Kekrnlj 8 TT 36 P 0 CSNNPF

CHNG 8
KHI QUT V CC PHNG PHP PHN TCH PH NGHIM

GV: Trn T Phng Tho BM Ha L (HBK) 1
NI DUNG CHNH (2LT)

1. Nguyn tc 2. Bc x in t 3. Nng lng ca vt cht 4. Tng tc gia bc x v vt cht 5. Nguyn l cu to quang ph k 6. nh lut Lambert Beer
GV: Trn T Phng Tho BM Ha L (HBK)
Bc sng kho st l xc nh
1. Nguyn tc
Kt qu GT o
Tn hiu Da vo s tng tc gia bc x v vt cht. Ty theo bn cht bc x v vt cht, kt qu tng tc l tn hiu (ph) hay i lng o (A, T) nh tnh v nh lng mu.
5
Bc x
Vt cht
2. Bc x in t
2.1. Tnh cht Bn cht sng Bn cht ht 2.2. Cc vng bc x in t
Bn cht sng
Bc x in t l dng nng lng truyn i trong khng gian vi vn tc rt ln theo dng sng hnh sin.
Bn cht sng
c trng bi hin tng: Nhiu x Giao thoa. Bc sng hay di sng (cm, m, nm, A..): khong cch gia 2 cc i hay 2 cc tiu ni tip nhau
Bn cht sng
Chu k T(s): thi gian sng truyn gia 2 cc i lin tip Tn s (s-1): s dao ng trong mt giy. v = 1/T S sng (cm-1): s bc sng trong 1 cm. = 1/ Tc truyn sng trong chn khng: C = v* = 3.1010 cm/s
Bn cht ht
Bc x in t c xem nh nhng dng ht photon truyn i vi vn tc nh sng, c nng lng t l vi tn s ca bc x. Vi h = 6,63.1027 (erg.s): hng s Plank Nhn xt: + Bc x c di sng cng b th nng lng ca cc ht photon cng ln.
2.2. Cc vng bc x in t
nm tng dn Tia Tia gamma X 160 UV 400 kh kin Hng Vi Sng ngoi sng radio
800
nh sng trng l tng hp cc bc x vng thy c.

12
(cm) (cm-1) (Hz)

3.10-11 3,3.1010 3.10-9 3,3.108 3.10-7 3,3.106 3.10-5 3,3.104 3.10-3 3.10-1 3.101 3.103 3,3.102 3,3.100 3,3.10-2 3,3.10-4 1021 1019 1017 1015 1013 1011 109 107
Bc x
Tia gamma Tia X UV Vis IR Vi sng Sng radio
E (Kcal/mol)
9,4.107 9,4.105 9,4.103 9,4.101 9,4.10-1 9,4.10-3 9,4.10-5 9,4.10-7
13
2.2. Cc vng bc x in t
Phn loi cc PPPT ph nghim: PP cng hng t (s dng sng radio, sng vi ba) PP Rontgen (s dng sng Rontgen tia X) PP hp thu UV Vis PP hp thu IR ..
3. Nng lng ca vt cht

Vt cht c cu to t cc nguyn t, ion, phn t Tng nng lng bn trong vt cht gi l ni nng
15

Et: nng lng do cc electron chuyn ng gy ra Ed: nng lng sinh ra do cc ht nhn nguyn t dao ng xung quanh v tr cn bng ca n Eq: nng lng sinh ra do phn t quay quanh trng tm ca n.
16

Cc mc nng lng trong nguyn t: Mc nng lng in t Mc nng lng dao ng Mc nng lng quay.

v3 v2 v1 v0 Eq Ed Trng thi electron kch thch
v3 Trng thi v2 electron v1 c bn v0 Trng thi nng lng ca phn t hai nguyn t
Nng lng

Phn t c cu to phc tp hn nguyn t s mc nng lng ca n s nhiu hn. Cc nt, pt mc E thp (c bn) nhn c nng lng thch hp t bc x E cao (trng thi kch thch).
4. Tng tc gia bc x v vt cht

