TIU LUN THUC TH HU C

ti
THUC TH HU C VI MT S ION KIM LOI

GVHD : PGS.TS L Vn Tn NHM TH : Nhm 7 LP : HPT3

1. NI DUNG
ng (Cu)

Coban (Co)

Gali (Ga)

BAO GM

Ch (Pb)

Gecmani (Ge)

Crom (Cr)

THUC TH HU C XC NH COBAN

Tnh cht ha l ca Coban Coban l nguyn t chuyn tip c electron ha tr 3d74s2, bn knh nguyn t 1,27 Ao, bn knh ion coban (II) 0,82 Ao v coban (III) l 0,64 Ao. Coban l kim loi mu xm c nh kim, c t tnh. N ha rn v rt chu nng, bn vi khng kh v nc, nhng d b oxi ha khi nghin nh nhit t n sng chi, n bc chy trong khng kh to Co3O4. S xi ha c trng ca Coban l +2 v +3 trong trng thi xi ha (II) l trng thi bn v c trng i vi Coban, cc dn xut ca Coban u c mu ring bit

Tnh cht ha l ca Coban

Mt s thng s vt l ca coban

T trng (g/cm
3)

Nhit nng Nhit chy (

oC)

cng (thang

Nhit thng hoa (

oC)

dn in tng i (Hg = 1) 10

si (

oC)

mox)

8,9

1493

3100

5,5

425

Mt s thuc th to phc ca Coban

8 Hydroxiquinolin
Phenylfluorone -nitrozo- -naphtol

8 Hydroxiquinolin

CTPT: C9H7ON M = 145,17

8 Hydroxiquinolin
Tnh cht l ha: Tn ti dng tinh th mu trng hi vng hay l nhng bt tinh th c mi

c trng. Hu nh khng tan trong nc v ete khi lnh; tan tt trong ru

etylic, axeton, clorofom, benzene cng nh trong axit v c long v kim. Dung dch lim ca 8 hydroxiquinolin c mu vng. Hng s phn ly K25 = 2.10-10. ng dng: 8 hydroxiquinolin tc dng vi mt s nguyn t (vi mi nguyn t c

pH xc nh) to thnh nhng mui ni phc kh tan. C mui ni phc ny

uwnggs dng rng ri trong thc t tch, phn tch trng lng, phn tch th tch cc nguyn t.

8 Hydroxiquinolin
Phn ng gia 8 Hydroxiquinolin v Coban Trong dung dch axetic axetat 8 Hydroxiquinolin tc dng vi coban

to phc kh tan kt ta.

Phc ny c tch v xc nh coban theo phng php phn tch khi lng.

Phenylfluorone

CTPT: C19H12O5 KLPT = 320,30

Phenylfluorone
Tnh cht ca thuc th Phenylfluorone l mt tinh th bt mu cam, c nhit nng chy ln hn 300oC. Xut hin hunh quang mu hi lc trong dung dch cn pH=8. Trong dung dch kim, thuc th phn ly yu. t tan trong nc (3.10-7M trong 20% ethanol, 25oC), t tan trong ethanol

lnh, nhng d tan trong cn b acid ho (HCl v acid H2SO4). N c th kt

tinh li t cn b acid ho vi s c mt ca ammoniac. Phenyfluorone c xem nh mt cht in ly lng tnh, v s phn ly

trong 25% ethanol c th c xc nh nh di:

Phenylfluorone
S to phc gia phenyfluorone vi Coban (II) Phenyfluorone to phc mu vi Coban (II) ti khong pH 4,5 5,0. Phc ny c cu to nh sau:

Dung dch phc ny c em o quang ti bc sng 645 nm xc nh hm lng Coban. Gii hn pht hin ca phng php ny cho php xc nh hm lng Coban n 2 ppm.

-nitrozo- -naphtol

CTPT: C 10 H 7 NO 2 M = 173,16

-nitrozo- -naphtol
Tnh cht l ha ca -nitrozo- -naphtol -nitrozo- -naphtol l hp cht tn ti dng bt tinh th mu vng nu. ha tan trong 100g dung mi: nc 0,1 g (20oC) ; ru etylic 2,4 g (13oC), d tan trong ru etylic nng, benzene, ete, acid acetic bng v trong dung dch kim, bay theo hi nc. Vi loi ha cht khng tinh khit s b nha ha.

ng dng:
Thuc th ny d to mui ni phc kh tan vi mt s nguyn t nn c dng trong cc phn ng mu, xc nh Coban, Paladi( tch ra khi Pt), Cu, Fe, theo phng php so mu hay phng php trng lng.

-nitrozo- -naphtol
S to phc gia -nitrozo- -naphtol v Coban Khi thm dung dch mui Coban trung tnh vo dung dch -nitrozo - naphtol trong acidacetic 50% ri thm vo dung dch CH3COONa. Khi un nng s cho kt ta mu nu .

-nitrozo- -naphtol

Phc mu c chit khi nc bng clorofooc hay cacbon tetraclorua, ri em o quang bc sng 540 nm. St, ng, niken cng to phc mu vi -nitrozo - -naphtol, dng natri xitrat loi b nh hng cn tr ca st. Loi b ng v niken bng trilon B. Nhng cht l lng v cht hu c gy cn tr, loi b bng cch chit

chng ra khi dung dch ngay sau khi axit ha.

