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QUANG PH�
(C) HKD 2012 2
QUANG PH� H�NG NGO�I
� Near Infrared: particle and composition analysis
� Middle Infrared: primarily used in compound characterization
� Far Infrared: not used
Visible IRUV
Middle IRNear IR Far IR
800nm�12,500cm-1�
2.5�m �4,000cm-1�
25�m �400cm-1�
50 � m �200cm-1�
(C) HKD 2012 3
Thermal Imaging (Thermography)
QUANG PH� H�NG NGO�I
(C) HKD 2012 4
Night Vision Goggles
QUANG PH� H�NG NGO�I
(C) HKD 2012 5
QUANG PH� H�NG NGO�I
(C) HKD 2012 6
C� S� LÝ THUY�T
(C) HKD 2012 7
C� S� LÝ THUY�T
Radiation Outcome
• h� 109 nm Radiowave Nuclear Spin Flips
• h� 106 nm Microwave Molecular Rotation
• h� 104 nm Infrared Bond Vibrations
• h� 500 nm Visible Electronic Excitation
• h� 200 nm Ultraviolet Electronic Excitation
• h� 10 nm X-ray Molecular Ionization
• h� 0.1 nm Gamma Ray Bond Cleavage
(C) HKD 2012 8
C� S� LÝ THUY�T
Ph�n ng ca phân t� khi nh�n n ng l��ng h�ng ngo�i
h�
Low Energy High Energy
(C) HKD 2012 9
C� S� LÝ THUY�T
Các ki�u dao ��ng
(C) HKD 2012 10
C� S� LÝ THUY�T
Các ki�u dao ��ng
Symmetrical Asymmetrical Scissoring
Twisting Rocking Wagging(C) HKD 2012 11
h� = k(m1 + m2)m1 m2
m2
m1
k
�obs O-H > N-H > C-H > C-O > C-C > C-F
�obs C� > C=C > C-C
C� S� LÝ THUY�T
Ph��ng trình c� b�n
(C) HKD 2012 12
C� S� LÝ THUY�T
(C) HKD 2012 13
C� S� LÝ THUY�T
(C) HKD 2012 14
C� S� LÝ THUY�T
(C) HKD 2012 15
ALKANES
C-H bond “saturated”
(sp3) 2850-2960 cm-1
+ 1350-1470 cm-1
-CH2- + 1430-1470
-CH3 + “ and 1375
-CH(CH3)2 + “ and 1370, 1385
-C(CH3)3 + “ and 1370(s), 1395 (m)
C� S� LÝ THUY�T
n-pentane
CH3CH2CH2CH2CH3
3000 cm-1
1470 &1375 cm-1
2850-2960 cm-1
sat’d C-H
CH3CH2CH2CH2CH2CH3
n-hexane
2-methylbutane (isopentane)
2,3-dimethylbutane
cyclohexane
no 1375 cm-1
no –CH3
22(C) HKD 2012
ALKENES
=C—H bond, “unsaturated” vinyl
(sp2) 3020-3080 cm-1
+ 675-1000
RCH=CH2 + 910-920 & 990-1000
R2C=CH2 + 880-900
cis-RCH=CHR + 675-730 (v)
trans-RCH=CHR + 965-975
C=C bond 1640-1680 cm-1 (v)
C� S� LÝ THUY�T
1-decene
910-920 & 990-1000 RCH=CH2
C=C 1640-1680
unsat’dC-H
3020-3080 cm-1
4-methyl-1-pentene
910-920 & 990-1000 RCH=CH2
2-methyl-1-butene
880-900R2C=CH2
2,3-dimethyl-1-butene
880-900R2C=CH2
27(C) HKD 2012
C� S� LÝ THUY�T
BENZENES
=C—H bond, “unsaturated” “aryl”
(sp2) 3000-3100 cm-1
+ 690-840
mono-substituted + 690-710, 730-770
ortho-disubstituted + 735-770
meta-disubstituted + 690-710, 750-810(m)
para-disubstituted + 810-840(m)
C=C bond 1500, 1600 cm-1
ethylbenzene
690-710, 730-770mono-
1500 & 1600
Benzene ring
3000-3100 cm-1
Unsat’d C-H
o-xylene
735-770ortho
p-xylene
810-840(m)para
m-xylene
meta
690-710, 750-810(m)
styrene
no sat’d C-H
910-920 & 990-1000
RCH=CH2mono
1640C=C
2-phenylpropene
mono880-900R2C=CH2
Sat’d C-H
p-methylstyrene
para
35(C) HKD 2012
C� S� LÝ THUY�T
ALCOHOLS và ETHERS
C—O: 1050-1275 (b) cm-1
1o ROH 1050
2o ROH 1100
3o ROH 1150
ethers 1060-1150
O—H: 3200-3640 (b)
1-butanol
CH3CH2CH2CH2-OH
C-O 1o
3200-3640 (b) O-H
2-butanol
C-O 2o
O-H
tert-butyl alcohol
C-O 3oO-H
methyl n-propyl ether
no O--H
C-O ether
40(C) HKD 2012
C� S� LÝ THUY�T
CARBONYLS
C=O (ketones, aldehydes, and carboxylic acids) absorb ~1710 cm-1
C��ng �� l�n.
