca n.
+ Tch loi cc anion trc khi cho thuc th X vo mu
1.3.2. Cc phng php nh lng

12

Ph hp th phn t da trn bc x UV-VIS l mt trong nhng cng c hu hiu phn tch

nh lng. Nhng c trng c bn ca phng php phn tch o quang l :
+ Kh nng p dng rng : Mt s rt ln cc cht hu c, v c, ha sinh hp thu c chm
sng trong vng t ngoi kh kin v nh vy c th phn tch nh lng trc tip chng. Nhiu hp
cht khng c kh nng hp th trc tip cng c kh nng p dng phng php ny sau khi chuyn
chng bng phng php ha hc thnh nhng dn xut c th hp th c. Ngi ta c lng rng
khong 90% cc phn tch trong phng th nghim bnh vin u da trn ph UV-VIS.
+ nhy cao : Gii hn d tm ca ph hp th phn t trong khong 10 -4 n 10-5M. Khong
ny c th c m rng n 10-6 thm ch n 10-7M vi nhng th tc b sung.
+ chn lc t trung bnh n cao : Nu mt bc sng c tm thy m cht phn tch ch
hp th mt mnh th khng cn phi thc hin php tch chng ra khi dung dch hn hp.
+ chnh xc cao : Sai s tng i v nng trong ph UV-VIS tiu biu nm trong
khong t 1% n 5%.
+ D thao tc v thc hin nhanh chng vi cc my hin i.
p dng vi nhng cht hp th trc tip : Bng lit k nhng nhm chc mang mu hu c. Vic xc
nh cc hp cht hu c cha mt trong nhng nhm chc ny l kh thi v c th tra cu trong cc
ti liu chuyn mn. Mt s cht v c cng hp th trc tip nh cc ion kim loi chuyn tip mang
mu trong dung dch nh Cu2+, Ni2+...hoc cc ion MnO4-, Cr2O72-...
p dng vi nhng cht khng hp th trc tip : i vi nhiu cht hay ion v d nh ion kim loi
khng hp thu trc tip hoc hp thu vi cng yu, ngi ta thm cc thuc th v c nh SCN cho trng hp Fe3+ hoc thuc th hu c vi lng d, thit lp mi trng thch hp chuyn
ton b cht hoc ion phn tch v dng phc c th hp th trc tip chm sng kh kin.

C x Cst
C

C x st .A x
A x A st
A st
Cx

Cst
.A x
A st

A x C x .tg
Cx

A Ax
A

C x x . C
C Cx
A

hx
tg

13

CHUN 1 IM

CHUN NHIU IM ( CHUN)

THM CHUN

1.3.3 Nguyn tc v trang thit b ca php o ph UV-VIS

1.3.3.1. Nguyn tc
Ph hp th phn t UV-VIS l ph hp th ca cht phn tch trng thi dung dch ng th
vi mt trong cc dung mi nh nc, methanol, benzen, aceton,... Nh vy cc bc o c th nh
sau:
+ Ha tan cht phn tch trong mt dung mi ph hp nu cht c ph hp th nhy trong
vng t ngoi kh kin ( v d cc cht hu c); hoc cho cht , thng l kim loi, tc dng vi mt
thuc th trong mt dung mi thch hp to ra mt hp cht c ph hp th UV-VIS nhy.
+ Chiu vo dung dch mu cha hp cht cn phn tch 1 chm sng c bc sng ph hp
cho cht phn tch hay sn phm ca n hp thu bc x to ra ph hp th UV-VIS ca n. V th
cht phn tch v dung mi cng c cha trong ng o ( cuvet) c chiu dy xc nh.
+Thu, phn ly ph v chn sng cn o ri ghi li gi tr mt quang A ca ph, ngha l
o cng chm sng sau khi i qua dung dch mu nghin cu.
1.3.3.2. Trang thit b
S my quang ph hp th phn t UV-VIS

Hnh 2.8 S my UV-VIS

1. Ngun sng
2. B phn n sc
3, Bn gng
4 Gng

5.