Cu
Gii thiu v Cu Nhm chc phn tch ca Cu Mt s thuc th hu c to phc vi Cu Natri dietyldithiocacbamat Porphyrin Dithizone

Gii thiu v Cu
ng l nguyn t ha hc trong bng h thng tun hon c k hiu l Cu v s nguyn t l 29 Tnh cht vt l: ng l mt kim loi c mu vng nh , c dn in v dn nhit cao. Trng thi vt cht: rn im nng chy: 1357,6oK (1984,3oF) im si: 2840oK (4653oF) Nhit bay hi: 300,3kJ/mol Nhit nng chy: 13,05kJ/mol

Gii thiu v Cu
Do s oxy ha kh d dng ca Cu(I) thnh Cu(0) v Cu(II), do nhng phc ca Cu(I) thng ch c to thnh trong trng hp khi chng khng tan (v d nh CuCN v CuI) hoc l nu lin kt kim loi phi t c c tnh ch yu l cng ha tr.

Gii thiu v Cu
Tnh cht ha hc:
Cu hnh ca nguyn t ng: 1s2 2s2 2p6 3s2 3p6 4s1 3d10

V c in tch thp v cu hnh in t 3d10 nn Cu(I) to nhng phc bn vng nht vi nhng phi t phn cc mnh
Trng thi thng thng ca Cu l ha tr 2 v Cu(II) to nhiu phc bn vng. Cu hnh d9 lm cho ion Cu2+ d b bin dng v nh n to lin kt bn vi nhng anion cha lu hunh nh dietylditiocacbamat, etyl-xantogenat, ditizon to nhng phc tan trong dung mi hu c

Nhm chc phn tch ca Cu

L nhng -axyloinoxim c cng thc tng qut cha nhm nguyn t L nhng thuc th c trng ca Cu (II), (phn ng xy ra trong mi trng amoniac). Nhng hp cht ny ng vai tr nh mt acid kp v to vi Cu(II) mui mu lc khng tan trong nc c cng thc

Nhm chc phn tch ca Cu

Khi nghin cu tc dng ca axyloinoxim vi Cu II ngi ta chia chng ra lm 2 loi: Mt loi bao gm nhng hp cht to mui vi Cu khng tan trong amoniac (trong nhng hp cht ny ng bo ho phi t) Mt loi bao gm nhng hp cht to mui vi Cu tan trong amoniac (trong nhng hp cht ny ng cha bo ho phi t)

Nhm chc phn tch ca Cu

Mui ng to thnh thuc loi ny hay loi khc l do bn cht nhng gc c trong phn t quyt nh: Nu trong phn t thuc t c gc thm th mui ng tng ng khng tan trong amoniac. Nu trong phn t c gc bo th mui ng trong nhiu trng hp tan trong amoniac. Trng lng ca gc khng nh hng n tan ca mui ng trong amoniac.

Mt s thuc th hu c to phc vi Cu Phc chelate kim loi iu kin H Bc Mu b s sng pH = 7 pH = 5.5, pyridine chit vi cyclohexa ne pH = 6 _ _ 630 _

Thuc th
Pyrocatechol tm

Ion cn

Diketonate

ML2

430

2,2 .103

Pyrogallol

ML

582

0.95

Mt s thuc th hu c to phc vi Cu Alizarin complexone Murexid Zincon pH = 10 ML tm Vn pH = 8 ML g pH = 5 Xan ML 9 h pH = 4,7 + Natri _ ML lauryl sulfate pH = 4 _ ML

570 _ 600

_ _ 1,9 .104

_ _

Pophyrin (TPP) Pophyrin (TPPS3)

414

4,7 .105

Ag, Hg, Zn > 10g; Pd > 5g

Zn

434

4,8 . 105

Mt s thuc th hu c to phc vi Cu

pH = 3 - 6
Pophyrin (T(3MPy)P)

ML

419

2,1 .105

pH = 6

ML

434

3,5.105

Pophyrin (T(4pH > 4.5 MPy)P)

ML

446

2,46.105

Pd (II) c che bng KI sau khi chit vi Chelex 100 Co (II); In; Pd(II); V(V) Sau khi tch bng Dithizone

Mt s thuc th hu c to phc vi Cu pH = 4.1 5.9 + acid L ascorbi c

Pophyrin (TTMAPP)

ML

411

5,1.105

pH = 9 Natridiethyldithi (trong o carbamate CCl4)

Nu

436

13.103

Olive Thiothenoyltriflu pH = 2 ML2 338 oro acetone xanh

5,6.103

Mt s thuc th hu c to phc vi Cu

Natri dietyldithiocacbamat

Porphyrin

Dithizone

Natri dietyldithiocacbamat

Danh php: Cupral, mui Carbamidat DDTC Natri

Natri dietyldithiocacbamat

c tnh : Thuc th ny thng l mt mononatri, mui trihydrate, dng tinh th khng mu. Dng mui khan nng chy 9496oC v tan t do trong nc (35g/100ml 20oC) to ra phn ng kim. dng rn th rt bn nhng trong dung dch acid th b phn hy rt nhanh. Hu nh khng tan trong dung mi phn (0.006g/100ml trong CCl4), nhng tan trong ru. cc

Natri dietyldithiocacbamat
Phn ng to phc v c tnh ca phc DDTC c xem nh l mt anionic phi t 2 nhnh ha tr 1 nhn 2 nguyn t sulfur v to thnh nhng kt ta c mu vi hn 30 nguyn t ti pH > 4. Phn ng xy ra c chn lc hn trong dung dch acid vi s u tin i vi ion kim loi. Chng hu ht khng c in tch dng phc bo ha phi tr v c th tch chit bng dung mi hu c nh Chloroform hay Tetrachloride.