Khi bc x truyn n vt cht: Bc x b phn x b mt vt cht Bc x b hp thu, tn x bn trong vt cht, mt phn bc x truyn qua. Vt cht pht ra nng lng di dng bc x
4.1. S hp thu bc x ca vt cht

+
E = h
21

Khi bc x truyn ti VC: mt phn NL ca BX b vt cht gi li c chn lc hin tng hp thu BX ca VC. Nng lng VC hp thu:
E1; E2: mc nng lng trng thi u v trng thi cui ca VC
:tn s ca bc x b hp thu

Theo thuyt lng t Nt, pt, ionc mt s gii hn cc mc nng lng nht nh. S hp thu hay pht x BX ca VC khng phi lin tc v bt k m c tnh cht gin on v chn lc. Nguyn t, phn t ch hp thu hay pht x 0, 1, 2,., n ln lng t h.
4.1. S hp thu bc x ca vt cht Khi chiu chm bc x c xc nh i qua vt cht VC hp thu BX:
24

Khi chiu bc x n vt cht, vt cht hp thu nng lng lm tng ni nng ca n bin thin mt i lng: E = Et + Ed + Eq Nhng bc x b vt cht hp thu c tn s ng bng: tn s kch thch in t t tn s dao ng d tn s quay q
25

Cho nn: Ch nhng BX c NL photon kch thch ph hp vi s chnh lch mc NL gia TTCB v TTKT no VC mi hp thu. Ch nhng BX c tn s ng bng cc tn s ring ca phn t th mi b vt cht hp thu.
Bc x c nng lng thp: to ra s dch chuyn cc mc nng lng ca Eq Bc x hng ngoi: to ra s dch chuyn cc mc nng lng ca Ed, Eq Bc x UV-Vis: to ra s dch chuyn cc mc nng lng ca Et, Ed, Eq
4.2. Quy tc chn lc ca ph phn t K phn t hp thu bc x: Nng lng bc x ph hp cc mc bin thin nng lng trong phn t. S chuyn mc nng lng km theo s phn b li in t trong phn t. C hai dng chuyn mc: Chuyn mc cho php (p ng quy tc chn lc) Chuyn mc b cm.
28
4.3. S bin i bc x hp thu

Khi vt cht hp thu bc x: Vt cht c b sung nng lng. Pt, nt chuyn t mc nng lng thp ln mc nng lng cao. Trng thi in t c bn chuyn ln trng thi in t kch thch (tn ti trong khong thi gian ngn 10-3 10-8 giy)
4.3. S bin i bc x hp thu

Phn nng lng vt cht hp thu b bin i: Thnh Equay; Edaong; Etnhtin cc phn t va chm nhiu hn sinh nhit. Trng thi kch thch trng thi c bn: phn t pht bc x c tn s .' ( = 'tn s bc x hp thu) : < 'pht x hunh quang hay ln quang
4.4. Ph hp thu
Ph hp thu: ng biu din cng hp thu (A, T) bc x theo (, , ).. Nu vt hp thu dng: Nguyn t ph hp thu nguyn t Phn t ph hp thu phn t
4.4. Ph hp thu
32
4.4. Ph hp thu
Tn s bc x b hp thu c ngha c trng cho cu trc VC QP nh tnh. Nu mu cha cng nhiu cu t X hp thu BX cng gim E ca BX cng mnh da vo ph hp thu nh lng X.
4.5. S pht x ca vt cht
34

Vt cht dng nt, pt,.. nhn c nng lng thch hp chuyn t mc NL thp (bn) ln mc NL cao (km bn). C khuynh hng quay v mc NL thp pht ra NL dng BX hin tng pht x.
35
2 1
h2 h1 h1'
h) 2 2( 2
0
5. Nguyn l cu to quang ph k
Gm cc b phn chnh:
Ngun bc x (1) B phn to n sc (2) Khe (3) Chu o (4) B phn nhn tng tc v chuyn thnh tn hiu (5) Quang nng in nng (TBQ) (UVVis) Quang nng nhit nng (cp nhit in) (IR) B phn ghi kt qu (T v A) (6) GV: Trn T Phng Tho
BM Ha L (HBK) 37
5. Nguyn l cu to quang ph k
S CU TO MY O QUANG
T A
(1)
(2)
(3)
(4)
(5)
(6)
38
Hitachi Instruments U-3010
Light Source, selector, Sample cell holder, Detector (amplifier, recorder)

