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NH4
Phn tch nh tnh o - t + OH NH3 + H2O co kh mui khai sinh ra lam xanh quy tm
Pb
2+
+ CrO4
2-
2. Cc yu cu ca ha phn tch
Pht trin ngang tm vi cc ngnh KH khc C kin thc v cc mn khoa hc t nhin v tin hc nm vng nguyn tc ca phng php, pht trin pp mi trn cc cn bn c sn. C tnh cn thn, kin nhn, chnh xc, sch s, trung thc v kh nng phn on kt qu phn tch.
GV: Trn T Phng Tho HBK 12
PP vt l Pht hin v xc nh thnh phn cc cht da trn tnh cht vt l : quang, in, nhit, t...
PP ho l (PP PT dng c) Kt hp PP ha hc v vt l
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PHN LOI THEO LNG MU PHN TCH HAY K THUT PHN TCH
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a. Phng php ho hc
Cau t khao sat Phh
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a. Phng php ho hc
CH3
O...... H
N
2+
2+
NH3
N Ni
N H...... O
CH3
C CH3
N O
CH3
(TUA O SON)
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NH4OH
DMG
Blue solution
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b. Phng php vt l
Tnh cht vt l v thnh phn ho hc c mi lin quan vi nhau. PPVL khng dng phh PPVL s dng cc tnh cht vt l: quang, in, t, t trng.. nh tnh v nh lng cu t kho st.
GV: Trn T Phng Tho HBK 21
b. Phng php vt l
Xc nh t trng ca dd acid, baz, mui tra bng bit nng Xc nh chit sut ca tinh du nh gi s b thnh phn ha hc. Xc nh nhit nng chy, nhit si ca hp cht Da vo tnh tan, tnh hp ph nh tnh v nh lng: PP sc k
GV: Trn T Phng Tho HBK 22
c. Phng php ha l
Va kt hp PPHH v PPVL S dng dng c v thit b kh tinh vi, phc tp gi l PPPT dng c. Gm c: pp ph nghim, pp in ho, pp sc k v mt s pp khc.
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c. Phng php ha l
Thc hin phh Kt hp my o quang ph thy c o cng mu ca phc Nng Fe cng nhiu th cng mu cng tng.
Fe
3+
+ nSCN
[Fe(SCN)n]
(3-n)+
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c. Phng php ha l
Co
2+ +
nSCN
[Co(SCN)n]
(2-n)+
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Blue solution
Solution of Co2+ (5 -10 drops) + Amyl Alcohol (2 - 3 drops)
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NHN XT
PP VT L v PP HA L: khng cn ranh gii r rng. PPVL + PPHL: ghp chung thnh PP phn tch dng c.
GV: Trn T Phng Tho HBK 28
PP nghin
Mu phn tch v thuc th rn c nghin trong ci s Nguyn t cn pht hin s to hp cht mi vi thuc th Hp cht mi c tnh cht c trng: mu, mi nhn din.
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PP nghin
VD: Nghin mu vi vi KSCN, nu mu xut hin du hiu mu mu vi c cha st (III)
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to
PP nh git
Da vo hin tng mao dn v hp ph. P thc hin trn tm s, thy tinh, giy lc Giy lc: cht lng thm vo giy, sn phm mang mu to thnh b hp ph mt phn nh ca giy lm tng nhy ca p.
GV: Trn T Phng Tho HBK 34
PP nh git
Nhn bit [Fe(CN)6]4- v SCN- trong cng mt mu Giy lc tm FeCl3
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PP th nghim ngn la
Mt s kim loi pht ra bc x c mu c trng khi t trn ngn la xanh ca n kh. Na: la vng K: la tm Ca: la gch Ba: la lc
GV: Trn T Phng Tho HBK 36
2. Phn loi theo lng mu phn tch hay k thut phn tch
PPPT Th Bn vi lng Cch thc hin
Tch rn khi lng bng lc ly tm
Lng mu
(1-10g) hoc 1-10ml (10-3-1g) hoc 10-1-1ml 10-6-10-3 g 10-3-10-1 ml <10-6g <10-3ml
Dng c
50-500ml <50ml <1ml
knh hin vi Vi lng hay phn ng git knh hin vi in t Siu v mi trng GV: Trn T Phng vi lng Tho c bit HBK
37
4. Theo trng thi cht kho st Phn tch li t: mu dng dd Phn tch li kh: mu dng rn
GV: Trn T Phng Tho HBK 39
C + X?