Natri dietyldithiocacbamat

Phn ng to phc vi Cu

DDTC l mt phi t 2 nhnh ha tr I nn khi cho thuc th vo dung dch cha ion Cu2+ th DDTC to thnh ion Na+ v ion m nh trn hnh, ion m tc dng vi ion Cu2+ to thnh phc mu nu v c th xc nh nguyn t ny bng phng php o quang.

Natri dietyldithiocacbamat

ng dng trong ha phn tch:

c s dng nh mt cht to ta v l dung mi thuc th tch chit cc ion kim loi nh. Cng nh c s dng lm thuc th trc quang cho Bi, Cu, Ni v mt s kim loi khc.

Porphyrin
Porphyrin l tn gi ca hp cht vng porphin. Cng thc cu to

Porphyrin

Xt thuc th tetraphenylporphin tetrasulfonic acid (TPPS4) ng vi gc R l

CTPT: C44H42N8S4O12.12H2O
Cng thc vit tch ra: (H2L)(NH4)4.12H2O

Porphyrin
c tnh ca thuc th Dng tinh th hnh kim im nng chy 300oC Thng hoa t 232 262oC Bn trong khng kh, khng tan trong nc (c th tan nu c mt mt cht hot ng b mt nh natri lauryl sulfate 5%)v cn, d tan trong chloroform, benzen. Hp thu tt bc sng 438nm (pH < 3.7) hoc bc sng 418nm (pH < 4.5)

Porphyrin
Phn ng to phc v tnh cht ca phc

Thuc th porphin to phc bn chealate dng 1:1 vi ion ca kim loi Cu

Cu trc Cu (II) chealate ca TPPS4

Porphyrin

Tc to phc hi chm, nht l khi hm lng ion kim loi thp. Tuy nhin tc c th tng nu c thm tc nhn xc tc (imidazole C3H4N2 hoc bipyridine)

Porphyrin
ng dng trong phn tch

L thuc th c nhy cao dng xc nh Cd, Co, Cu(II), Fe(II), Hg(II), Mg, Mn(II), Ni, Pb, Pd (II), Zn v mt s kim loi khc TPPS4 b phn ly bi KBrO3 vi s c mt ca Ru(III) dng vt c th xc nh Rb nng rt thp (10-10 M)
C th xc nh kim loi da vo s xut hin hunh quang trong phc ca thuc th porphyrin (Mg, Zn) hoc s tt hunh quang bi cc kim loi Co(II), Cu(II), Pb, Pd(II)

Dithizone

Danh php: Dithizone hay cn gi l 1,5 diphenylthiocarbazone; n,n-diphenyl-Cmercaptoformazane; phenylazothio-formic acid 2phenylhydrazide

c tnh ca thuc th Dng bt tinh th mu tm en, c nh kim, im nng chy 165oC-169oC, thng hoa 40oC 123oC.

Thc t khng tan trong nc pH < 7 (5 7,2.10-5g/l) nhng tan hon ton trong kim (pH > 7; >20g/l) c mu vng ca ion dithizoneate (HL-) v tan nhiu trong dung mi hu c khc.

Phn ng to phc v tnh cht ca phc Dithizone cho phi t S, N nn u tin phn ng vi cc kim loi nh Phc to thnh gia ion kim loi v dithizone c cu trc nh sau

 Nhng phc ny tan trong dung mi hu c nh chloroform hoc carbon tetrachloride. p dng i vi kim loi Cu, khi tc dng vi dithizone, Cu2+ s lin kt cng ha tr vi 2 phi t S ng thi nhn 2 lin kt phi tr t 2 phi t N, phc Cu vi Dithizone c cu trc nh sau:

Trong trng hp kim loi d hoc pH qu cao, Cu2+ s to phc ph vi Dithizone, khi 2 ion Cu2+ s lin kt vi 2 ion dithizoneate, trong 1 ion Cu2+ s lin kt cng ha tr vi 2 phi t N v nhn 2 lin kt phi tr t phi t S; chiu ngc li, 1 ion Cu2+ s lin kt cng ha tr vi 2 phi t S v nhn 2 lin kt phi tr t phi t N. phc ph c cu trc nh sau

ng dng trong phn tch

Dithizone c s dng rng ri trong phng php chit trc quang xc nh cc kim loi nng nh Cd, Cu, Pb, Hg, Zn v c tnh chn lc v nhy cao

Thuc th vi ion kim loi ch

Tnh cht vt l L mt kim loi bn, d un, mu xm, mi ct c mu sng sau xm dn do to thnh lp Pb2O (sous oxide), d = 1,37, chy 3250C, bc hi 5500C, hi ch c v ngt. im nng chy im si 600,61 K (621,43 F) 2.022 K (3.180 F) 18,26 10-6 m/mol 179,5 kJ/mol 4,77 kJ/mol

Th tch phn t
Nhit bay hi Nhit nng chy p sut hi Trng thi trt t t Vn tc m thanh

100.000 Pa ti 2.027 K nghch t

1.190 m/s ti r.t K

Thuc th vi ion kim loi ch

Tnh cht ha hc ca ch

Cu hnh Ch : [Xe]4f145d106s26p2 Cu hnh in t ny cn phi to nhng phc bn vng nht vi nhng phi t phn cc mnh. C nhng in t 6s2 ca ion Pb2+ lm trng thi ha tr II ca ch trong cc hp cht bn hn rt nhiu so vi trng thi ha tr IV do nhng hp cht loi tetra axetat ch u l nhng cht oxy ha mnh
Cu trc tinh th lp phng tm mt m in 2,33 (thang Pauling) Nhit dung ring 128,61 J/(kgK) dn in 4.807,7 /m dn nhit 28,9 W/(mK

