PHN TCH KIM LOI

Bao gm cc ch tiu:
+ Xc nh Asenic bng to phc vi Molydat.
+ Xc nh Cardimi bng to phc vi Dithizone.
+ Xc nh Cu phng php Carbamat
+ Xc nh Fe bng to phc 1-10 Phenantrolin
+ Xc nh Pb bng to phc Dithizon
+ Xc nh Thit bng trch ly Dithiozone
+ Xc nh Zn bng to phc Dithiozone
+ Xc nh Thit bng chun Iod

XC NH ASENIC BNG TO PHC

AMONIMOLIPDAT

Nguyn tc: Mu thc phm c x l trong mi

trng HNO3 v H2SO4 m c . Sau Asenat (V)
c kh v As (III) bng Zn trong mi trng HCl v
NaBrO. Cui cng c to phc vi NH4MoO4 , hm
lng As c o bng hp th ti bc sng 845nm.

XC NH ASENIC BNG TO PHC

AMONIMOLIPDAT
Tch Asen ra khi hn hp phn gii:
Ly 20ml dung dch sai khi phn gii cho vo bnh phn
ng, thm 10ml nc ct, 5ml HCl 2:1, 5 ml KI 15%, 4
git SnCl2 40%. Lc bnh sau mi ln thm.
ng thu gi As c nhi Bng thy tinh, ct sch, bi
thy tinh, cng vi dung dch HCl v NaBrO. Ni ng
gi As vi bnh phn ng trong 30 pht. Lc ny As tn
ti di dng AsCl3.
Tch phn ng gi As ra khi thit b v ra bng nhiu
ln bng nc ct mi ln 2ml, nc ra cho vo bnh
m 25ml. Thm 0,5 NH4MoO4 , 1ml Hydrazin, nh
mc ng 25ml. yn 75 pht ri o bc sng
845nm.

XC NH ASENIC BNG TO PHC

AMONIMOLIPDAT

Xy dng ng chun:
+ Chun b dy chun c cha : 0,1ml; 1ml; 2ml; 3ml;
4ml;5ml; 6ml dung dch 2g/ml As2O3 cho vo cc bnh
m 25ml, thm 3ml NaBrO v H2O ti 15ml, thm 0,5
NH4MoO4 , 1ml Hydrazin, nh mc ng 25ml. Lc
u ri yn 75 pht sau o hp thu 845nm
T phng trnh ng chun v hp thu ca mu
c tnh c hm lng As.

Quy trnh phn tch Arsen

Mu

Cn

HNO3
m (bnh Kjeldahn)
Sng trong + H2O + Amonicitrat
H2SO4 t0

As2O3

Vm

Pha chun gc
Chun lm vic
Chng ct

Tin hnh chng ct

Vx

To phc Molipdat
Thu AsCl3
o = 845 nm

To phc Molipdat

Thu AsCl3

HCl + KI+ SnCl2

o = 845 nm

y = ax+b Ax

XC NH CADIMI BNG TO PHC

DITHIZON
Nguyn tc: Mu c phn gii trong HNO3 v
H2SO4. Sau pH c chnh ti 9. Phc ca cc kim
loi v Cd vi Dithizon c trch ly trong Cloroform.
Loi cc kim loi ra khi Cd v Zn bng HCl (Cd v
Zn vn to phc vi Dithizon trong mi trng
CHCl3). Kim ha mi trng Dithizon phc Zn b
loi b. Tch lp phc Cd vi dithizon, tin hnh o
hp thu tnh hm lng

XC NH CADIMI BNG TO PHC

DITHIZON
X l mu:
+ Mu c cn t 5-10g, thy phn bng 10ml H2SO4
1:1 v HNO3 , b sung acid trong qu trnh thy phn
cho n hon ton, cn li phn cht bo khng tan.
+ Thm 15ml (NH4)2C2O4 bo ha ri gia nhit ln na
cho ti si. Lm lnh lc b phn khng tan, ra bng
nc nng.
+ Pha long dung dch ra bng 25ml nc, 1g
diamonicitrat, 1ml ch th thimolxanh ri chnh pH v
9 bng NH4OH t t cho n khi dd chuyn t vng
xanh ti xanh bin. Sau dnh mc ti 125ml

