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Thesis - Automation of a Hydrogen Probe for Determination of Hydrogen
Solubility in Coal Liquids Solvents - 1987

Karlezi, Carlos R. Alonso

University of Pittsburg

In this pdf format, this document has 199 pages and is 4.47MB.

Table of Contents

Acknowledgement

iI

Abstract

iii

Table of Contents

v

List of Figures

x

List of Tables

xiv

Nomenclature

xvi

1.

Introduction

1

2.

Background

3

2.1

Literature Review

3

2.1.1

Effect of Pressure and Temperature on Hydrogen Solubility

3

2.1.2

Solubility of hydrogen in organic solvents

4

2.2

Theoretical Basis for Nickel Probe

5

2.2.1

Hydrogen Permeation through Nickel

5

2.2.2

Permeability Coefficient of Hydrogen Through Nickel

7

3.

Experimental

8

3.1

High Pressure Section

8

3.1.1

Source Section

8

3.1.2

Equilibrium Cell

10

3.1.3

High Pressure Microflowmeter

13

3.1.4

Hydrogen Probe

17

3.2

Low Pressure Section

22

3.2.1

Liquid and Gas Phase Sampling Section

22

3.2.2

Toepler pump

24

3.2.3

Gas Chromatograph

24

3.3

Control System

27

3.3.1

Basic Computer/Controller

27

3.3.2

A/D Board

28

3.3.3

Printer

28

3.3.4

Control Programs

29

3.4

Electrical Panel

29

3.5

Operational Procedures

31

3.5.1

Equipment Calibration

31

3.5.1.1

Thermocuples read by the computer

31

3.5.1.2

Heise Gauges

31

3.5.1.3

Pressure Transducers

31

3.5.1.4

Glass Section Volume

32

3.5.1.5

Gas Chromatograph

32

3.5.2

Leak Test

32

3.5.2.1

High Pressure Section.

33

3.5.2.2

Low Pressure Section

33

3.5.2.3

Gas Chromotograph

33

3.5.3

Conditioning

33

3.5.3.1

Probe Conditioning

33

3.5.3.2

Capillary Conditioning

34

3.5.3.3

Gas Chromatograph

34

3.5.4

Vacuum and Vent

34

3.5.5

Pressurization of the Source Section

35

3.5.6

Pressurization of the Equilibrium Cell

35

3.5.7

Pressurization of the Microflowmeter

35

3.5.8

Charging liquid into the cell

36

3.5.9

Charging other gases into the cell

36

3.5.10

Sampling

36

3.5.11

Transferring the Sample

37

3.5.12

Analysis of the Sample

37

3.6

Experimental Procedures

38

3.6.1

Hydrogen Permeation Experiments

38

3.6.2

Solubility of Hydrogen in Tetralin

38

3.6.3

Effect of Methane in Hydrogen Solubility in Tetralin

39

3.7

Commercial Equipment

40

3.7.1

Use of the Apparatus

40

3.7.2

Construction of the Equipment

40

3.7.3

precaution of the Equipment

41

3.7.4

Operation Instructions

41

4.

Experimental Results

51

4.1

Ancillary Results

51

4.1.1

Gas Chromatograph Calibration

51

4.1.2

Pressure Transducer Calibration

52

4.1.3

Volume

52

4.1.3.1

Sample Flask

52

4.1.3.2

Glass Section

52

4.1.3.3

Diameter of Capillary Tube

53

4.2

Results

53

4.2.1

Permability Coefficient

53

4.2.2

Hydrogen Solubility in Tetralin

53

4.2.3

Hydrogen Solubility in Tetralin under the presence of Methane

60

4.2.4

Hydrogen Solubility in Tetralin under the presence of Ethane

60

4.2.5

K-Value for Each Experiment

60

5.

Analyses of Results

79

5.1

Vapor Pressure of Tetralin

79

5.2

System Hydrogen-Tetralin

79

5.3

System Hydrogen-Tetralin-Methane

81

5.4

System Hydrogen-Ethane-Tetralin

82

5.5

K-Values

83

5.5.1

Prediction of K-values

88

5.5.1.1

K-value for Hydrogen

89

5.5.1.2

K-value for tetralin

89

5.6

Results from Commercial Equipment

98

6.

Conclusions

99

6.1

Automation of Hydrogen Probe

99

6.2

Experimental Results

99

6.3

Commercial Equipment

100

7.

Recommendations

101

7.1

Equipment

101

7.2

Experimental

102