Cuvet mu

6 Dung dch so snh

7,8 T bo Quang- in
9 X l tn hiu

a)Ngun sng

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Ngun sng cho hp th phn t cn c nng lng ln trong vng bc sng hp thu ca
cht phn tch cho php sn sng d tm v o. Ngoi ra n cn phi n nh trong sut thi gian o.
C nh vy th cc php o mt quang mi cho kt qu lp li.
Ngun sng ph bin nht to ra bc x kh kin v cn hng ngoi l n dy tc vonfram
W t 320 nm n 2500 nm. n vonfram-halogen cha mt lng nh iot trong v bc bng thy tinh
thch anh cha dy tc W, cho php n hot ng nhit khong 3500 K. iu ny dn n n
hot ng cho cng cao hn v m rng khong bc sng pht ra vo mt phn vng t ngoi.
n loi ny cng c tui th cao hn do gim s bay hi ca W khi hot ng. Cc hi W s tc dng
to WI2 khuch tn quay li dy tc n phn hy to li W.
n hydro nng deuterium D2
n ny cn gi l n h quang D2 do s phng in lm phn hy D 2 v pht ra ph lin tc trong
vng t ngoi t 200 n 400 nm
b) H quang hc
Vi nhng my n gin th cc b knh lc mu cho mt vng ph nht nh hoc dng lng
knh tch cc chm tia n sc. Trong cc my c phn gii cao v nhy cao, cc b n sc
ha l cc b cch t phn x.
B cch t phn x l mt b thy tinh c ph ln trn b mt ca n mt lp nhm mng v
khc cc vch c khong cch u nhau. S lng vch trn mt n v chiu di (nm) cng ln th
phn gii cng cao v cc tia tch ra cng n sc. Cc my UV-VIS hin nay c b cch t c s vch
khong 1200-1800 vch/nm, c khi ln ti 2400 vch/nm i vi nhng my c phn gii rt cao.
Trn b mt ca nhng lp nhm ny li c ph mt lp mng SiO 2 b mt kim loi ny trnh b
oxi ha lm gim s phn x ca n. Nguyn tc n sc ha cc chm tia a sc l da vo hin
tng nhiu x. Khi nh sng a sc p vo khe hp ca cc vch th b nhiu x v mi khe tr thnh
mt ngun sng phn chiu nhng gc khc nhau nhng tia n sc.
H quang hc ca nhng my n gin thng l h mt chum tia cn trong my hin i l h
hai chum tia.
c) Detector
Detector l b phn thu nhn chum sng v chuyn chng thnh tn hiu in o lng
cng ca chum sng . Trong cc my n gin ngi ta dng t bo quang in cn trong cc
my hin i c nhy cao th ngi ta dng cc ng nhn quang in . Cu to ca hai loi ny
tng t nhau nhng electron pht ra t catot trong ng nhn quang in c gia tc hng v

15

dynode c duy tr mt th cao hn 90 V so vi catot. Electron ny khi p vo b mt ca dynode

th to ra nhng electron th cp v sau c gia tc hng v dynode th hai c th dng hn
90 V so vi dynode th nht. Mt ln na s khuch i electron xy ra v khi qua hang lot dynode
lin tip s electron to thnh tng ln n 10 6 n 107 cho mi photon p vo catot. Nh vy dng
in c khuch i v c o.

CHNG HAI

XC NH TARTRAZINE TRONG THC PHM

2.1.nh tnh
* Pha long 1 ml dung dch S (cht chun phn tch) thnh 100 ml bng dung dch acid hydrocloric 0,1
N. Ph t ngoi ca dung dch thu c trong khong 230 n 550 nm c hai hp th cc i 256 5

16

nm v 430 3 nm.
Pha long 1 ml dung dch S thnh 100 ml bng dung dch natri hydroxyd 0,1 N. Ph t ngoi ca
dung dch thu c trong khong 230 n 550 nm c hai hp th cc i 260 5 nm v 396 3 nm.
*Trong phn cht mu lin quan, vt chnh trong sc k thu c ca dung dch th (2) phi ph
hp vi vt chnh trong sc k thu c ca dung dch i chiu (1) v v tr, mu sc v kch
thc.
* trong ca dung dch
Dung dch S: Ha tan 50 mg ch phm trong nc v pha long thnh 50 ml bng cng dung mi.
Dung dch S phi trong
*Cht mu lin quan
Xc nh bng phng php sc k lp mng
Bn mng: Silica gel G
Dung mi khai trin: Amoniac m c nc ethanol n-butanol (10 : 25 : 25 : 50).
Dung mi ha tan: Hn hp nc methanol (1 : 1).
Dung dch th (1): Ha tan 40 mg ch phm trong dung mi ha tan v pha long thnh 10 ml vi
cng dung mi.
Dung dch th (2): Pha long 2 ml dung dch th (1) thnh 10 bng dung mi ha tan.
Dung dch i chiu (1): Ha tan 40 mg tartrazin chun (C) trong dung mi ha tan v pha long
thnh 50 ml vi cng dung mi.
Dung dch i chiu (2): Pha long 1 ml dung dch i chiu (1) thnh 20 ml bng dung mi ha tan.
*Cch tin hnh:
Ly lml mi dung dch trn. Trin khai sc k chm ring bit ln bn mng n khi dung mi i
c 15 cm. Ly bn mng ra v kh ngoi khng kh. Quan st sc k di nh sng ban ngy.
Trn sc k thu c ca dung dch th (1), ngoi vt chnh ra, khng c c vt no m mu
hn vt chnh trn sc k thu c ca dung dch i chiu (2).
*Cht chit c bng ether
Khng c qu 0,5%.
Cn chnh xc 2,0 g ch phm ( sy trong chn khng nhit 600C ti khi lng khng i) vo
bnh nh mc nu 200 ml, thm ether khan (TT) va n vch. Lc c hc trong 30 pht, lc. Ly
100,0 ml dch lc, cho bay hi n kh trong chn khng nhit 200C. Lm kh cn trong bnh ht
m ti khi lng khng i. Khi lng rn thu c khng c qu 5 mg.