XC NH CADIMI BNG TO PHC

DITHIZON
+ Tin hnh trch ly nhiu ln vi 5ml Dithizon/
Cloroform cho n khi lp Cloroform c mu xanh.
+ Chuyn ton b lp Cloroform qua phu chit th 2,
thm 40ml HCl 0.2M lc mnh, yn tch phn
Cloroform. Dng mt lng nh CCl4 tch phn
Dithizon cn li,
+ Thm vo phn Cloroform va tch bng 10 ml
NaOH 5%, Lc mnh tch phn Cloroform cha phc
Cd qua phu chit th 3 Lp li nhiu ln bng 5ml
Dithizon/ Cloroform cho n khi lp Cloroform khng
mu.
+ Tin hnh o bc sng 510nm

XC NH CADIMI BNG TO PHC

DITHIZON
Xy dng dy chun:
+ Cho tng th tch cha 0, 5, 10, 15, 20, 25 g Cd vo
tng phu chit
+ Thm 40ml HCl 0.2M, 10ml NaOH 5% v 25ml
Dithizon.
+ Lc mnh trong 1 pht, yn trong 3 pht.
+ Tch b 5 ml u lp lng Cloroform, sau o
bc sng 510nm.
+ Xy dng ng chun t kt qu o

Chu Trnh Phn Tch Cardimi

Mu

Cn

Lc + Diamonicitrat
Trong sut + (NH4)2C2O4
5-10 g
0
HNO3 , t
NH4OH
HCl

pH= 9
Thu phc to thnh

Dithizon/Cloroform
Nhiu ln

HCl 0.2M

Ht

Vx

Cd tinh kit
Pha

Thu lp Cloroform

Dy chun

Dithizon/Cloroform NaOH 5%
Tch phc Cd- Dithizon

HCl, NaOH, Dithizon

Tch ly lp phc

o = 510nm

Ax

Vm

y= ax+ b

o = 510nm

XC NH CU BNG TO PHC
DIETYL DITHIO CARBAMAT
Nguyn tc: Mu c phn hy trong HNO3 v H2SO4 .
ng c tch ra v xc nh pH = 8.5 cng vi Dietyl
dithiocarbamat trong s hin din ca EDTA. Bi v Te
cng to phc tng t nhng bn mu trong NaOH 1N.
Khong mu o t 0 ti 50g.

XC NH CU BNG TO PHC
DIETYL DITHIO CARBAMAT
Chun b mu:
+ Cn khong 10g mu vo cc Pyrex 250ml, thm 20ml
HNO3 v 10ml H2SO4, dy bng np knh. un nh cho
n si, thm HNO3 khi ly dung dch c mu nu.
+ Lc b phn bo khng tan, thm 25m nc v 10ml
H2SO4 un si li. Lc b phn khng tan,
+ Lp li bc thm 25ml nc v un si, lc ly phn
dung dch v nh mc thnh 100ml.

XC NH CU BNG TO PHC
DIETYL DITHIO CARBAMAT
Tch v nh lng:
+ Ht mt th tch ph hp cho php o vo phu chit
100ml, thm H2SO4 2N cho n 25ml, 10ml CitratEDTA, 2 git ch th Thimol xanh v tng git NH4OH
cho n khi c mu xanh bin.
+ ngui thm 1ml Carbamat, 15ml CCl4. Lc mnh
trong 2 pht.
+ yn yn tch ly phn CCl4 o bc sng 400nm.
+ Kim tra s c mt ca Bi v Te bng cch cho phn
CCl4 vo phu chit thm 10ml KCN 5% vo lc mnh,
yn nu c mu th Bi v Te c. Ly phn CCl4 cho vo
10ml NaOH 1N, lc mnh tch ly phn CCl4 ri o

XC NH CU BNG TO PHC
DIETYL DITHIO CARBAMAT
Chun b dy chun:
+ Cho 0;1; 2,5; 5; 10 v 20ml dung dch chun Cu 2g/ml
vo cc phu tch, thm H2SO4 2N cho n 25ml.
+ Thm 10ml Citrat- EDTA v tin hnh nh mu
+ Phc Cu c tch bng CCl4 v o bc sng
400nm

Chu trnh phn tch ng

Mu

Cn

Lc, ra

HNO3

Vm
Dch trong sut
m(g)
0
nh mc
H2SO4, t
Ht
Vx
NH4OH
Thimol xanh

Chun Cu tinh kit

Pha

pH = 9
Carbamat
Lc
CCl4

Dy chun
NH4OH H2SO42N
Thimol xanh Citrat- EDTA
pH = 9
Carbamat Lc
CCl4
Tch phn CCL4

H2SO42N
Citrat- EDTA

Tch phn CCL4

o = 400nm

y= ax+b
o = 400nm

Ax

XC NH ST BNG TO PHC
1-10 PHENANTROLIN
Nguyn tc: Mu thc phm c tro ha, sau tro c
ha tan bng HCl ri nh mc n th tch bit trc, St
trong dch c kh ton b v Fe( II) sau to phc vi
1-10 phenantrolin. Phc hnh thnh c o bc sng
510nm.

