Luận văn thạc sĩ determination of ammonia in water samples using nda fluorescence derivatization

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THAI NGUYEN UNIVERSITY

UNIVERSITY OF AGRICULTURE AND FORESTRY

PHẠM THỊ HẢI VÂN

TOPIC TITLE: DETERMINATION OF AMMONIA IN WATER SAMPLES

USING NDA FLUORESCENCE DERIVATIZATION WITH DIFFERENT

NUCLEOPHILES

BACHELOR THESIS

Study Mode : Full-time

Major : Environmental Science and Management

Faculty : International Training and Development Center

Batch : 2011-2015

Thai Nguyen, 9/2015

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Thai Nguyen University of Agriculture and Forestry

Degree Program : Bachelor of Environmental Science and Management

Student name : Phạm Thị Hải Vân

Student ID : DTN 1153070072

Thesis Title :

Determination of Ammonia in Water Samples Using NDA

Fluorescence Derivatization with Different Nucleophiles

Supervisor (s):

- Assoc.Prof. WU ,Chien-Hou

- Assoc.Prof .Dr. Do Thi Lan

Abstract: Fluorescence has been in use by physical chemists for many years.

Based on emission capacity of substance that has absorbed light or other

electromagnetic radiation, fluorescence seems as one method with highest

applicability in chemical analysis. An attraction of fluorescence is its sensitivity,

which helps scientists save time in research. Based on that

advantage, fluorescence has widely application for determining ammonia and other

possible nitrogen-containing photoproduct compounds (amine, amino acid...)

with derivatizing reagent, OPA (o-phthaldialdehyde). On the other hand,

naphthalene-2,3-Dicarboxaldehyde (NDA) has been estimated as another popular

derivatizing reagent, that can form much more stable derivatives with amines than

OPA derivatives(Carlson, 1986).

This study was to optimize the derivatization conditions including concentration

of NDA, maximum excitation and emission wavelengths, reaction pH, reaction

temperature and time, and choice of nucleophiles for analysis of ammonia in aqueous

solution.

Keywords: Fluorescence, Naphthalene-2,3-dicarboxaldehyde (NDA),

Ammonia, Cyanide, Sulfite.

Number of Pages: 53

Date of Submission: September, 30, 2015

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ACKNOWLEDGEMENT

To have completed this thesis, in addition to the ongoing efforts of myself, I would

like to thank for teachers in faculty of International Training and Development as well as

teachers in Thai Nguyen University of Agriculture and Forestry, who have dedicated

teaching to me the valuable knowledge during study time in university and gave me a

chance to do my thesis oversea. It is with immense gratitude that I acknowledge the

support and help of Biomedical Engineering & Environmental Science Department,

National Tsing Hua University for accepting me to working in this wonderful place.

Furthermore, express my sincere deepest gratitude to Assoc. Prof. Wu Chien Hou,

from Biomedical Engineering & Environmental Science Department, National Tsing Hua

University and Assoc.Prof. Dr. Do Thi Lan from Thai Nguyen University of Agriculture

and Forestry, who directly guided and created favorable conditions for me during the

implementation of this thesis.

Next, i would like spend special thanks to Mr. Bill (Wang Chin Yi) PhD student

and my friends in the laboratory facilitated and provided the information and data

necessary for my implementation process and helped me finish this thesis.

Finally, I would like to sincerely thank my family, all of my friends who always

beside me all the time, giving spiritual help for me complete the tasks assigned during

learning and research doing this thesis experiment.

In the process of implementing the project, my thesis might have inevitable

shortcomings. Therefore, would like to receive the attention and feedback from teachers

and friends to this thesis is more complete

Sincerely,

Pham Thi Hai Van

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TABLE OF CONTENT

LIST OF FIGURES ............................................................................................................. 1

LIST OF TABLE ................................................................................................................. 3

PART I. INTRODUCTION ................................................................................................ 5

1.1.Research rationale.......................................................................................................... 5

1.2.Objectives of the research ............................................................................................. 6

1.3.Research questions and hypothesis ............................................................................... 6

1.4.Limitations of research .................................................................................................. 6

PART II. LITERATURE REVIEW. ................................................................................... 7

2.1. Ammonia .................................................................................................................... 7

2.1.1 The properties of ammonia ......................................................................................... 7

2.1.2. Origins of ammonia pollution in water ..................................................................... 8

2.2.Methods for determinate ammonia ................................................................................ 9

2.2.1.Ion Chromatography ................................................................................................... 9

2.2.2.Voltammetry ............................................................................................................. 10

2.2.3Fluorescence .............................................................................................................. 11

2.3.Overview of research and application of NDA in fluorescence .................................. 12

2.3.1.o-phthaldialdehyde (OPA) ........................................................................................ 12

2.3.2.Naphthalene-2,3-dicarboxaldehyde (NDA) ............................................................. 14

PART III. METHODS ....................................................................................................... 16

3.1. Material ....................................................................................................................... 16

3.1.1 Chemicals ................................................................................................................. 16

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3.1.2 Equipment ................................................................................................................. 16

3.2 Methods ....................................................................................................................... 18

3.2.1. Determine the optimum concentration .................................................................... 18

3.2.2. Fluorescence Spectrophotometer ............................................................................. 21

3.3. HPLC system .............................................................................................................. 24

PART IV. RESULTS ........................................................................................................ 27

4.1. NDA-ammonia-sulfite reaction .................................................................................. 27

4.1.1 Optimization Excitation and Emission wavelength ................................................. 27

4.1.2. Effect of pH value on the fluorescence of NDA-

-sulfite product .................... 28

4.1.3. Effect of reaction time on the fluorescence of NDA-

-sulfite product ............. 29

4.1.4. Effect of reaction temperature on the fluorescence of NDA-

-sulfite product . 30

4.1.5. Effect of ratio between NDA and sulfite on the fluorescence of NDA-

-sulfite

product ............................................................................................................................... 31

4.1.6 Apply Pertinent Parameters on determine ammonia ................................................ 33

4.2. NDA-ammonia-cyanide reaction ................................................................................ 34

4.2.1 Optimization Excitation and Emission wavelength ................................................. 34

4.2.2 Effect of reaction time on the fluorescence of NDA-

-Cyanide product ........... 35

4.2.3 Effect of reaction temperature on the fluorescence of NDA-

-Cyanide product 36

4.2.4. Effect of ratio between NDA and cyanide on the fluorescence of NDA-

-sulfite

product ............................................................................................................................... 37

4.2.5 Apply Pertinent Parameters on determine ammonia ................................................ 38

4.3 Determine ammonia using HPLC-fluorescence system .............................................. 40

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