Hnh dng: Khi ch nht hoc ng tr ng Kch thc: ng knh 0,05-50mm (ph bin nht l 10mm)
40
6. nh lut Lambert Beer

tn x IR Io hp thu IA nng C IT
b
Bc x trc v sau khi hp thu
41

Nu b mt chu o tht nhn (IR = 0) Cng hp thu biu din thng qua cc i lng (T, A): truyn sut: Phn trm truyn sut:

hp thu A:
Phn trm hp thu:
43

Bng thc nghim, Lambert chng minh:
Bng thc nghim, Beer chng minh:
44

nh lut Lambert Beer: hp thu A ca bc x t l vi b dy v nng ca cht hp thu
Vi : h s hp thu (c trng cho cng hp thu bc x ca cht kho st).


ph thuc: + Bn cht vt cht + Bc x vt cht hp thu. + Nhit . b = 1cm, C =1mol/l b = 1cm, C = 1g/l
46
6. nh lut Lambert Beer A = bC

b = const
Nng mu qu cao mc lin hp hay phn li ca phn t thay i quan h tuyn tnh trit tiu.

A A peak
Cmax Ti C
48

iu kin nghim ng ca L: Bc x phi n sc. C < 0,01M A = 0,2 0,8 hoc A < 3,0
ng dng PPPT ph nghim

nh tnh: p dng cho mu hu c: so snh gia chun v mu theo C , Cn kt hp thm: sc k, ph hng ngoi, khi ph, ph cng hng t NMR tng chnh xc.
ng dng L Lambert Beer

NH LNG: nh lng mt cu t PP trc tip Php o trc tip Php so snh Php lp ng chun Php thm chun PP chun o quang nh lng nhiu cu t.
NH LNG MT CU T
PHP O TRC TIP

o hp thu Am ca DD mu Tra l thuyt (s tay) Xc nh b (chu o)
Nhc im: km chnh xc v l thuyt thc t

53
PHP SO SNH
Pha DD chun CC (bit trc) o AC o hp thu Am ca DD mu (dng cng 1 chu o b)
54
PHP SO SNH
IU KIN NG DNG PHP SO SNH: MU = CHUN A v C tuyn tnh trong khong nng kho st. Chun v mu ng nht v iu kin nn.
PHP LP NG CHUN
Fe+2
56
PHP LP NG CHUN
A
A (mu)
C1 C2 C3 C4 C5
57
PHP LP NG CHUN
CCH TM CMU: PP th PP bnh phng cc tiu. U IM: Hiu chnh sai s ngu nhin m php so snh c th mc phi. Kim tra khong nng thch hp A v C tuyn tnh.
PHP THM CHUN

THM CHUN VO MU V SO SNH
THM CHUN VO MU V S DNG NG CHUN

THM CHUN VO MU V SO SNH

DD 1: (Cm? + CC) o Athmchun DD 2: mu Cm? o Amu
60
61

Lp ng chun A = f(C). DD 1: (Cm? + CC) o Athmchun T th DD 2: mu Cm? o Amu T th

A
A (mu thm chun) Am (mu )
C2
C1
C1 C2 C3 C4 C5
63

Theo l thuyt Cm? = C1 v Cm? + CC = C2 C2 C1 = CC nhng do c cu t nh hng nn kq c th khc.
64
65
PHNG PHP CHUN O QUANG