+ Fe2+

3
N

N-N
Fe

2+

XC NH ST BNG TO PHC
1-10 PHENANTROLIN
Chun b mu:
+ Cn chnh xc mt lng mu ng nht cho vo chn
nung. Tin hnh un nh lm bay hi bt mu. Chuyn
chn cn vo l nung t nhit 450oC .
+ Tin hnh nung nhit trn khong 2 gi th lm ngui
cho vo 1ml MgNO3 50%. Tip tc nung cho n hon
ton,.
+ Ha tan tro bng 5ml HCl m c, y np knh ng h
ri un nng cho n cn. Thm tip 3 ml HCl na ri un
nng.
+ Ra mt knh bng nc nng, ha tan tro bng nc
nng. Tin hnh lc , ra , nh mc 100ml .

XC NH ST BNG TO PHC
1-10 PHENANTROLIN
Xc nh st:
+ Ht10ml dch sau khi nh mc, thm 1ml Hydroxylamin.
+ Sau 5 pht thm 5ml m Acetat , 1ml 1-10 phenantrolin
+ o hp thu bc sng 510nm
+ T hp thu, xc nh hm lng st qua phng trnh
ng chun

Chu trnh phn tch St

Mu

Cn

m(g)

4500C

Than ha

Chun St

Mg(NO3)2
5500C

Tro ha
HCl
un nng

Ha tan bng nc nng

nh mc

Pha dy chun
Hydroxylamin
m Acetat

Vm
Ht

Vx

+ 1-10 phenantrolin
o = 510nm

Hydroxylamin
m Acetat

y = ax+b

Ax

o = 510nm
+ 1-10 phenantrolin

XC NH CH BNG TO PHC
DITHIZON/CLOROFORM
Nguyn tc: Mu c tro ha, ha tan trong acid. Trung
ha lng acid bng NH4OH/Citrat. Cc cht gy cn tr
bng to phc vi CN-. Ch to phc vi Dithizon/CHCl3.
Phc Ch v Dithizon c tch ra sau c phn b mt
ln na trong HNO3 long. Lp cht lng c chnh ti pH
= 9,5 10 sau cho to phc vi Dithizon/CHCl3 v
bc sng hp thu 510 nm

XC NH CH BNG TO PHC
DITHIZON/CLOROFORM
Chun b mu:
+ Cn chnh xc t 5 ti 100 g ty theo HL ch c trong mu
vo chn nung. Sy mu trn bp in. Nu mu c hm
lng tro thp c th thm t 2-5ml Ash aid
+ Trong qu trnh than ha khng c pht la, khi mu
than ha v kh hon ton, t mu vo trung tm l
nung, tng nhit ln t t cho n 5000C.
+ Thc hin qu trnh nung trong vng t 8 gi. Nu tin
trnh khng hon ton, thm vi ml HNO3 sau nung tip.
+ Khi qu trnh tro ha hon ton dng nm knh y li,
cho vo 15ml HCl . un nh ha tan tro, ra mt di
knh bng nc nng. Lp li tin trnh mt ln na, sau
nh mc 100ml bng nc ct.

XC NH CH BNG TO PHC
DITHIZON/CLOROFORM
Tch v nh lng:
+ Ly mt lng dung dch thch hp thm dung dch citrat
sao cho khong 10 g citric.
+ Trung ha nh bng NH4OH, yn 1-2 pht
+ Thm t t H2S vo cho n khi c kt ta. Lp tc tch
kt ta bng lc chn khng. Ha tan bng HNO3 . un
nng loi H2S.
+ Chuyn dung dch vo phu tch, thm 10ml dung dch
Citric 0,5g/ml. trung ha bng NH4OH.
+ Thm 5ml KCN 10% kim tra pH bng ch th Thymol
xanh pH phi t c 8.5 9.5.