Thuc th vi ion kim loi ch

Bng tm tt tnh cht ha hc ca ch
S ch Phn loi kim loi Nhm , Chu k, Khi Khi lng ring cng B ngoi Khi lng nguyn t Bn knh nguyn t (calc.) Bn knh cng ho tr Bn knh van der Waals Trng thi xi ha (xt) 82 yu,kh mm 14, 6, p 11.340 kg/m 1,5 trng xm 207,2(1) .v.C 180 (154) pm 147 pm 202 pm 4, 2 (lng tnh)

Thuc th vi ion kim loi ch

STT 1 2 3 4 5 6 7 8 9 10 11 12 13 TN THUC TH Eriocrom en T Xylen da cam Pyridin (NH4CNS) Mecaptobenzothiazol 8-Hydroxyquinolin Axit salixylic hoc salyxilat natri Thiour Galoxyanin Hematoxylin iphenylthiocacbazon (ithizon) Rodizonat natri Tetrametyldiaminodiphennylmetan sunfacsazen Phng php mu v phng Phng php trng lng v kt ta NG DNG Phng php th tch

php o mu

14
15 16 17

i--naphtolthiocacbazon
1-(2-pyridilazo)- 2- naphtol (PAN) Benzidin + (H2O2) Rodizonat natri Phn ng git

18

Axetat ng + axit axetic + (KNO3)

Phn ng tinh th

Thuc th vi ion kim loi ch

1
2 3

Dithizonat

1-(2-pyridilazo)- 2- naphtol (PAN)

Xilen da cam (XO)

Dithizonat
Dithizone hay cn gi l 1,5diphenylthiocarbazone, n,ndiphenylC mercaptoformazane, phenylazothioformic acid 2phenylhydrazide. Cng thc

Dng bt tinh th mu tm en c nh kim, im nng chy 165o C n 169oC, thng hoa 40 n 123oC (0,02 Torr). Thc t khng tan trong nc pH nh hn 7 (5 n 7,2.10 -5 g/l), nhng tan hon ton trong kim (pH >7, > 20 g/l) c mu vng ca ion dithizoneate (HL - ) ( max = 470 nm, = 2,2.10 4 ) v tan trong nhiu dung mi hu c khc.

Dithizonat
Ph ca dithizone trong nhng loi dung mi hu c biu din thnh hai di ph kh r m n c quan h ti hin tng h bin thione (1) v thiol (2). Ph hp th ca dithizone (H2L) trong carbon tetrachloride, ion dithizonate (HL- ) trong nc, v mercury dithizoneate [Hg(HL)2] trong tetrachloride biu din trong hnh (2).

Dithizonat
ng dng iphenylthiocacbazon (ithizon), l thuc th truyn thng c s dng rt rng ri xc nh lng vt ch mt cch chc chn da vo phn ng vi ithizon Mc d phc ch - ithizon cho ta mt phng php kh nhy ( = 520 nm, h s hp th mol phn t = 65 000), nhng iu kin khng thun li l s quang ho dung dch ithizon v phc khng tan c trong nc. Nguyn tc : Mu dung dch sau khi hiu chnh pH v thm cc cht b tr cn thit, lc lin tc chia carbon tetrachloride hoc chloroform ca dung dch dithizone n khi tt c kim loi bt u tch ra. Giai on cui cng ca qu trnh chit, mu ca dung dch dithizone cn li l mu xanh l cy.

Dithizonat
C ch Ion Pb2+ phn ng vi dithizone c minh ha trong hnh di . Phc ny tan trong cc dung mi hu nh chloroform hoc carbon tetrachloride. Cu trc chnh ca dithizonate cho ion kim loi tetra coordinate ha tr II c th trnh by nh sau

Dithizone c th c di chuyn d dng trong dung dch carbon tetrachloride hn trong dung dch chloroform. Bn cnh kh nng thay i phc chnh thnh phc ph do s ty ra ca kim. V th, trong thc t khng th loi b dithizone tha mt cch trit khng hnh thnh vi phc ph.

Dithizonat

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Thuc th 1-(2-pyridilazo)- 2- naphtol (PAN).

Cng thc

Khi lng phn t: M = 249,27. - Cng thc phn t ca PAN: C15 H11ON3
Gm hai vng c lin kt vi nhau qua cu -N = N- , mt vng l pyridyl , vng bn kia l vng naphtol ngng t PAN l thuc th hu c c dng bt mu , khng tan trong nc, tan tt trong ru v axeton. V c im ny m ngi ta thng chn axeton lm dung mi pha PAN. Khi tan trong axeton c dung dch mu vng hp th bc sng cc i max = 470nm, khng hp th bc sng cao hn 560nm. Tu thuc vo pH ca mi trng m thuc th PAN c th tn ti cc dng khc nhau, n c ba dng tn ti H2R+ , HR v R- v c cc hng s phn ly tng ng: pK 1 = 2,9 v pK 2 = 12,1.

Thuc th 1-(2-pyridilazo)- 2- naphtol (PAN).

ng dng nh lng ch bng 1-(2-pyridilazo)- 2- naphtol vi s c mt ca cht hot ng b mt khng in li bng phng php trc quang. C ch PAN l mt thuc th n baz tam phi v, cc phc to c vi n c kh nng chit v lm giu trong dung mi hu c nh CCl 4 , CHCl 3 , ru isoamylic, ru isobutylic, ru n-amylic, ru n-butylic,. C th m t dng phc ca n vi kim loi nh sau:

+ Pb

Thuc th 1-(2-pyridilazo)- 2- naphtol (PAN).

