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PGS.TS. Nguyen c Tuan Bo mon Hoa Phan Tch Kiem Nghiem Khoa Dc ai hoc Y Dc TPHCM
Nguyen c Tuan
ai hoc Y Dc TPHCM
Nguyen c Tuan
ai hoc Y Dc TPHCM
M au
Tach la nhom cac phng phap hoa hoc, vat ly va hoa ly nham i t mot hon hp phc tap hon hp n gian tng chat Hon hp phc tap tach mot chat hoac mot nhom chat Dc: oi tng phan tch a dang kho xac nh trc tiep mot chat ma phai qua giai oan tach nh lng Tach co the dung e tinh che hoac nghien cu thanh phan cua mot hon hp
Nguyen c Tuan ai hoc Y Dc TPHCM
Nguyen c Tuan
ai hoc Y Dc TPHCM
V: the tch dung dch co n phan t d: Khoi lng rieng cua dung dch P: ap suat tham thau n/V = hdg/RT hay C = hdg/RT Tham tch: Mang tham thau cho cac phan t nho va trung bnh i qua Qua trnh ngoai tham
Nguyen c Tuan
- Hang so mot nhiet o xac nh va trong nhng ieu kien ly tng - ac trng cho mot chat tan va mot cap dung moi xac nh A va B - Phu thuoc vao nhiet o, ap suat, tnh chat cua chat tan va dung moi K cang ln, qua trnh chiet cang hieu qua V du: Fe3+ Pha A Ether etylic Ether etylic Pha B Nc + HF Nc + HCl K 0,001 99,0
Nguyen c Tuan
ai hoc Y Dc TPHCM
S2 (pha 2)
[S ] K = 2 K: he so phan bo [S ] 1
m q 1 - q1 la % S con lai trong pha 1, nong o S trong pha 1: V 1 (1 q ) m 1 - (1-q1) la % S c chiet sang pha 2, nong o S trong pha 2: V 2 (1 q ) m 1 V V 2 1 K= q = q m 1 V + KV 1 1 2 V 1
Nguyen c Tuan ai hoc Y Dc TPHCM
qn
V 1 = V + KV 1 2
q luon luon nho hn 1, sau n lan chiet nao ay tc la qn se vo cung nho va co the coi nh bang 0 V du: Chat tan A trong nc - benzen co K = 3, co nong o 0,01 M trong 100 ml dung dch nc
100 q1 = = 0,062 = 6,2% a) Chiet mot lan vi 500 ml benzen: (100 + 3500) 5 100 b) Chiet 5 lan moi lan vi 100 ml dung moi q5 = = 0,00098# 0,1% (100+ 3100)
ai hoc Y Dc TPHCM
Nguyen c Tuan
CB C
A
CB, CA: tong nong o cac dang khac nhau cua chat tan trong B va A
KD: khong bat buoc la hang so B la mot base hu c: BH+ ch ton tai trong pha nc Pha 1: pha nc Pha 2: pha DMHC BH+ <=====> B [ B] 2 D= [ B]1 + [ BH + ]1 + H+
D=
K Ka Ka + [H + ]
Nguyen c Tuan
ai hoc Y Dc TPHCM
CB C
A
CB, CA: tong nong o cac dang khac nhau cua chat tan trong B va A
KD: khong bat buoc la hang so HA la mot acid: A- khong ton tai trong pha hu c Pha 1: pha nc Pha 2: pha DMHC HA <=====> H+ + A-