XC NH CH BNG TO PHC
DITHIZON/CLOROFORM
+ Lp tc thm 20 ml Dithizon, lc t 2 ti 5 pht, yn,
Chuyn lp Clorpform vo phu nh cha 25ml HNO3 1%.
+ Lp li bc trn cho n khi lp Cloroform c mu xanh.
+ Thu ton b dung dch HNO3 cha ch, nh mc 100ml
bng HNO3 1%.
+ Ly 50ml dch sau kh nh mc, thm 10ml NH4OH v
Cyanide, lc u ( pH = 9,7)
+ Thm 8ml Dithizon vo, lc trong mt pht v yn.
+ Tch ly phn phc ch vi Dithizon trong CHCl3 ra khi
h v o bc sng 510nm

XC NH CH BNG TO PHC
DITHIZON/CLOROFORM
Chun b dy chun:
+ Dng Pypet ht mt lng chun Pb 1g/ml 0 - 5- 10
-15 20 25ml vo cc phu tch. Thm HNO31% vo
cho 50ml.
+ Thm 10ml dung dch NH4OH KCN vo ( pH = 9,7)
+ Thm 8ml Dithizon/CHCl3, lc 1 pht cho phc hnh
thnh, yn tch phn phc ra.
+ Chuyn t t phn cht lng phc vo ng thy tinh sch
o bc sng 510nm

Chu trnh phn tch Ch

Mu

Cn

y = ax+b

m(g)

Ax

o = 510nm

4500C

Than ha

Ash aid

o = 510nm

Pha
Chun Ch

HCl
un nng

Dithizon Ha tan bng nc nng

nh mc
pH= 9.7
NH4OH,Citric

Dithizon/CHCl3 Ch/HNO3
pH= 9.7
NH4OH
HNO3
Citric
Pha dy chun

5000C

Tro ha

HNO3
Tch Phc
Dithizon
pH= 8.5-9.5

Vm
Ht

Vx
Dd Citrat = 10 g
Trung ha bng NH4OH

Lc kt ta H2S
HNO3
Thu KT
Citric, KCN, NH4OH

XC NH THIT BNG TO PHC

CATECHOL VIOLET
Nguyn tc: mu l c phn hy trong HNO3 v H2SO4.
Tip theo l trong hn hp HClO4 v H2O2. Sau c ho
tan bng nc cho n th tch c nng acid khong
4.5M . Thit (IV) c chuyn qua SnI4 bng KI, sau
c trch ly qua mi trng cyclohexan. Thit c a v
dng Sn(OH)4 bng dung dch NaOH. Sau khi loi b Iod.
Thit c to phc vi Catechol Violet, trong mi trng
m pH = 3.8. hp th A c o bc sng 555nm

XC NH THIT BNG TO PHC

CATECHOL VIOLET
Chun b mu:
+ Cn chnh xc mt lng mu sau khi ng nht c
lng Sn khong 2-25g vo bnh Kjeldahn.
+ Thm tun t 50ml HNO3 , 12,5ml H2SO4, 3 vin bi
thy tinh, lc u.
+ Gia nhit cc cht trong bnh n si bng n x, v gi
si sut qu trnh. Thm HNO3 khi thy bnh c mu nu.
+ Qu trnh kt thc khi bnh c mu nht, lm lnh v nhit
phng thm 1ml HClO4 gia nhit tr li trong 5 pht.
+ Lm lnh dung dch thm 1ml H2O2 gia nhit tr li sau
thm tip 1ml H2O2 lp li thm mt ln na.
+ Ra c bnh bng 5ml nc v gia nhit thm ln na.

XC NH THIT BNG TO PHC

CATECHOL VIOLET
nh lng:
+ Chun phn dch sau khi phn gii vo phu chit 100ml,
thm 37,5 ml nc lc ny nng acid t 4,5M. Lc u
bng tay.
+ Thm 5ml KI 5M, 10ml Cyclohexan, lc mnh trong 2
pht ri lng.
+ Chuyn lp cht lng vo phu th 2, gi li phn
Cyclohexan. Thm 10ml cyclohexan vo phu th 2, lc
mnh tch ly phn Cyclohexan, gp vi phn 1.
+ Thm 5ml nc, 1,5ml NaOH 5M, lc mnh trong 2 pht,
chuyn phn cht lng NaOH vo beaker 50ml cha sn
2,5ml HCl 5M.

XC NH THIT BNG TO PHC

CATECHOL VIOLET
+ Lp li bc trn vi 3ml NaOH 5M v thc hin nh
trn.
+ Loi b Iod trong dch acid bng Acid Ascorbic 5%.
+ Thm 2ml Catechol Violet, lc u, Chnh pH v 3.8 bng
NH4OH 5M v HCl 5M
+ Chuyn lng dung dch sau khi chnh pH vo bnh nh
mc 25ml, 2ml etanol v nh mc bng nc . yn
nhit phng 45 pht trc khi o
=