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Thuc th 1-(2-pyridilazo)- 2- naphtol (PAN).

Bng so snh bc sng hp th cc i ca PAN v ca phc aligan

Kt qu cho thy pH = 7,80 thuc th PAN hp th cc i bc sng 470 nm. Khi c s to phc aligan th c hin tng chuyn bc sng cc i t 470 nm n 550 nm, max = 80 nm, ng thi mt quang tng, mt khc mt quang ca phc aligan (PAN-Pb2+-CCl3COO) ln hn rt nhiu so vi phc nligan (Pb2+-PAN). iu chng t c s to phc aligan trong h PAN-Pb2+-CCl3COO Nh vy phc aligan hp th bc sng ti u l 550 nm.

Thuc th 1-(2-pyridilazo)- 2- naphtol (PAN).

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Xilen da cam
Xilen da cam (XO) c tng hp u tin vo nm 1956, c cng thc nguyn l C31H32O13N2S, khi lng phn t l 672,67 vC, nng chy 1950C. Cng thc cu to l :

o XO l mt axit su ln axit H6In (pK 1 = 1,15; pK 2 = 2,58; pK 3 = 3,23; pK 4 = 6,4; pK 5 = 10,46; pK 6 = 12,8)

Xilen da cam
Trong dung dch nc mu XO thay i: C 10 -3 :dung dch c mu C <10 -3 : dung dch c mu hng pH = 1 5: dung dch c mu vng pH > 7: dung dch c mu tm Nng cng cao, pH cng ln th cng mu cng ln. S thay i mu sc ca XO c gii thch do s tch H+ cc v tr khc nhau Thng dng XO dng mui Natri: C31H28O13N2SNa 4 , khi lng phn t l 760,59 vC. XO kt tinh l cht c mu nu sm, d tan trong nc d ht m, khng tan trong ru etylic

Xilen da cam

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Xilen da cam
ng dng XO l thuc th truyn thng c s dng rng ri xc nh cc kim loi Dng xilen da cam xc nh ch trong l cy bng phng php trc quang C ch Pb(II) phn ng vi XO pH = 5,0 6,0 trong mi trng m axetat chuyn mu t - vng nhng thy phn pH > 6

Nguyn t Crom
Tnh cht vt l ca Cr Crom l mt kim loi cng, mt bng, mu xm thp vi bng cao v nhit nng chy cao. N l cht khng mi, khng v v d rn. Cc trng thi xi ha ph bin ca crom l +2, +3 v +6, vi +3 l n nh nht. Cc trng thi +1, +4 v +5 l kh him. Cc hp cht ca crom vi trng thi xi ha +6 l nhng cht c tnh xi ha mnh. Trong khng kh, crom c xy th ng ha, to thnh mt lp mng xt bo v trn b mt, ngn chn qu trnh xi ha tip theo i vi kim loi pha di.
im nng chy im si Th tch 2.180 K (3.465 F) 2.944 K (4.840F) 1,843 x 10-6 m/mol

phn t Nhit bay

hi Nhit nng chy p sut hi Trng thi trt t t Vn tc m thanh

339,5 kJ/mol

21 kJ/mol 100.000 Pa ti 2944 K Phn st t 5.940 m/s ti 293,15K

Tnh cht ha hc ca Cr
S Cu hnh Phn loi kim loi Nhm, Chu k, Khi Khi lng ring 24 [Ar]3d54s1 Kim loi chuyn tip ,6,4, d 7.150 kg/m

cng
B ngoi Khi lng nguyn t Bn knh nguyn t(calc.) Bn knh cng ho tr

8,5
Kim loi mu trng bc 51,9961(6) .v.C 140 (166) pm 127 pm

Trng thi xi ha (xt)

6,4,3,2 (lng tnh)

Tnh cht ha hc ca Cr
Crm c th tn ti trng thi s oxy ha II,III, VI nn d dng tch n khi cc nguyn t cn. V d nh: oxy ha bng H2O2 hoc brm, Cr(III) n Cr(VI) trong

dung dch natri hydroxyt v sau lc th c th tch nhiu kim loi khi crm. Vic
tch tip theo (v d dung dch Natri hydroxyt v natri cacbonat d to Cr(OH)3 khng tan. Nu nh crm tn ti lng khng ng k th c th kt n vi hydroxyt st ba. CrO3, CrO42- (u l nhng cht oxy ha mnh) v CrO2Cl2 bay hi u l nhng hp cht ca Cr(VI). xc nh trc tip crm ngi ta s dng tnh hp th ca CrO42- trong dung dch kim 366nm. Phn ng gia Cr(VI) v Cis-diphenylcacbazit

trong mi trng axit l phn ng nhy nht xc nh crm nhng bn cht ca

cation mu tm to thnh b chit bng cc dung mi hu c cn cha c nghin cu..

Tnh cht ha hc ca Cr

Ngoi nhng hp cht ca Cr(VI) c cu hnh t din, phn ln nhng phc ca crm c cu to bt din v trong trng hp ca Cr(II) cu hnh b bin dng do hiu ng Jahn-Teller. Nhng hp cht ca Cr(II) (d4) thu c khi kh nhng hp cht ca Cr(III) (bng Zn). Nhng

hp cht ny d b oxy ha n Cr(III) v d nh bng oxy ca khng

kh. S n nh ha bi trng phi t to iu kin thun li cho s to phc vi nhng phi t nh , dipyridin, etylendiami, ion tioxyanat v xyanua.

