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Thc phm c th b nhim cc kim loi nng t nhiu ngun khc nhau:
Nguyn liu dng ch bin thc phm, trong qu trnh ch bin, bo qun thc
phm, qu trnh chuyn ch thc phm..
Trong thi i ngy nay vic s dng ho cht a vo sn xut kh ph
bin nn nguy c nhim cc kim loi nng vo thc phm ngy cng tng do
tnh trng ng c do cc kim loi nng ang gia tng. V vy vic tm ra
cc phng php xc nh hm lng kim loi nng c trong thc phm l
vn cn quan tm hng u bo v sc kho v mi trng.
I0
= .l.C
I
A : hp th
: h s hp th mol (lit.mol-1.cm-1).
c trng cho kh nng hp th nh sng ca dung dch. Ph
thuc vo bn cht dung dch v bc sng .
l: b dy dung dch (cm)
C: nng dung dch (mol/l)
HDz
H+
Ditizon to vi ion nhiu kim loi nhng ditizon c mu, t tan trong
nc nhng tan trong cacbon tetra clorua hay cloroform.
Cc ditizon c th tn ti di hai dng, tu thuc vo acid ca mi
trng.
- Trong mi trng acid hay trung tnh th chng tn ti di dng
xeton.
- Trong mi trng kim chng tn ti di dng enol.
NH N C6H5
MI
S=C
N N - C6H
MI S C
N = N - C6H5
MI
N = N - C6H5
MDz + nH+
Dz-
HDz
pKA = 8,7
1.2.2. ng dng.
1. 3. Chun b mu
Km, ng, ch c trong lng thc phm vi lng nh nn mun xc
nh chng cn phi v c ho lng thc thc phm. C hai phng php v
c ho:
1.3.1. Phng php kh.
a. Dng c, ho cht
Capxun dung tch 250 ml
Bp cch ct
Pipet 100 ml
Giy lc
Cn k thut
Phu
Bp cch ct
5
Pipet 100 ml
Giy lc
Phu
Cn k thut
Bp in, l nung iu chnh c nhit ( 600- 7000 C)
- Ho cht:
b. Tin hnh
- Ly lng mu nh trn cho vo capxun. Thm vo capxun 3 ml acid
nitric c v 50 ml acid sunfuric c.
- t capxun ln bp in, un si dung dch trong capxun. Tip tc un
v c mi pht li nh thm 5- 20 git acid nitric c. Kh NO 2 mu nu s
thot ra (lm trong t ht hi).
- Nu thy dung dch trong capxun thm mu li th tng tc nh acid
nitric c. Khi dung dch tr nn nht mu th gim tc nh acid nitric c,
n khi dung dch khng mu th thi. Tip tc un cho khi trng bc i ht,
ri li tip tc un si 10 pht na.
- Nu sau dung dch vn khng mu th vic v c ho hon ton
xong. Nu dung dch en tr li th nh acid nitric.
- Ly capxun ra khi bp in. Cho vo capxun 0,20g amonaxetat, khuy
cho tan ht.
- Chuyn ton b dung dch t capxun vo bnh nh mc dung tch 250
ml. Thm nc ct hai ln n vch mc, lc k.
Nu dung dch capxun b c th phi lc trc khi chuyn vo bnh nh
mc.
gian 20 giy; nguyn t ho nhit 1900oC, trong thi gian 3 giy. Vng
tuyn tnh l: 2 50 ng/ml.
2. ng dng.
Phng php ny c dng xc nh hm lng kim loi c trong
mu thu sn, mu nc v nc thi.
III. Phng php cc ph.
Phng php Von Ampe l nhm cc phng php phn tch in
ha da vo vic o dng ti in cc ch th theo th p vo, qua xc nh
nng cht cn phn tch. Mt trong hai in cc c din tch b mt kh
nh (b hn din tch b mt in cc kia kh nhiu ) nn rt d b phn cc
v qu trnh kh hay oxi ha ca ion kim loi kho st xy ra trn chnh in
cc ny. o cng dng in chy qua bnh in phn ng vi cc gi tr
in th khc nhau t vo hai in cc, v I = f(E) ta s nhn c mt
ng cong gi l ng cong phn cc. Qua xc nh nng cht cn
phn tch.
Phng php Von Ampe c hai nhm chnh l phng php cc ph
v phng php Von Ampe ha tan. y l nhng phng php s dng
rng ri nht trong phn tch in ha.
3.1. Khi nim v phng php cc ph.
Phng php cc ph cng l phng php in phn, nhng y vic
xc nh nng thng qua vic nghin cu quan h gia in p t vo hai
in cc (E) vi dng in (I) hnh thnh trong qu trnh phn cc.
Phng php cc ph c th nh tnh v nh lng nhiu cht bng
cch in phn dung dch phn tch trn in cc git thu ngn, ri sau v
ng biu din Dng-Th ghi s bin i cng dng theo s bin i
cng th in cc ca s thu phn.
V nguyn tc ca phng php cc ph
Phng php cc ph bao gm cc giai on:
- t cc th khc nhau vo in cc kh cc ion khc nhau v mi
ion c mt th kh tng ng xc nh, do qua th kh ca ion c th nh
tnh c ion .
x= h
tc
10
tstep
11
Chu k git
: Bin xung
Estep : Bc th mt xung in
tstep
13
15
m Pb
. 25
M
25
CPb = mPb . V 1 .
M
d
Trong :
CPb: hm lng ch c trong mu th (mg/g)
mPb: hm lng ch c trong dung dch mu tnh c theo ng
chun mg/mol.
