Study of Barium Diphenylamine 4-Sulfonate

9
Democratic and Popular Republic of Algeria
Ministry of Higher Education and Scientific Research
University of Batna2
Faculty of Medicine
Department of Pharmacy
Serie N°: ....../FM/DP/2023
A thesis entitled
Study of Barium Diphenylamine-4Sulfonate
Submitted in partial fulfillment of the requirements for the Doctor of Pharmacy Degree
Defended publicly in ……, 2023

By
SALHI Chaima
Thesis Supervisor: Pr. AYACHE Rachid Professor in Applied Physics
Examination Committee:
- HARKAT Hassina Professor in Organic Chemistry Chair
- MANSOURI Sakina Assistant Professor Class A in Physics Examiner
University Year : 2022-2023

N° Série : ....../FM/DP/2023
Mémoire de fin d’études

En vue de l’obtention du diplôme
De Docteur en Pharmacie
Thème
Étude de Barium Diphenylamine-4-Sulfonate
Présenté par :
-SALHI Chaima
Membres du jury :
- HARKAT Hassina Professeur en Chimie Organique Présidente
-AYACHE Rachid Professeur en Physique Appliquée Rapporteur
- MANSOURI Sakina Maitre Assistante (A) en Physique Examinatrice
Année universitaire : 2022-2023

LISTE DES RESPONSABLES DE LA FACULTE DE
MEDECINE.
LE DOYEN Pr. BENABBES Elmouncef
LE VICE DOYEN A LA GRADUATION Pr. LAHMAR Mourad
LE VICE DOYEN A LA POST GRADUATION Pr. DERDOUS Chawki
LE PRÉSIDENT DU CONSEIL SCIENTIFIQUE Pr. HARKAT Hassina
LISTE DES RESPONSABLES DU DEPARTEMENT DE PHARMACIE.

CHEF DE DÉPARTEMENT Dr. GUACEM Hocine
ADJOINTE DU CHEF DU DÉPARTEMENT Dr. MAKHLOUF Youcef

CHARGÉE DES ÉTUDES ET DE
L’ENSEIGNENMENT DE GRADUATION
ADJOINT DU CHEF DU DÉPARTEMENT Dr. ZAITER Thamer

CHARGÉ DE LA POST-GRADUATION ET DES
LABORATOIRES
PRÉSIDENT DU COMITÉ SCIENTIFIQUE Pr. BEN MOUSSA Mohammed Tahar

LISTE DES ENSEIGNANTS DU DÉPARTEMENT DE PHARMACIE
N° Nom &Prénom Spécialité Module(s)