Aldehydes: 2 dao ��ng liên k�t C-H 2700 và 2800 cm-1
C=O liên hp v�i C=C: ~1680 cm-1.
C=O ca aminde:1640-1680 cm-1
The C=O ca ester ~1730-1740 cm-1
41(C) HKD 2012
C� S� LÝ THUY�T
CARBONYLS
42(C) HKD 2012
C� S� LÝ THUY�T
CARBONYLS
43(C) HKD 2012
C� S� LÝ THUY�T
CARBONYLS
44(C) HKD 2012
C� S� LÝ THUY�T
CARBONYLS
45(C) HKD 2012
C� S� LÝ THUY�T
LIÊN K�T C-N
C - N ~1200 cm-1
C = N ~ 1660 cm-1 m�nh h�n dao ��ng ca C = C.
C N h�p thu m�nh > 2200 cm-1 (tín hi�u ca C C y�u h�n và <
2200 cm-1
46(C) HKD 2012
C� S� LÝ THUY�T
LIÊN K�T C-N
47(C) HKD 2012
C� S� LÝ THUY�T
DAO ��NG C�A O-H VÀ N-H
Xu�t hi�n � vùng 3300 cm-1.
M�i O-H r�ng v�i m�i bè tròn.
Amin b�c 2 (R2NH), m�i r�ng v�i broad m�t ��nh nh�n.
Amin b�c 1 (RNH2), m�i r�ng v�i hai ��nh nh�n.
Amin b�c 3: không có tín hi�u h�p thu cho N-H
48(C) HKD 2012
C� S� LÝ THUY�T
DAO ��NG C�A O-H VÀ N-H
49(C) HKD 2012
C� S� LÝ THUY�T
DAO ��NG C�A O-H VÀ N-H
�Ph� IR có các m�i h�p h�n ph� UV
�Ph� IR cho nhi�u thông tin h�n ph� UV
�Có th� thu ph� IR t� nhi�u ��i t�ng m�u khác nhau: r�n, l�ng, khí
�Ph� IR kém thích h�p cho ��nh l��ng h�n ph� UV
�Ph� IR ��c thu nh�n ch�m và khó h�n ph� UV
�M�u cho ph� UV d� dàng chu�n b� h�n
�Quang ph� k� UV r! h�n
PH� IR VÀ PH� UV
(C) HKD 2012 50
230 240 250 260 270 280 290
Abs
orba
nce
PH� IR VÀ PH� UV
(C) HKD 2012 51
QUANG PH� K� H�NG NGO�I
� Quang ph� k� h�ng ngo�i tán s�c
� Dùng cách t�
� Quang ph� k� h�ng ngo�i bi�n ��i Fourrier (FTIR)
� Dùng giao thoa k�
(C) HKD 2012 52
QUANG PH� K� H�NG NGO�ITÁN S"C
(C) HKD 2012 53
FT = Fourier Transfrom
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
(C) HKD 2012 54
path “a”
path
“b”
ab
moving mirror
fixed mirror
detector
50% beamsplitter
x
sourcesample
j- stop
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
(C) HKD 2012 55
� = 0
for �= m�, get constructive interference
� is “retardation”
�=�/2
for �= (m+1/2)�, get destructive interference
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
(C) HKD 2012 56
Mirror travel
Frequency, (cm-1)
x = 0
x = 0
4004000
Interferogram:
Single beamspectrum of air
FT
100%
H2O H2OCO2
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
(C) HKD 2012 57
F(�) = f(t)e dt��t
Converts from units of time to units of frequency
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
(C) HKD 2012 58
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
(C) HKD 2012 59
�“Neat” (phân tích m�u l�ng tinh khi�t)
� Pellet (ép viên cho phân tích m�u r!n)
�Thin Cell (phân tích dung d�ch)
�Long Cell (phân tích m�u khí)
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
Chu#n b� m$u
(C) HKD 2012 60
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
Phân tích m$u “Neat”
(C) HKD 2012 61