A+B
DD chun
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Phn ng oxy ha kh
Phn ng to ta
Phn ng to phc
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3Cu + 8 HNO3
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Phn ng oxy ha kh
nh tnh
2Fe
3+
+ 2I
2+
+ 8H
+ 5Fe + 4H2O
3+
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Phn ng to ta
nh tnh: AgCl (ta trng), PbCrO4 (ta vng), AgBr (vng nht), AgI (vng) Fe3+ + K4[Fe(CN)6] kalihexacianoferat (II) Fe2+ + K3[Fe(CN)6] kalihexacianoferat (III)
GV: Trn T Phng Tho HBK
Phn ng to ta
nh lng: SO42- + BaCl2 BaSO4 + 2ClTch nhm: Vd: tch Ag+, Pb2+, Hg22+ ra khi hn hp dd ca chng vi Fe3+, Al3+, Zn2+ bng ion ClGV: Trn T Phng Tho HBK 51
Phn ng to phc
K hiu: [MLx]n+ M: thng l nguyn t kim loi chuyn tip (ph tng d cha lp y in t) Ligand L: nguyn t hoc nhm nguyn t c electron t do
GV: Trn T Phng Tho HBK 52
Mt s loi Ligand
CH2COOH
CH2COOH
CH2COOH
GV: Trn T Phng Tho HBK
COMPLEXON I
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Mt s loi Ligand
CH2COOH N CH2COOH
H2 C
H2 C
N CH2COOH
CH2COOH
COMPLEXON II (EDTA)
GV: Trn T Phng Tho HBK
acid EtylenDiaminTetraAcetic)
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Mt s loi Ligand
CH2COONa N CH2COONa
H2 C
H2 C
N CH2COOH
CH2COOH
COMPLEXON III
GV: Trn T Phng Tho HBK
(TRILON B)
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Phn ng to phc
Ho tan: AgCl + 2NH4OH [Ag(NH3)2]Cl + 2H2O Che cu t di dng phc bn: Vd: hn hp c Fe3+ v Co2+ u to phc vi SCN-, do nh tnh Co2+ phi che Fe3+ bng F- hoc C2O42- di dng phc FeF63- hoc Fe(C2O4)33GV: Trn T Phng Tho HBK 56
Phn ng to phc
nh tnh:
Fe
3+
+ nSCN
[Fe(SCN)n]
(3-n)+
Gii che:
GV: Trn T Phng Tho HBK
57
3. Yu cu ca phn ng HH
3.1. Yu cu ca P phn tch 3.2. Yu cu ca thuc th trong ho phn tch 3.3. Yu cu ca dd chun (thuc th c nng chnh xc)
GV: Trn T Phng Tho HBK 58
tinh khit cao H/ cht k thut X 99% H/ cht tinh khit (P): 99,0% X 99,9% H/ cht tinh khit PT(PA):
99,90% X 99,990% X 99,99% 99,999%
nhy cao - Gii hn pht hin : lng ti thiu ca X (g / ml) cn pht hin c bi thuc th. - long gii hn : th tch dung mi ti a (ml) dng ha tan 1 g cu t X m vn cn pht hin c X
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3.3. Yu cu ca dd chun C
Tr vi mi trng Dng bt mn c th cn chnh xc ti 0,1 - 1mg Phn t lng ln gim sai s khi cn
GV: Trn T Phng Tho HBK 64
1. Giai on chn mu
Phi c tnh cht i din cho ton l hng. Chn mu ring: chn ngu nhin cc v tr (n v) khc nhau ca l hng. Chn mu ban u: chn i din cc v tr (n v) khc nhau ca mu ring mu chung. Chn mu trung bnh: mu chung nghin ry trn
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1. Giai on chn mu
Mu trung bnh th nghim chia lm 3 phn: Ni giao hng gi Ni nhn hng gi Ni phn tch gi
GV: Trn T Phng Tho HBK 67
1. Giai on chn mu
Nu mu chung qu ln
GV: Trn T Phng Tho HBK 68
4. Kim chng kt qu v x l kt qu phn tch PTT: kim tra bng phn ng c hiu khc.
PTL: tnh ton theo d liu ghi nhn, biu din kt qu theo yu cu ca pp thng k.
GV: Trn T Phng Tho HBK 71
VD v cc giai on ca 1 PPPT
Yu cu: nh lng st trong mt mu vi. 1. Chun b mu th nghim: chn mu i din: mu TB th nghim. 2. Cn chnh xc m(g) mu ha tan bng acid thch hp lc mu nh mc thnh V(ml) 3. St trong dd l Fe3+: ty hm lng Fe3+ c th dng:
GV: Trn T Phng Tho HBK 72
VD v cc giai on ca 1 PPPT
Nu [Fe3+] > 10-3M: dng PP ha hc. PP phn tch khi lng PP phn tch th tch (chun oxy ha kh, chun to to phc vi EDTA) Nu hm lng st (III) qu b: Dng PP so mu (PP quang ph hp thu thy c). 4. Tnh kt qu theo yu cu v x l kt qu phn tch theo PPTK
GV: Trn T Phng Tho HBK
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VD: e xac nh ham lng SiO2; Al2O3, Fe2O3, CaO, MgO; K2O va Na2O trong mot mau cao lanh, ngi ta can 0,3000 g mau, chuyen vao chen Ni va them vao 3g KOH. Nung chay hon hp noi tren nhiet o thch hp, lam nguoi va hoa tan khoi ran thu c bang acid HCl. ?. Phng phap (PP) a c s dung e hoa tan mau?
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C cn 2 ln, lc ta SiO2; nung; cn v xc nh hm lng ca n trong mu. Dung EDTA e chuan o Al3+, Ca2+, Mg2+ ieu kien thch hp. Dung 1,10- phenanthroline tao phc o cam vi ion Fe (dang Fe2+ ) roi em o quang va so sanh vi cac dung dch cha Fe2+ a biet trc nong o. o cng pht x ca nguyn t K v Na trong mu ri so snh vi chun bit hm lng.
GV: Trn T Phng Tho HBK 75
??. Ten goi cua PP a c s dung e nh lng SiO2; Al2O3, Fe2O3, CaO, MgO; K2O va Na2O. Theo bn cht phng php Theo k thut phn tch Theo hm lng cht kho st (nu bit rng mu cha 55,19%SiO2; 24,4%Al2O3, 6,5%Fe2O3, 0,51%CaO, 1,07%MgO; 3,2%K2O & 0,10%Na2O).
GV: Trn T Phng Tho HBK 76