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*Cht khng tan trong nc

Khng c qu 0,2%.
Ha tan 2,0 g ch phm trong 200 ml nc bng cch un nng ti khong 900C. ngui, lc qua
phu thy tinh xp s 4 c sy kh 100 -1050C ti khi lng khng i. Ra cn thu c vi
nc cho n khi thu c dch lc khng mu. Sy cn 100 1050C ti khi lng khng i. Khi
lng cn thu c khng c qu 4 mg.
*Amin thm bc nht
Khng c qu 40 phn triu.
Ha tan cn thu c phn cht chit c bng ether trong 10 ml toluen (TT). Ly 2,5 ml dung dch
thu c, thm 6 ml nc v 4 ml dung dch acid hydrocloric 0,1 N (TT). Lc mnh, yn cho tch
lp, loi b lp hu c. Thm vo pha nc 0,4 ml dung dch natri nitrit 0,25% (TT) mi pha. Lc u
v yn 1 pht. Thm 0,8 ml dung dch amoni sulfamat 0,5% (TT) v yn 1 pht. Thm 2 ml dung
dch N-(1-naphthyl)-ethylendiamin dihydroclorid 0,5% (TT). yn 1 gi. Dung dch khng c
m mu hn dung dch i chiu c chun b bng cch thay pha nc bng hn hp 1 ml dung
dch naphthylamin 0,001% (TT), 5 ml nc v 4 ml dung dch acid hydrocloric 0,1 N (TT).
*Crom ha tan
Khng c qu 50 phn triu.
Xc nh bng phng php quang ph hp th nguyn t
Dung dch th: Ha tan 0,500 g ch phm trong 25 ml nc bng cch un nng ti khong 900C.
ngui, thm nc va 25 ml, lc qua phu thy tinh xp s 4.
Cc dung dch chun: Dng dung dch crom mu 100 phn triu (TT) pha cc dung dch chun 0,5
phn triu, 1 phn triu v 2 phn triu.
Cch tin hnh: S dng my hp th nguyn t c trang b n cathod rng crom, u t s dng
ngn la acetylen khng kh nn. o hp th ca cc dung dch chun v dung dch th 357,9
nm. T hp th o c ca cc dung dch chun v dung dch th, tnh hm lng crom ha tan
trong ch phm.
*Kim loi nng
Khng c qu 20 phn triu (Ph lc 9.4.8).
Ly 1,0 g ch phm v tin hnh theo phng php 3. Dng 2,0 ml dung dch ch mu 10 phn triu
(TT) chun b mu i chiu.
2.2.nh lng

18

Cn chnh xc 0,150 g ch phm sy trong chn khng nhit 600C ti khi lng
khng i, ha tan trong dung dch amoni acetat 2 M (TT) mi pha v pha long thnh 100,0 ml bng
cng dung mi. Pha long 2,0 ml dung dch thu c thnh 200,0 ml bng dung dch amoni acetat 2 M
(TT) mi pha. Pha dung dch chun tng t trong cng iu kin, dng khong 0,150 g tartrazine
chun sy trong chn khng nhit 600C ti khi lng khng i.
Ph t ngoi ca dung dch th c mt hp th cc i khong 426 nm, khng lch qu 5 nm
so vi bc sng hp th cc i ca dung dch chun o trong cng iu kin. o hp th ca hai
dung dch ti bc sng hp th cc i.
Tnh hm lng C16H9N4Na3O9S2 trong ch phm, da vo hp th o c ca dung dch
chun, dung dch th v nng ca dung dch chun
*Lu : Vic xc nh hp th quang phi tin hnh ngay khi pha xong dung dch, bi v
mu ca dung dch c th nht dn theo thi gian.

PHN TH BA

KT LUN

1. tm hiu v phm mu Tartrazine v nhng nh hng ca n i vi sc khe con ngi.

2. Tm hiu v phng php ph hp th phn t UV-VIS

19

3. Vn dng phng php ph hp th phn t UV-VIS xc nh nh tnh v nh lng

Tartrazine

TI LIU THAM KHO

1.Thng t s: 27/2010/TT-BYT nm 2010 ban hnh Quy chun k thut quc gia v ph gia thc
phm phm mu.
2. Bi Xun Vng, Phn tch cng c trong ha hu c, Nng 2010

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