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
Ép viên
(C) HKD 2012 62
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
Ép viên
(C) HKD 2012 63
�S� d"ng b�t khan KBr, KI, CsI
�Tr�n m�u v�i KBr theo t# l� 1:10
�Nghi�n ��n kích th��c 2 m diameter
�Cho vào khuôn và ép tay ho$c máy thy l'c
�L�y m�u ra kh�i khuôn, ti�n hành �o
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
Ép viên
(C) HKD 2012 64
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
Dùng cell l�ng
(C) HKD 2012 65
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
Dùng cell l�ng
(C) HKD 2012 66
� Lo�i tháo r�i (demountable liquid cell)
� ��nh tính.
� Ráp và tháo ra cho m�i l�n �o.
� B� dày có th �i�u chnh ���c (thông qua spacer).
� Lo�i kín (sealed liquid cell)
� Ch t l�ng d� bay h�i.
� B� dày có th �i�u chnh ���c (thông qua spacer).
� Lo�i kích th��c c� ��nh (fixed liquid cell)
� ��nh l��ng.
� B� dày c� ��nh.
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
Dùng cell l�ng
(C) HKD 2012 67
������� �����
���������� ����
������ ��������
����������� ���
� �����������
��� � !"��#$ $%&' ( )"�
*�+� �,""��#$ $%!) ( )"�
��-#& �'&"��#$ '% . / ."�
��0' �.."��#$ $%!' / )"�
+�0' �$$""��#$ $% ) 1 )&�
� KBr là v�t li�u ph� bi�n nh t.
� KRS-5, BaF2 or CaF2 có th ���c dùng � �o dung d�ch trong n��c mà n�ng�� tác ch t l�n h�n vài %.
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
Dùng cell khí
(C) HKD 2012 68
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
Dùng cell khí
(C) HKD 2012 69
Long Path Cell
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
ATR (Attenuated Total Reflection)
(C) HKD 2012 70
� Không c�n ti�n x� lý m�u.
� Phân tích b� m�t.
� M�u ph�i ti�p xúc v�i l�ng kính.
� Lo�i m�u: film, nh�a (plastic), cao su (rubber), ch t ph! (coating on
same materials), …..
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
ATR (Attenuated Total Reflection)
(C) HKD 2012 71
IR Beam
Prism
SampleSample Press
n1: Refractive Index of prism
212
2 )n/n(sin2dp
�
�
�Penetration Depth (dp) : �: Incident Angle
n2: Refractive Index of sample
�: Wavelength
Sample
Prism
dpZoom
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
ATR (Attenuated Total Reflection)
(C) HKD 2012 72
� Ch�t l�ng� M�u có b mt ph�ng� B�t� M i h�p thu l�n (���ng truyn l�n)
� Ch�t l�ng� M�u không có b mt ph�ng� B�t� M i h�p thu nh� (���ng
truyn ng�n
Infrared beam
Prism
Sample
Prism
Infrared beam
Sample
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
ATR (Attenuated Total Reflection)
(C) HKD 2012 73
� Multi-reflection ATR1) ATR-8000A
�Solid sample (Film, Plastic, Rubber, Coating)
�The incident angle can be selected form 302, 452, or 602
2) ATR-8200HA
� Liquid and Solid sample.