XC NH THIT BNG TO PHC

CATECHOL VIOLET
Lp ng chun:
+ Dng pypet ht 0; 1; 2; 3; 4; 5ml chun Sn 5g/ml vo
cc phu chit, thm H2SO4 4,5M cho n 50ml.
+ Thc hin ging nh mu t giai on thm KI cho n
thm thuc th Catechol Violet v chnh pH v 3,8.
+ Tin hnh o hp thu 555nm, xy dng phng trnh
chun
+ Tnh ton hm lng Thit t phng trnh ng chun

Chu trnh phn tch Thit

Mu

Cn

HNO3

Mu sng trong
H2SO4,t0
HClO3
t0
H2O2
o = 555nm
+ 37ml H2O

m(g) Bnh Kjeldahn

Chun Thit
Pha

Cyclohexan

Pha dy chun
Thc hin cc bc t thm KI
Phc Thit
o = 555nm

y = ax+b

Ax

+ KI

Tch phn phc SnI4/Cyclohexan

H2O

NaOH 5M

Thu phn NaOH

Ascorbic HCl 5M
NH4OH 5M
o = 555nm
Catechol Violet
pH= 3.8
Phc Thit

XC NH KM BNG TO PHC
DITHIZON
Nguyn tc: Mu l c phn gii trong mi trng HNO3
v H2SO4 . Cc kim loi gy tr ngi nh : Ch. ng,
Cadimi, Bimus, Antimon, Thit, Bc c kt ta di dng
Sulful (H2S). Co v Ni c loi bng s to phc vi
Nitroso- Naphthol v Dimetylglyoxim. Km c chit ra
di dng phc vi Dithizon/ CCl4.. Phc o hp th
540nm.

XC NH KM BNG TO PHC
DITHIZON
X l mu: Cn chnh xc khong 25 g mu cho vo bnh
kjeldahn. Lm kh mu n th tch nh, thm 5ml HNO3 ,
25ml H2SO4 un nng. Thm tng lng nh HNO3 trong
qu trnh phn gii, cho n khi dch phn gii c mu trong
sut. Tip tc un nng ha hi lng acid. ngui,
hon tan bng 25ml nc ct, tin hnh lc ra bng nc
nng , nh mc 100ml.

XC NH KM BNG TO PHC
DITHIZON
Tch v nh lng:
+ Ly mt lng dung dch sau khi phn gii, thm 2 git
ch th MR, trung ha bng NH4OH, thm HCl sao cho pH =
2.
+ Cho t t H2S vo cho n khi kt ta hon ton .
+ Lc qua giy lc bng xanh, ra bng HCl 1:6, sau
bng nc ct.
+ Lm ngui trung ho bng NH4OH v HCl bng ch th
Phenol .
+ Pha long nh mc dung dch ( 0,2- 1g/ml)

XC NH KM BNG TO PHC
DITHIZON
+ Ly 20ml trn cho vo phu tch 125ml, thm 5ml
NH4OH- Citrat, 2 ml Dimetylglyoxim, 10ml Nitroso-
Naphthol. Lc trong 2 pht.
+ Loi b lp dung mi cha phc ca Ni v Co, thu lp
cht lng cn li.
+ Ch pH v 8.2, thm 2ml Dithizon v 10ml CCl4, lc
mnh. Thu ly phn cht lng cha phc ca Km.
+ Chnh v pH= 8.8 bng 5ml Amoni- Citrat, lc trong 2
pht.
+ Ht 5ml dung dch to phc. Cho vo p6ng1 nghim kh,
pha long bng 10ml CCl4, ri o bc sng 540nm

XC NH KM BNG TO PHC
DITHIZON
Chun b dy chun:
+ Chun b mt lot phu cha dung dch Km : 0; 5; 10; 15
v 20g Km. Pha long vi 25ml HCl 0,04N
+ Thm vo mi phu 5ml Amoni- Citrat. 10ml CCl4, lc
trong 2 pht. Ht 5ml phn dch to phc, thm 10ml CCl4,
lc u v o bc sng 540nm

Chu trnh phn tch Km

Mu

Cn

m(g) Bnh Kjeldahn

Chun Km

HNO3

Mu sng trong

H2SO4,t0

t0

Pha

Vm

Pha dy chun
NH4OH
Citrat

Nitroso-Naphthod
Dimetylglyoxim

Thu phn cht lng (loi phc Ni,Co)

pH= 8.2
Dithizon/CCl4
Phc Km

+ H2O

y = ax+b

Ax

o = 540nm
Phc Km

Ht Vx
Phu tch
NH4OH
Citrat

Nitroso-Naphthod
Dimetylglyoxim

Thu phn cht lng (loi phc Ni,Co)

Dithizon/CCl4
pH= 8.2