[ HA]2 D= [ HA]1 + [ A ]1
q=
50 (3,0 1,0 10 9 ) q= = 0,65 = 65% b) pH = 8,00 D = = 0,273 9 8 (50 + 0,273 100) (1,0 10 + 1,0 10 )
D=
K Ka qn + Ka + [H ]
So sanh: pH 10,00 8,00
V 1 = V + DV 2 1
n
0 -2 Log D -4 -6
BH+ B
6 pH
10
12
Nguyen c Tuan
ai hoc Y Dc TPHCM
Q R=
Q AO
Nguyen c Tuan
ai hoc Y Dc TPHCM
1 R = 1 1+ k'
vi
VB k'= KD VA
Chiet lap: hieu suat chiet cao hn nhng ton nhieu thi gian, cong sc
1 K D VB 1 + n V A
n
Phong th nghiem: chiet gian oan hay chiet lien tuc Chiet ngc dong: hieu suat chiet rat cao, tach c nhieu chat
Nguyen c Tuan ai hoc Y Dc TPHCM
Nguyen c Tuan
ai hoc Y Dc TPHCM
Bc 1
U1mi L0
U0 L1mi
Bc 2
U2mi L0
U1 L1
U0 L2mi
Bc 3
U3mi L0
U2 L1
U1 L2
U0 L3mi
Nguyen c Tuan
ai hoc Y Dc TPHCM
Bc 2:
Nguyen c Tuan
ai hoc Y Dc TPHCM
Phan chia ngc dong cua A va B S: % A hoac B trong moi ong sau 5 bc
(A) 0,64 (A) 0,16 (A) 0,256 (A) 0,064 (A) 0,0768 (A) 0,0192 (A) 0,02048 (A) 0,00512 (A) 0,00512 (A) 0,00128 (A) 0,0064 (B) 0,25 (B) 0,25 (B) 0,25 (B) 0,25 (B) 0,1875 (B) 0,1875 (B) 0,125 (B) 0,125 (B) 0,078125 (B) 0,078125 (B) 0,15625 (A) 0,512 (A) 0,128 (A) 0,3072 (A) 0,0768 (A) 0,12288 (A) 0,03072 (A) 0,04096 (A) 0,01024 (A) 0,0512 (B) 0,125 (B) 0,125 (B) 0,1875 (B) 0,1875 (B) 0,1875 (B) 0,1875 (B) 0,15625 (B) 0,15625 (B) 0,3125
0 1 2 3 4 5 S*
(A) 0,8 (A) 0,2 (A) 0,16 (A) 0,04 (A) 0,032 (A) 0,008 (A) 0,0064 (A) 0,0016 (A) 0,00128 (A) 0,00032 (A) 0,000256 (A) 0,000064 (A) 0,00032
(A) 0,4096 (A) 0,1024 (A) 0,32768 (A) 0,08192 (A) 0,16384 (A) 0,04096 (A) 0,2048
(B) 0,0625 (B) 0,0625 (B) 0,125 (B) 0,125 (B) 0,15625 (B) 0,15625 (B) 0,3125
(A) 0,32768 (A) 0,08192 (A) 0,32768 (A) 0,08192 (A) 0,4096
(B) 0,03125 (B) 0,03125 (B) 0,078125 (B) 0,078125 (B) 0,15625
Nguyen c Tuan
ai hoc Y Dc TPHCM
Nguyen c Tuan
ai hoc Y Dc TPHCM
Vi:
Pha tren U di ong doc theo pha di L bat ong Pha tren goi la pha ong MP (Mobile Phase) Pha di goi la pha tnh SP (Stationary Phase)
Gia s A c chiet bang phan chia ngc dong theo s o tren. Phan oan A pha tren la p% va pha di la q%. Ta co p + q = 1
Nguyen c Tuan ai hoc Y Dc TPHCM
0 1
0 2
0 3
0 4
0 2
0 3
0 4
ai hoc Y Dc TPHCM
0 q2 0
p2 0 2 p3 p 2q 2 p3 0 3 p4 p 3q 3
0 3
0 4
0 3
0 4
Bc chiet n 1 2 3 4 ....
0 q q2 q3 q4 .....