Cc thuc th ca ion Cr
Cc thuc th hu c phn ng to phc phenylfluorone iu kin to phc T l max(nm) Gii hn xc nh (ppm) 0,01- 1,7

pH=1,5;etanol

1:1

500

Oxine -5-sunfonic acid

Diphenylcacbazit

pH= 6-8

1:3

420

0,5 - 8

pH= 3-5 ;etanol

1:3

540

0,005-1

Mt s thuc th to phc vi ion Crom

. Oxine5sulfonic Acid:
CTPT : C9H7NOS KPPT : 225,22

Oxine5sulfonic Acid
Cc tnh cht ca thuc th: dng tinh th bt mu vng. D dng ho tan trong nc; pKa

(N+H) = 4,10 v pKa (OH) = 8,76 ( 0,250).

ng dng: Thuc th ny c dng lm thuc th trc quang cho rt nhiu ion kim loi hoc nh mt thuc th hunh quang (Al, Cd, Ce(IV), Ga, In, Mg v Zn) cho ion kim loi trong dung dch nc.Cr(3) to phc vi thuc th pH = 6 8 ,vi t l 1:3 vi thuc th:

Oxine5sulfonic Acid

Diphenylacbazit (1,5 diphenylcacbohidrazit)

. Tnh cht : CTPT : C13H14ON4 Khi lng phn t : 242,28 Nhit si : 172 1750C

L cc tinh th nh hu nh khng mu hoc mu hng nht .Mu sm li khi ngoi khng kh .t tan trong nc (k c nc nng) .Khng tan trong

ete v clorofom .Tan trong ru etylic (khi un nng) ,trong aceton,v acid
acetic bng.

Diphenylacbazit (1,5 diphenylcacbohidrazit)

ng dng ca thuc th: Dng xc nh Cr3+ ; Hg2+ ; Pb2+ trong o quang: Crmat v icrmat phn ng vi thuc th diphenylcacbazit to thnh phc mu tm c hp th cc i ti bc sng 540nm rt thun li cho vic so mu.:

Lm ch th oxy ha kh trong php nh phn dicromat Phn tch nh tnh Cl- ; Cr6+; Cu2+ ; Fe3+

Diphenylacbazit (1,5 diphenylcacbohidrazit)

Cc ion cn tr: Cc ion Hg2+, Hg22+( khi hm lng ln hn 200mg/l), vanadi v

molipden( VI) cng c kh nng phn ng vi thuc th to

thnh hp cht c mu, song nhng cht ny thng c rt t trong nc. St (ln hn 1mg/l) cng phn ng c vi thuc th to thnh hp cht c mu vng nu ,nhng ta c th loi tr nh hng ca st bng cch thm vo dung dch mt lng axit photphoric. Nu trong mu c mt lng ln Mangan th khi oxi ha bng

pesunfat trong mi trng kim hoc trung tnh, n s to thnh

kt ta Mangan oxit, khi ta lc b bng bng thy tinh hay phu thy tinh.

Diphenylacbazit (1,5 diphenylcacbohidrazit)

Nu trong nc c mi trng kim hay trung tnh th kh xc nh ring Cr(III) v Cr(VI). Bi v khi oxi ha, nu trong dung dch c cht kh

(thng l Fe2+, sunfit v cc cht hu cth Cr(VI) s kh xung Cr(III).

Trong trng hp ny ch nn nh tng hm lng Crm. Mun xc nh Cr(VI) v Cr(III) th ta phi tch ring Cr(III) bng cch kt ta n bng magi oxit ( pH = 10.5-11). Khi Cr(OH)3 gp li trn b mt magie oxit, cn Cr(VI) li trong dung dch. Lng ln cht hu c, cc cht kh v ion clorua khng cn tr php xc nh. Ngoi ra, Cr(VI) cn c xc nh di dng phc mu ta vi o- nitrophenyl floron v

bromua axetyltrimetl amoni, hp th cc i bc sng 582nm.

GECMANI

Tnh cht vt l Tnh cht ha hc Thuc th Ge4+

2
3

GECMANI
im nng chy

TNH CHT VT L
Gecmani l mt nguyn t mu trng nh xm, cng c nc bng kim loi v cu trc tinh th tng t nh kim cng. Ngoi ra, mt iu quan trng cn lu l gecmani l cht bn dn, vi cc tnh cht in nm gia cc kim loi v cc cht cch in. trng thi nguyn cht, kim ny l cht kt tinh, gin v duy tr bng trong khng kh nhit phng

1.211,4 K (1.720,85 0F) 3.106 K (5.131 F) 13,63 10-6 m/mol 334 kJ/mol 36,94 kJ/mols 10 Pa ti 1,814 K nghch t 5.400 m/s ti 293,15 K

im si Th tch phn t Nhit bay hi Nhit nng chy p sut hi Trng thi trt t t Vn tc m thanh

GECMANI
TNH CHT HA HC Cu hnh Ge : [Ar]3d104s24p2
S Phn loi kim loi Nhm, chu k, khi Khi lng ring cng B ngoi Khi lng nguyn t Bn knh nguyn t Bn knh cng ha tr Trng thi oxi ha 32 kim 14, 4, p 5.323 kg/m 6.0 trng nh xm 72,64(1) .v.C 125 (125) pm 122 pm 4 (lng tnh)

GECMANI
THNG TIN KHC 1. 2. 3. 4. 5. m in 2,01 (thang Pauling) Nhit dung ring 319,68 J/(kgK) dn in 0,6.100 /m dn nhit 60,2 W/(mK) Nng lng ion ha 762,0 kJ/mol ,1.537,5 kJ/mol ;3.302,1 kJ/mol