Chun dd kho st X bng dd chun CC C+XA+B o hp thu ca mt trong bn cu t trn mt bc sng thch hp trong sut qu trnh chun . V A = f(Vc) tm im tng ng
66
Vd: chun Bi3+ v Cu2+ bng EDTA. Bit: pH4 ch c phc Cu.EDTA hp thu =745nm, phc Bi.EDTA khng hp thu. BiY = 1011.8 CuY = 1010.2 ng biu din A = f(VEDTA) c dng:
67
NH LNG NHIU CU T
NH LNG NHIU CU T
S dng tnh cht cng hp thu: hp thu dd (cha n cu t) ti 1 bc sng i bng tng hp thu ca tng cu t ti bc sng . nh lng tng cu t m khng cn tch lp h phng trnh.
NH LNG NHIU CU T
A 1 = A 1 + ..... + A 1 I N A 2 = A 2 + ..... + A 2 .......... .......... .......... ..... I N A = A n + ..... + A n n

NH LNG 2 CU T
71
NH LNG NHIU CU T
AI1 AII I
2
II
AI2 AII1
72

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CHNG 8

KHI QUT V CC PHNG PHP PHN TCH PH NGHIM

NI DUNG CHNH (2LT)

GV: Trn T Phng Tho BM Ha L (HBK)

GV: Trn T Phng Tho BM Ha L (HBK)

GV: Trn T Phng Tho BM Ha L (HBK)

GV: Trn T Phng Tho BM Ha L (HBK)

GV: Trn T Phng Tho BM Ha L (HBK)

nh sng trng l tng hp cc bc x vng thy c.

GV: Trn T Phng Tho BM Ha L (HBK)

(cm) (cm-1) (Hz)

GV: Trn T Phng Tho BM Ha L (HBK)

3. Nng lng ca vt cht

GV: Trn T Phng Tho BM Ha L (HBK)

3. Nng lng ca vt cht

GV: Trn T Phng Tho BM Ha L (HBK)

3. Nng lng ca vt cht

3. Nng lng ca vt cht

3. Nng lng ca vt cht

4. Tng tc gia bc x v vt cht

4.1. S hp thu bc x ca vt cht

GV: Trn T Phng Tho BM Ha L (HBK)

4.1. S hp thu bc x ca vt cht

E1; E2: mc nng lng trng thi u v trng thi cui ca VC

4.1. S hp thu bc x ca vt cht

GV: Trn T Phng Tho BM Ha L (HBK)

4.1. S hp thu bc x ca vt cht

GV: Trn T Phng Tho BM Ha L (HBK)

4.1. S hp thu bc x ca vt cht

4.1. S hp thu bc x ca vt cht

4.3. S bin i bc x hp thu

4.3. S bin i bc x hp thu

GV: Trn T Phng Tho BM Ha L (HBK)

4.5. S pht x ca vt cht

GV: Trn T Phng Tho BM Ha L (HBK)

4.5. S pht x ca vt cht

GV: Trn T Phng Tho BM Ha L (HBK)

4.5. S pht x ca vt cht

GV: Trn T Phng Tho BM Ha L (HBK)

Hitachi Instruments U-3010

Light Source, selector, Sample cell holder, Detector (amplifier, recorder)

GV: Trn T Phng Tho BM Ha L (HBK)

6. nh lut Lambert Beer

Bc x trc v sau khi hp thu

6. nh lut Lambert Beer

6. nh lut Lambert Beer

Phn trm hp thu:

GV: Trn T Phng Tho BM Ha L (HBK)

6. nh lut Lambert Beer

Bng thc nghim, Beer chng minh:

GV: Trn T Phng Tho BM Ha L (HBK)

6. nh lut Lambert Beer

Vi : h s hp thu (c trng cho cng hp thu bc x ca cht kho st).

6. nh lut Lambert Beer

6. nh lut Lambert Beer A = bC

6. nh lut Lambert Beer

6. nh lut Lambert Beer

ng dng PPPT ph nghim

ng dng L Lambert Beer

PHP O TRC TIP

GV: Trn T Phng Tho BM Ha L (HBK)

Nhc im: km chnh xc v l thuyt thc t

GV: Trn T Phng Tho BM Ha L (HBK)