2

(Final Examination of Spectroscopic Methods for Chemical Analysis)

8/26/2011


(Multi-Component Analysis)

Commercial xylene 3 1,2 dimethylbenzene (O - Xylene) 1,3 dimethylbenzene - (m - Xylene) 1,4 - dimethylbenzene (p - Xylene) standard
xylene solution Cyclohexane
0.1 mm IR Spectra

Asolution

Xylene
Fig.1 IR spectrum of 1 vol%, o-xylene

CH3

CH3

Asolution(vol%)-1
1 vol%

Asolution

Fig.2 IR spectrum of 2 vol%, m-xylene

Fig.3 IR spectrum of 2 vol%, p-xylene

o-xylene, m-xylene, p-xylene

740, 770 800 cm-1
1)

solution

measured

Anoise

Asolution
Ameasured
Anoise

2)

solution

A measured A noise A measured

Solution
Solution

[Solution]

o-xylene 740 cm-1;

o xylene

Asolution
0.440 0.012

0.428 ( vol %) 1
1 vol %
:


baseline

(noise signal)

(wave number)

m-xylene 770 cm-1 ;

m xylene

p-xylene 800 cm-1 ;

p xylene

0.460 0.015
0.223 ( vol %) 1
2 vol %
0.545 0.015

0.265 ( vol %) 1
2 vol %

5 vol% Commercial xylene

IR spectrum

p-xylene

o-xylene

m-xylene
Fig.4 IR spectrum of 5% Commercial xylene
Asolution
o-xylene 740 cm-1 ;
m-xylene 770 cm-1 ;
p-xylene 800 cm-1 ;

[o-xylene] Ao-xylene = 0.156
Astd = 0.482 (vol%)-1

Astd = 0.482
1 vol%
Ao-xylene = 0.156

0.156/(0.482 (vol%)-1)
= 0.364 vol%

Ao-xylene = 0.194 0.038 = 0.156

Am-xylene = 0.720 0.034 = 0.686
Ap-xylene = 0.133 0.030 = 0.103

Commercial xylene vol%

[o-xylene] 740 cm-1
[m-xylene] 770 cm-1
[p-xylene ] 800 cm-1

0.156 1 vol %
0.364 vol %
0.482
0.686 1 vol %

3.076 vol %
0.223
0.103 1 vol %

0.389 vol %
0.265

baseline
-

:

Aspirin, Phenacetin Caffein

chloroform solution carbonyl
group calibration data NaCl transmission cell 0.1 mm

Component
Aspirin
Phenacetin
Caffein

Concentration
(mg ml-1)
90
65
15

C=O stretching
wavenumber (cm-1)
1764
1511
1656

Absorbance
0.217
0.185
0.123

Aspirin, Phenacetin Caffein mg ml-1
wavenumber (cm-1)
1764
1511
1656

1) A

Aspirin

1764 cm-1;

Phenacetin 1511 cm-1 ;

Caffein

A measured A noise
Solution
0.217
Aaspirin 90 mg ml 1 2.4110 3 ml mg 1
0.185
A phenacetin 65 mg ml 1 2.8510 3 ml mg 1
0.123
Acaffein 15 mg ml 1 8.20 10 3 ml mg 1

Absorbance
0.207
0.202
0.180

1656 cm-1 ;

solution

2) A
[Aspirin]
[Phenacetin]
[Caffein]

0.207 1 mg ml 1

85.9 mg ml 1
3
2.4110
0.202 1 mg ml 1

70.9 mg ml 1
3
2.8510
0.180 1 mg ml 1

22.0 mg ml 1
3
8.20 10