THUC TH VI Ge

PHENYLFLUORONE
CTPT: C19H12O5 Mol wt = 320.30

HO

OH

HO

PHENYLFLUORONE
Tn gi khc: _ 2,3,7Trihydroxy9phenyl6fluorone _ 2,6,7trihydroxy9phenylisoxanthene3one Ngun gc v phng php tng hp y l thuc th c gi tr v mt kinh t. N c tng hp bi phn ng 1,2,4benzenetriol vi benzotrichloride Tnh cht ca thuc th _ Phenylfluorone l mt tinh th bt mu cam, c nhit nng chy ln hn 300oC. Xut hin hunh quang mu hi lc trong dung dch cn pH=8. Trong dung dch kim, thuc th phn ly yu. _ t tan trong nc (3.10-7M trong 20% ethanol, 25oC), t tan trong ethanol lnh, nhng d tan trong cn b acid ho (HCl v acid H2SO4). N c th kt tinh li t cn b acid ho vi s c mt ca ammoniac.Nhng mu thng mi thng c tinh khit khng tho mn.

PHENYLFLUORONE
ng dng trong phn tch N c dng nh thuc th o quang v nhy, c tnh chn lc vi Ge v Sn; ngoi ra thuc th cn dng xc nh Co, Fe, In, Mo(VI), Nb, Ti v Zr bng phng php o quang. Phn ng to phc cht v tnh cht ca phc cht Phenylfluorone phn ng vi mt s ion kim loi to thnh chelate c mu khng ho tan. Trong dung dch acid 0,1M, Ge (IV) to phc c mu vi t l 1:2 xy ra theo phng trnh: Ge(OH)4 + 2H3L [ Ge(OH)2(H2L)2 ] + 2H2O

PYROGALLOL RED

(C19H12O8S)

PYROGALLOL RED

(C19H12O8S)

Danh php: PR: Pyrogllolsulfonephthaline Ngun gc v phng php tng hp PR c tng hp bng phng php ngng t o-sulfobenzoic anhydride vi pyrogallol Tnh cht thuc th: _ L tinh th dng bt mu sm khi kt hp vi kim loi sng t tan trong nc, alcohol v trong dung mi hu c khng phn cc. _ Trong mi trng acid mnh c mu cam, mu trong mi trng trung tnh, mu tm trong mi trng kim. ng dng trong phn tch: _ L ch th kim loi cho qu trnh chun chelate ca Bi, Co (II) , Ni, Pb. PR cng c dng nh ch th trong phng php trc quang i vi mt s kim loi nng

_ S dng nh thuc th trc quang: Nhng Ion kim loi c th xc nh bng phng php trc quang vi PR nh Ag, Cu (II), Ga, Ge, In, Mo (VI), Ti (III)

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REZARSON
CTPT: C12H10N2O6AsCl KLPT = 388,60 Rezarson to phc mu theo t l 1:1 vi nhiu kim loi, bao gm Cu, Ga, Ge, Ni, Pd v Sn trong nc acid trong bnh vi methanol t 50 70 %. N c ngh nh mt thuc th trong php o trc quang cho Ge v Sn (trong dd HCl, max = 510nm).

REZARSON
TO PHC VI Ge

REZARSON
TO PHC VI Ge

Bng tm tt thuc th ca Ge
Thuc th iu kin (pH) T l max (nm) Cc ion (x104) cn tr Gii hn cho php (ppm) 0,05 0,5

Phenylfluorone

Pyrogallol Rezarson

HCl 0.1M, chit vi Carbon Tetrachlorid e 5 HCl vi methanol 50-70% 0,5 4,5

ML2

508

14,5

ML2 ML

500 510

0,28 ~ 2 -

Bromopyrogallor

ML3

550

3,8

GALI

1. Tnh cht vt l
2. Tnh cht ha hc 3. Thuc th Ga3+

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GALI
TNH CHT VT L
L mt kim loi yu mu bc nh kim, gali cng v gin nhit thp nhng ha lng rt d dng, ch cao hn nhit phng mt cht (29,8C) v v th n s nng chy khi nm trong lng bn tay ca ngi. N xut hin di dng du vt trong bxt v qung km
im nng chy im si Th tch phn t Nhit bay hi 302,9146 K (85,5763 F) 2.477 K (3.999F) 10-6 m/mol 254 kJ/mol 5,59 kJ/mol 10 Pa ti 1,448 K nghch t

Nhit nng chy

p sut hi Trng thi trt t t

Vn tc m thanh

2.740 m/s ti 293,15K

GALI
TNH CHT HA HC
Cu hnh Ga : [Ar]3d104s24p1
31 Kim loi yu 13, 4, p 5910 kg/m 1,5 Kim loi mu bc nh kim 69,723(1) .v.C 130 (136) pm 126 pm 187 pm 3,1 (lng tnh)
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S Phn loi kim loi Nhm, Chu k, Khi Khi lng ring cng B ngoi Khi lng nguyn t Bn knh nguyn t (calc.) Bn knh cng ho tr Bn knh van der Waals Trng thi xi ha (xt)
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GALI
THNG TIN KHC
1. 2. 3. 4. 5. m in 1,81 (thang Pauling) Nhit dung ring 370,90 J/(kgK) dn in 6,78.106 /m dn nhit 40,6 W/(mK) Nng lng ion ha 578,8 kJ/mol , 1.979,3 kJ/mol ; 2.963 kJ/mol

