Principles of Instrumental Analysis
Principles of Instrumental Analysis
7th Edition
ISBN: 9781305577213
Author: Douglas A. Skoog, F. James Holler, Stanley R. Crouch
Publisher: Cengage Learning
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Chapter 17, Problem 17.13QAP
Interpretation Introduction

(a)

Interpretation:

For an angle of incidence of 450, the effective penetration depth of the evanescent wave should be determined. Penetration depth if the angle changed to 600 should be determined.

Concept introduction:

The effective penetration depth can be calculated as follows:

dp=λc2π[sin2θ(ns/nc)2]1/2

Here,

dp effective penetration depthλc Wavelength of the beamθ incident anglens refractive index of the samplencrefractive index of the crystal

Expert Solution
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Answer to Problem 17.13QAP

When the angle of incidence = 450

dp=1.64×106 m

When the angle of incidence = 600

dp=1.14×106 m

Explanation of Solution

When the angle of incidence = 450

dp=(1/2000)×1022×3.14[sin245(1.03/2.00)2]1/2dp=5×1062×3.14[0.50.265]1/2dp=1.64×106 m

When the angle of incidence = 600

dp=(1/2000)×1022×3.14[sin260(1.03/2.00)2]1/2dp=5×1062×3.14[0.750.265]1/2dp=1.14×106 m

Interpretation Introduction

(b)

Interpretation:

The penetration depths for sample refractive indexes varying from 1.00 to 1.70 in steps of 0.10 should be determined. Penetration depth should be plotted as a function of refractive index. The refractive index for which the penetration depth becomes zero should be determined.

Concept introduction:

dp=λc2π[sin2θ(ns/nc)2]1/2dp effective penetration depthλc Wavelength of the beamθ incident anglens refractive index of the samplencrefractive index of the crystal

Expert Solution
Check Mark

Answer to Problem 17.13QAP

The plot is represented as follows:

Principles of Instrumental Analysis, Chapter 17, Problem 17.13QAP , additional homework tip  1

Explanation of Solution

The data given is as follows:

Refractive index of sample dp, m
1.00 1.12597E-06
1.10 1.19018E-06
1.20 1.27491E-06
1.30 1.39125E-06
1.40 1.56143E-06
1.50 1.8387E-06
1.60 2.40057E-06
1.70 4.80114E-06

The plot for the data is represented as follows:

Principles of Instrumental Analysis, Chapter 17, Problem 17.13QAP , additional homework tip  2

From the graph, it can be seen that the refractive index never approaches zero.

Interpretation Introduction

(c)

Interpretation:

For a sample with a refractive index 1.37 at 2000 cm-1 and incident angle of 450, the penetration depth versus the ATR crystal refractive index should be plotted.

Concept introduction:

The effective penetration depth can be calculated as follows:

dp=λc2π[sin2θ(ns/nc)2]1/2

Here,

dp effective penetration depthλc Wavelength of the beamθ incident anglens refractive index of the samplencrefractive index of the crystal

Expert Solution
Check Mark

Answer to Problem 17.13QAP

Ge crystal will give smaller penetration depth as a refractive index of the crystal increases, the effective penetration depth decreases.

Explanation of Solution

The data given is as follows:

Refractive index of Crystal dp, m
2.00 4.53849E-06
2.25 2.21456E-06
2.50 1.78166E-06
2.75 1.58661E-06
3.00 1.47477E-06
3.25 1.40242E-06
3.50 1.35201E-06
3.75 1.31509E-06
4.00 1.28702E-06

The plot is represented as follows:

Principles of Instrumental Analysis, Chapter 17, Problem 17.13QAP , additional homework tip  3

Ge crystal will give smaller penetration depth as a refractive index of the crystal increases, the effective penetration depth decreases.

Interpretation Introduction

(d)

Interpretation:

The effective penetration depth at 3000 cm-1, 2000 cm-1 and 2000 cm-1 should be determined.

Concept introduction:

The effective penetration depth can be calculated as follows:

dp=λc2π[sin2θ(ns/nc)2]1/2

Here,

dp effective penetration depthλc Wavelength of the beamθ incident anglens refractive index of the samplencrefractive index of the crystal

Expert Solution
Check Mark

Answer to Problem 17.13QAP

At 3000 cm-1

dp=8.69×107 m

At 2000 cm-1

dp=1.31×106 m

At 1000 cm-1

dp=2.61×106 m

Explanation of Solution

At 3000 cm-1

dp=(1/3000)×102 m2×3.14[sin245(1.003/2.8)2]1/2dp=3.33×1063.83dp=8.69×107 m

At 2000 cm-1

dp=(1/2000)×102 m2×3.14[sin245(1.003/2.8)2]1/2dp=5×1063.83dp=1.31×106 m

At 1000 cm-1

dp=(1/1000)×102 m2×3.14[sin245(1.003/2.8)2]1/2dp=1×1053.83dp=2.61×106 m

In case of analyzing aqueous samples, pouring shallow amount over the surface of the crystal is sufficient. Since trace amounts are used to analyze, absorption by the aqueous solvent is not a problem.

Interpretation Introduction

(e)

Interpretation:

The principles of the new method to obtain a depth profile of a sample surface using ATR spectroscopy should be described.

Concept introduction:

In ATR spectroscopy through the ATR crystal, an infrared beam is passed such that it reflects off the internal surface at least once when in contact with the sample. This reflection results in an evanescent wave which goes into the sample. The penetration depth is determined by the wavelength of IR beam, angle of incidence, refractive indexes of sample and the crystal.

Expert Solution
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Explanation of Solution

A new depth profiling method using multiple-angle ATR/FT-IR spectroscopy has been developed.

First, a profile frequency is defined then the stratified medium is defined. Matrix A is generated from interpolated absorptances and matrix E is generated from estimated mean square electric fields. Linear equations of absorptance by SVD method is solved and the first estimated refractive index profile from matrix X is calculated. Nonlinear fittings of the reflectances are determined by Levenberg-Marquadt method. Finally, complex refractive index profile is obtained.

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