25: th tch dung dch acid clohydric nng 1M dng ho tan mu
(ml)
Vd: th tch dung dch mu th b sung 1ml dung dch m phn
tch (ml)
M: khi lng mu th (g)
18
19
20
21
22
24
25
26
27
dung dch chun c nng thch hp vo dung dch phn tch v ghi cc ph
ln na. lng Km c thm vo nh th no sng th hai c chiu cao
gp ri hoc gp i ca chiu cao sng th nht.
Cch tin hnh nh sau:
Trong bnh nh mc dung tch 50 ml, thm vo 25ml mu nc hm
lng ca km trong l 1 25 mg. Nu trong mu c hm lng Km nh
hn 0,15mg/l, th ly 250ml nc thm vo 1 ml HCl c v lm bay hi n
cn kh hai ln nh nhau v ho tan b kh trong 25ml nc ct. Sau thm
tip vo 5ml dung dch nn, 1ml gielatin, 1ml Na2SO3 v nh mc bng nc
ct, lc u dung dch trong bnh, chuyn 25ml dung dch vo bnh in phn
v ghi cc ph t -0,8 V n -1,5 V, nhy ca my sao cho sng thu
c c chiu cao t nht 20 mm. Thm vo bnh in phn 0,2ml dung dch
chun (loi no tu thuc vo nng Km trong dung dch mu) v ghi cc
ph dung dch ny nhy c. Chn nng dung dch chun thm vo sao
cho sng th hai c chiu cao gp ri hoc gp hai ln sng th nht.
Nu trong nc c ng, Cadimi, Niken vi hm lng hm lng cho
php xc nh cng vi Km, th cng tin hnh nh trn v ghi cc ph t
-0,2V n -1,5V. vic xc nh cng c tin hnh theo phng php thm
chun.
Nu hm lng ca cc nguyn t ngn cn qu ln th cn tch Km
trc nh sau: ly mt th tch nc sao cho hm lng km trong t 0,010,5mg trong 50ml. Ly 50ml thm vo 2 git metyl v trung ho cn
thn bng HCl long hoc bng NH3 long cho n khi cht ch th va i
mu. Thm tip vo 20ml dung dch che. Chit km mt vi ln, mi ln bng
20ml dithizon, chit n khi ln chit cui mu xanh ca dithizon khng thay
i. Gp tt c cc phn chit khc, thm vo 25ml HCl 1:5 v lc phu
gii chit km tr li tng nc. Gi tng nc v lp li s gii chit hai
ln na, mi ln 25ml HCl. Gp ton b dung dch nc thu c, lm bay
hi trn bp cch thu n cn kh v ho tan b kh trong nc ct. Tin
hnh xc nh km nh trn.
I.3.2.3 Phng php AAS
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29
xut hin khi trng SO3. Nu dung dch thu c cn c mu th thm 5ml
HNO3 c v lm bay hi ln na, ng tc ny c lp li cho n khi thu
c dung dch khng mu. Sau lm bay hi dung dch n cn kh. Phn
b sau khi ngui c ho tan trong nc ct hai ln, un nng ho tan
ht cc mui tan, lc qua phu kh bng thu tinh xp v gi ly xc nh
ng. loi tr cc i cc ph dng dung dch gielatin.
Nu mu cha t 2 50 mg Cu/l, th ly 25 ml dung dch mu cho vo
bnh nh mc dung tch 50 ml. nu mu nc ch cha khong 0,2 3 ml
Cu/l th ly 250 ml cho vo cc chu nhit sch, thm vo 1 ml HCl c v
lm bay hi trn ni cch thu. Sau khi ngui tm t bng 1 ml HCl c,
ho tan mui bng nc ct v chuyn ton b dung dch vo bnh nh mc
50 ml. Trung ho mu bng NH 3 n khi i mu metyl da cam, thm vo 10
ml dung dch nn, 1 ml gielatin, 1ml Na2SO3 nh mc bng nc ct hai ln
v lc u. trng bnh in phn bng vi ml dung dch , mt phn dung
dch trong bnh nh mc vo bnh in phn. Ghi cc ph t -0,2Vn -0,8 V
nhy thch hp. Sau da vo ng chun xc nh hm lng
ng.
Nu mu c hm lng Cu trong khong 0,02 5ml Cu/ lit nc th ly
250 ml mu nc thm vo 1 ml axit HCl c, lm bay hi n kh, sau
ngui thm vo 5ml HCl c na v li lm bay hi ln na n kh. Sau khi
ngui thm vo 5 ml dung dch c ch nh sau: 10 ml dung dch nn
c trn u vi 1 ml gielatin + 1 ml Na2SO3 + 38 ml nc ct, dng a
thu tinh nh khuy u cho mui trong cc tan ht. Chuyn ton b dung
dch vo bnh in phn kh cha thu ngn kh v sch dng lm anot
y. Ghi cc ph t -0,2 V n 0,8 V. Ri da vo ng chun tnh hm
lng ca ng.
Hin nay c nhiu phng php cc ph hin i c th xc nh Cu c
nng 10-9 M v c th xc nh trong nhiu nn khc nhau.
Bng phng php Vn-Ampe ho tan hp ph, s dng thuc th
catechol (pH = 7,8) Cu cho pc ti -0,2 V vi gii hn pht hin ti 1.10 -11 M.
Vi thuc th 6-hydroxi quinolin (pH = 6 9) Cu cho pc ti -0,45 V vi gii
hn pht hin l 2,4.10-10 M.
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iacc . tacc
C
=
VHg . n . F
( F : l hng s Faraday )
Trong :
VHg = AF . v
AF : Din tch b mt mng
v : dy ca mng
+ C ch ca phng php vn ampe ho tan catot ( CSV ):
Bc 1 :
2Hg
Hg22+ + 2e
Hg22+ + 2ABc 2 :
Hg2A2
2e
Hg2A2
2Hg
2A-
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