� Single Reflection ATR�MIRacle A
�DuraSamplIR�
ATR-8000A
ATR-8200HA
MIRacle A DuraSamplIR�
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
ATR (Attenuated Total Reflection)
(C) HKD 2012 74
� MIRacle A: l�ng kính có ��"ng kính 1,5mm.
� L�ng kính ���c ch� t�o t# ZnSe, Ge ho�c kim c��ng.
� L�ng kính ZnSe��o l��ng m�u nh�.
�C�"ng �� m$i tín hi�u cao h�n l�ng kính Ge.
� L�ng kính Ge�Dùng cho m�u có chi�t su t l�n (black rubber).
� Phân tích b� m�t.
�
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
ATR (Attenuated Total Reflection)
(C) HKD 2012 75
!&","".&")""$"&"$'""$ &"$&""$,&"$3""$)&"'!""'."" """ "" ,"" )""$4��
"
'%&
&
.%&
$"
$'%&
$&
$.%&
'"
''%&
'&
�5
6789:;<�=�����>?�@
Ge
ZnSe
Diamond/ZnSe
Diamond
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
ATR (Attenuated Total Reflection)
(C) HKD 2012 76
Prism Banned Samples
ZnSe Acid (less then pH 5), strong alkaline (more than pH 9)
KRS-5*)
acetoneammonium salt solutionsulfuric acidammoniaEDTAA solution of a compound that reacts with thallium to form a Complex
Ge Hot concentrated sulfuric acid
Diamond -*) Consist of TlBr and TlI
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
ATR (Attenuated Total Reflection)
(C) HKD 2012 77
ATR-8200HA
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
ATR (Attenuated Total Reflection)
(C) HKD 2012 78
"%"
"%""&
"%"$
"%"$&
��-
$"""%"$&""%"'"""%" """%"!"""%"$4���� �������A����B������#�5�
"%"
"%"'&
"%"&
"%".&
��-
$"""%"$&""%"'"""%" """%"!"""%"$4��C���B������#�5�
Single Hair with Hair Spray
Untreated Hair
Single Hair on Diamond Prism
DuraSamplIR�
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
ATR (Attenuated Total Reflection)
(C) HKD 2012 79
"%"
"%$
��-
$"""%"'"""%"!"""%"$4��
"%"&
"%$
"%$&
��-
$"""%"'"""%"!"""%"$4��
"%&
��-
$"""%"'"""%"!"""%"$4��
"%'&
"%&
��-
$"""%"'"""%"!"""%"$4��
Acrylic Rubber NBR
So sánh hai lo�i l�ng kính MIRacle A
ZnSe ZnSe
Ge Ge
3""$"""$'""$!""$,""$3""'"""'!""'3"" '"" ,""!"""$4��
).
).%&
)3
)3%&
))
))%&
$""
�5
-�D ��� ���A�� ���D� ������E����� ��
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
ATR (Attenuated Total Reflection)
(C) HKD 2012 80
C=O1750cm-1 : ch�t béo.1700 - 1500cm-1: protein.1000cm-1 : lactose (n�i ether).
3""$"""$'""$!""$,""$3""'"""'!""'3"" '"" ,""!"""$4��
�5
���E
Spectra of water and milk
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
ATR (Attenuated Total Reflection)
(C) HKD 2012 81
V�t li�u gói th�c ph�m nhiu l�pPh� h�ng ngo�i c�a mt sau (PE) và mt tr��c(PET)
3""$"""$'""$!""$,""$3""'"""'!""'3"" '"" ,""!"""$4��
�5
���E
PE
PET
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
ATR (Attenuated Total Reflection)
(C) HKD 2012 82
3""$"""$'""$!""$,""$3""'"""'!""'3"" '"" ,""!"""$4��
�D�
FG5
polyethylene terephthalate (PET)
ATR corrected spectrum
ATR spectrum
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
Ph�n x� (Specular Reflectance method)
(C) HKD 2012 83
� �o ���c hai d�ng m�u:
� Nh�a bóng (glossy flat plastic).