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THUC TH VI Ga3+
PYROCATECHOL TM
CTPT: C19H14O7S KLPT: 386,38 Tn gi khc: 3,3,4Trihydroxyfuchsone 2sulfonic acid, Catechol sulfonephtalein, Catechol tm, PV

Tng hp t s ngng t ca osulfonephthalein anhydrit vi pyrocatechol

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THUC TH PYROCATECHOL TM
TNH CHT THUC TH

L loi bt nu thm c nh kim loi mu xanh dng. N rt ht m, v th nn bo qun tht kn. Sn phm thng mi thnh thong c mi v acid acetic m khng hon ton loi b c t s kt tinh dung mi. N tan t do trong nc v cn pha trong nc, t tan trong cn nguyn cht lnh hoc acid acetic bng v khng tan trong dung mi khng phn cc chng hn: benzene, xylene,
NG DNG TRONG PHN TCH

S dng nh l cht ch th kim loi trong chun to phc Xc nh Ga, Fe, Al, Cu v.vv theo phng php so mu
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THUC TH PYROCATECHOL TM
TO PHC VI Ga

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THUC TH CHROMAZUROL S

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CHROMAZUROL S
COOH
Cng thc tng qut: C23H16O9Cl2S OH 3-sulfo-2,6-dichloro-3,3-dimethyl-4hydroxyfuchson-5,5dicarboxylic acid. Ngun gc v phng php tng hp Chromazurol S l tn thng mi ca thuc H3C nhum c sn xut bi tp on Geigy; loi thuc nhum ny l mt loi thuc th c ng dng rng ri. Chng ch yu dng mui trinatri. N c tng hp bng s ngng t ca sulfoodichlorobenzaldehyde cng 2,3 cresotic acid, km theo qu trnh oxi ha.

COOH
O

Cl

Cl

SO 3H

CHROMAZUROL S

c im -Dng thng mi C23H13O9CL2SNa3.2H2O l bt mu nu . -C kh nng ht m v d ha tan trong nc. -Trong dung dch nc: pH = 3-4 c mu cam. pH = 4 c mu vng. B acid ha pH < 0 to thnh ta dng t do H4L v li b ha tan trong dung dch acid hn (pH< -0.3).

CHROMAZUROL S
NG DNG TRONG PHN TCH
Chromazurol S c dng lm ch th kim loi trong phng php chun phc cht xc nh Al, Ba, Ca, Fe, Mg, Ni v Th; v cng l thuc th trc quang cho nhiu ion kim loi khc nhau nh l: Al, Be, Ce, Co, Cr, Cu, Fe, Ga, Hf, In, La, Mn, Mo, Ni, Pd, Rh, Se, Th, Ti

THUC TH PYROGALLOL RED (C19H12O8S)

THUC TH PYROGALLOL RED (C19H12O8S)

Danh php: PR: Pyrogllolsulfonephthaline Ngun gc v phng php tng hp PR c tng hp bng phng php ngng t o-sulfobenzoic anhydride vi pyrogallo Tnh cht thuc th: _ L tinh th dng bt mu sm khi kt hp vi kim loi sng t tan trong nc, alcohol v trong dung mi hu c khng phn cc. _ Trong mi trng acid mnh c mu cam, mu trong mi trng trung tnh, mu tm trong mi trng kim. ng dng trong phn tch: _ L ch th kim loi cho qu trnh chun chelate ca Bi, Co (II) , Ni, Pb. PR cng c dng nh ch th trong phng php trc quang i vi mt s kim loi nng

Phn ng to phc ca Ag-Phen-BPR

_ S dng nh thuc th trc quang: Nhng Ion kim loi c th xc nh bng phng php trc quang vi PR nh Ag, Cu (II), Ga, In, Mo (VI), Ti (III)

Thuc th Oxine5sulfonic Acid

CTPT: C9H7NOS KLPT = 225,22 dng tinh th bt mu vng. D dng ho tan trong nc; pKa (N+H) = 4,10 v pKa (OH) = 8,76 ( 0,250). Chelate c tnh tng t nh oxine, nhng chelate khng ho tan trong nc. Do , thuc th ny c dng nh l thuc th hunh quang cho ion Ga3+ trong dung dch nc

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Thuc th Oxine5sulfonic Acid

TO PHC VI Ga

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THUC TH REZARSON
CTPT: C12H10N2O6AsCl KLPT = 388,60 Rezarson to phc mu theo t l 1:1 vi nhiu kim loi, bao gm Cu, Ga, Ge, Ni, Pd v Sn trong nc acid trong bnh vi methanol t 50 70 %. N c ngh nh mt thuc th trong php o trc quang cho Ge v Sn (trong dd HCl, max = 510nm).

THUC TH REZARSON
TO PHC VI Ga

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Bng tm tt thuc th
Thuc th iu kin (pH) T l max (nm) 570 580 565 (x104) 11,4 ~ 7,3 10,7 Cc ion cn tr Gii hn cho php (ppm) 2 60

Phenylfluorone pyrocatechol tm diketonate

pH 8,0 9,0; CPB(X) pH 6,05 6,4 pH 4,5 6,0, Rhodamine B, chit vi xylene 4,5 pH 3,0 ~11,7 pH 3 ~ 3,5

ML2X2 ML2 -

pyrogallol Oxine5 sulfonic Acid Rezarson

ML ML3 ML

530 393 550

1,4 6,47 -

Ce(IV), Cu, Fe,Tl(III),U22+ nh hng.

0,28~4,8 3,5~10 0,4 ~ 5,6

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