So ong r 2
p3 4p3q .....
p4 ....
f=
n! pr qnr (n r)!r!
rmax # np
V du: A co p = 4/5, sau 100 bc chiet ta co rmax # 100 x 4/5 # 80: ong 80 B co p = , sau 100 bc chiet ta co rmax # 100 x 1/2 # 50: ong 50
Nguyen c Tuan
ai hoc Y Dc TPHCM
B
DA = 4 va DB = 7/3
Ong 59 - 72 Ong 81-90 38,90% 0,82%
DA = 4 va DB = 1
- Ong 70 - 90 hoan toan la A - Ong 40 - 60 hoan toan la B A B
Nguyen c Tuan
2,27% 66,06%
ai hoc Y Dc TPHCM
Nguyen c Tuan
ai hoc Y Dc TPHCM
N H N N C
N SH N N OH N O O NH4
Dithizone
Nguyen c Tuan
8-hydroxyquinolin
Cupferron
ai hoc Y Dc TPHCM
He so nay phu thuoc vao nong o cua ligand va pH cua dung dch
Nguyen c Tuan
ai hoc Y Dc TPHCM
N S N C N
N H +
+ 2H
C N N
SH
C6H5
Dithizone (xanh)
Khong mau
A (ml) 10 0 0 7 3 Xanh lam B (ml) 0 10 0 7 3 o
o
C (ml) 0 0 10 7 3 o
Ong nghiem Nc cat Nc may Dung dch Pb(NO3)2 2mM Hexan Dithizone/CHCl3 0,01% Lac yen e phan lp: Mau cua lp hexan
Nguyen c Tuan
ai hoc Y Dc TPHCM
cap ion tao thanh tac nhan tao cap ion (ion pair agent, IPA)
C s cua phng phap chiet o quang, acid mau, acid mau-base hu c ng dung trong kiem nghiem Chiet va o quang: chlorpheniramin, loperamid, promethazine Chuan o tao cap ion: dung dch chuan o la chat dien hoat anion dung nh lng alcaloid, ch th vang methyl, moi trng chloroform
Nguyen c Tuan ai hoc Y Dc TPHCM
Nguyen c Tuan
ai hoc Y Dc TPHCM
Nguyen c Tuan
ai hoc Y Dc TPHCM
Nguyen c Tuan
ai hoc Y Dc TPHCM
Cot SPE Poly tetrafluoroethylen (PTFE), poly ethylen (PE), poly propylen (PP) Khong eu 40 m < 100 Lu gi va ra giai ke tiep nhau Dung mot lan
ai hoc Y Dc TPHCM
Cu trc
Cu trc
ai hoc Y Dc TPHCM
Nguyen c Tuan
ai hoc Y Dc TPHCM
Nguyen c Tuan
ai hoc Y Dc TPHCM
Nguyen c Tuan
ai hoc Y Dc TPHCM
Nguyen c Tuan
ai hoc Y Dc TPHCM
Chat hap phu khong phan cc Nc Methanol Isopropanol Acetonitril Aceton Ethyl acetat Ethyl ether Tetrahydrofuran Methylen chlorid Chloroform Toluen Isooctan
MANH
Hexan
ai hoc Y Dc TPHCM
Nguyen c Tuan
ai hoc Y Dc TPHCM
Nguyen c Tuan
ai hoc Y Dc TPHCM
Nguyen c Tuan
ai hoc Y Dc TPHCM
Nguyen c Tuan
ai hoc Y Dc TPHCM
Nguyen c Tuan
ai hoc Y Dc TPHCM
Nguyen c Tuan
ai hoc Y Dc TPHCM
Nguyen c Tuan
ai hoc Y Dc TPHCM
Nguyen c Tuan
ai hoc Y Dc TPHCM
Nguyen c Tuan
ai hoc Y Dc TPHCM
Chit pha rn
Lng dung mi dng t hn nhiu so vi chit lng lng. c mt s thit b kt ni chit pha rn vi GC hoc HPLC, d dng t ng ha phn tch mu. C nhiu la chn pha rn dng cho SPE, nn c c ch chit a dng, ph hp hn vi cht phn tch, tnh chn lc tt hn.
Nguyen c Tuan
ai hoc Y Dc TPHCM