� Phim m�ng ph! trên kim lo�i (thin film on metal plate).
Det
ecto
r
Inte
rfer
omet
er
Sample
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
Ph�n x� (Specular Reflectance method)
(C) HKD 2012 84
Film
Metal plate
abInfrared beam
a << bb
0.1�20�mSample
Infrared beama
b
Glossy flat plasticThin film
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
Ph�n x� (Specular Reflectance method)
(C) HKD 2012 85
'%"
!%"
,%"
�5
&""%".&"%"$"""%"$'&"%"$&""%"$.&"%"'"""%"'&""%" """%" &""%"!"""%"$4��HIJ7K<LMNO
3&%"
)"%"
)&%"
$""%"
$"&%"
�5
&""%".&"%"$"""%"$'&"%"$&""%"$.&"%"'"""%"'&""%" """%" &""%"!"""%"$4���+�$%=�-PQR��STUVW6XI;7>YZ005O@
Bi�n ��i Kramers-Kronig
polymethylmethacrylate
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
Ph�n x� khu�ch tán (Diffuse Reflectance )
(C) HKD 2012 86
� Dùng �o m�u b�t: b�t h�u c�, xúc tác, g�m s� (ceramic powder).
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
Ph�n x� khu�ch tán (Diffuse Reflectance )
(C) HKD 2012 87
� Dùng �o m�u b�t: b�t h�u c�, xúc tác, g�m s� (ceramic powder).
S
D
S : Specular reflectionD : Diffuse reflection
Infrared beam
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
Ph�n x� khu�ch tán (Diffuse Reflectance )
(C) HKD 2012 88
&"%"
.&%"
$""%"
�5
&""%"$"""%"$&""%"'"""%" """%"!"""%"$4��
&"%"
.&%"
$""%"
�5
&""%"$"""%"$&""%"'"""%" """%"!"""%"$4��
Bi�n ��i Kubelka-Munk
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
Ph�n x� khu�ch tán (Diffuse Reflectance )
(C) HKD 2012 89
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
Ph�n x� khu�ch tán (Diffuse Reflectance )
(C) HKD 2012 90
UV(254nm)
RI
A
B
C
Sebacic Acid Dialkyl Ester
Phthalic Acid Dialkyl Ester
(B)
(C)
Dual Channel GPC Chromatograms of Polyvinyl Chloride
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
H%p thu ph�n x� (Reflection Absorption Spectroscopy)
(C) HKD 2012 91
� Phim m�ng trên kim lo�i (thin film on metal).
� Có th �o ���c phim có b� dày <1&m..
� �ôi khi k�t h�p v�i thi�t b� phân c�c ánh sáng (polarizer).
Det
ecto
r
Inte
rfer
omet
er
Sample
Mask
Shield Plate
RAS-8000A
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
H%p thu ph�n x� (Reflection Absorption Spectroscopy)
(C) HKD 2012 92
Metal plate
Thin film1�1000nm
70��85�
(1) Vertical polarized light (2) Parallel polarized light
Incident beam Reflected beam
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
H%p thu ph�n x� (Reflection Absorption Spectroscopy)
(C) HKD 2012 93
Lead Stearate
� Ki�m tra ��nh tính thu�c (vùng “vân tay”,fingerprint)
� Ki�m tra sàng l�c và nhanh chóng ��nh danh C=O
� Phân tích ��nh tính m�u r!n (kem, viên nén)
� Phát hi�n crystal isoforms (polymorphs)
� Xác ��nh hàm l�ng n��c
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
'NG D*NG
(C) HKD 2012 94
�Phân tích n��c ti�u và các ch�t l�ng sinh h�c (urea,creatinine, protein)
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
'NG D*NG
(C) HKD 2012 95
� *o glucose b;ng k? thu�t không xâm l�n
QUANG PH� K� H�NG NGO�IBI�N ��I FOURRIER
'NG D*NG
(C) HKD 2012 96