enseigné(s)
PROFESSEUR
1 AYACHE Rachid Physique Physique
pharmaceutique
2 BITAM Fatma Chimie organique Chimie
pharmaceutiquegénérale
3 BOURAS Mourad Biochimie-Biologie moléculaire Biochimie structural
4 HARKAT Hassina Chimie organique Chimie
pharmaceutiqueorganiqu
e
MCA HU
5 BEN MOUSSA Mohamed Pharmacognosie Pharmacognosie
Tahar
6 GACEM Hocine Pharmacologie Pharmacologie
MCA
7 MEGHCHICHE Abdelhak Chimie analytique Chimie analytique
8 OUAHAB Ammar Génie Pharmaceutique Pharmacie industrielle
MCB HU
/ / /
MCB
9 BAZIZ Karim Biologie végétale Botanique
pharmaceutique
10 BELAZOUI Abdelouahab Informatique Biomath-Info/Biostat
11 BELDJOUDI Mouna Biochimie-biologie moléculaire Biochimie structural
12 BENSEDDIK Khadidja Biologie moléculaire Génétique
13 CHENINI Halima Chimie analytique Chimie analytique
14 DJENIDI Habiba Biotechnologie Génétique
15 DJOUIMAA Mounir Electronique Biophysique
pharmaceutique
16 FETNI Samira Biochimie-biologie moléculaire Génétique
17 GUENFOUD Fatiha Chimie organique Chimie minérale
pharmaceutique
18 HALOUI Meriem Neurosciences Biologie cellulaire
19 KHALED Meyada Pharmacologie Pharmacologie
20 MEZAACHE Rofia Chimie organique Chimie pharmaceutique
générale
21 SMAIL Hassen Electrotechnique Biophysique
pharmaceutique
22 ZAOUI Lilia Biologie animale Biologie animale
23 ZIDANI Ghania Electronique Biomath-Info/Biostat
MA HU
24 ABERKANE Ahlem Pharmacie Galénique Pharmacie galénique,
Pharmacie hospitalière
25 ACHACHI Nawel Pharmacologie Pharmacologie
26 AHMANE Amel Pharmacologie Pharmacologie
27 AISSAOUI MdalaDalal Chimie thérapeutique Chimie thérapeutique
28 AMROUNE Abdelkader Botanique médicale Botanique
pharmaceutique
29 BELAID Kaouther Pharmacognosie Pharmacognosie
30 BOUDJEMAA Soumia Toxicologie Toxicologie
31 BOUKHERBACHE Samira Toxicologie Toxicologie
32 BOULESBIAAT Karim Pharmacologie Pharmacologie
33 BOULKROUNE Ines Toxicologie Toxicologie
34 DJOUAD Seifeddine Chimie thérapeutique Chimie thérapeutique
35 HADJI Aymen Chimie Minérale Hydro-bromatologie
pharmaceutique
36 HAMICI Abderrazek Pharmacie Galénique Pharmacie galénique
37 KHANFRI Yacine Immunologie Immunologie
38 LAICHE Rafika Toxicologie Toxicologie
39 LALAYMIA Youcef Chimie Minérale Chimie minérale
pharmaceutique pharmaceutique
40 MAKHLOUF Youcef Pharmacie Galénique Pharmacie galénique
41 MEZHOUD Ines Biochimie clinique Biochimie Clinique
42 ZAITER Thamer Biochimie clinique Biochimie Clinique
MAA
43 AMRANI Iman Pharmacie clinique Pharmacie Clinique
44 AMRANI Nassima Biologie végétale Biologie végétale
45 BENMASSAOUDA Nadjet Chimie organique Chimie pharmaceutique
organique
46 BERRAK Hakima Biologie animale Biologie cellulaire
47 CHAIRA Safa Développement du médicament Pharmacie industrielle
48 ELATECHE Zahia Physique Physique
pharmaceutique
49 KADRI Keltoum Français Langues vivantes
50 MEZIANE Khadidja Mathématiques Biomath-Info/Biostat
MAB
51 GHECHAMI Naanaa Mathématiques Biomath-Info/Biostat
52 MANSOURI Sakina Physique Physique
pharmaceutique
‫ق‬
‫س‬
‫م‬
‫ا‬
‫لصيدلي‬
‫أقسم باهلل العظيم‬
‫‪.‬أمام أساتذة الكلية‪ ,‬مستشاري نظام الصيادلة‪ ,‬وأمام زمالئي‬
‫أن أشرف الذين أطروني في هذا الميدان‪ ,‬وأن أشهد – مع‬
‫‪.‬اعترافاتي ‪ -‬أ ن أبقى وفيا لمن علموني‬
‫أن أمارس مهنتي خدمة للصحة العمومية‪ ,‬و أال أحترم فقط التشريع‬
‫‪.‬الساري المفعول بل حتى مبادئ الشرف و النزاهة و اإلستقامة‬
‫أن ال أنسى مسؤولياتي و واجبي اتجاه المريض و كرامته‬
‫‪.‬اإلنسانية‬
‫أن ال أسمح في كل حال من األحوال استغالل عملي و معارفي و‬
‫‪.‬مكانتي لإلخالل باألخالق الفاضلة‬
‫فليمنحني الناس ثقتهم و تقديرهم ‪ -‬إن كنت وفيا بعهودي‪-‬‬
‫‪.‬وليتجاوزوا عن خطئي إن أخللت بشيء منها‬
‫" وهللا على ما أقول شهيد "‬
SERMENT DE GALIEN
JE JURE, EN PRÉSENCE DES MAITRES DE LA FACULTÉ, DES CONSEILLER DE

L’ORDRE DES PHARMACIENS ET DE MES CONDISCIPLES.
D'HONORER CEUX QUI M'ONT INSTRUIT DANS LES PRÉCEPTES DE MON ART
ET DE LEUR TÉMOIGNER MA RECONNAISSANCE EN RESTANT FIDÈLE Â LEUR
ENSEIGNEMENT.
D'EXERCER, DANS L'INTÉRÊT DE LA SANTÉ PUBLIQUE, MA PROFESSION

AVEC CONSCIENCE ET DE RESPECTER NON SEULEMENT LA LÉGISLATION EN
VIGUEUR MAIS AUSSI LES RÈGLES DE L'HONNEUR DE LA PROBITÉ ET DU
DÉSINTÉRESSEMENT.
DE NE JAMAIS OUBLIER MA RESPONSABILITÉ ET MES DEVOIRS ENVERS LE

MALADE ET SA DIGNITÉ HUMAINE, DE RESPECTER LE
SECRET `PROFESSIONNEL
EN AUCUN CAS, JE NE CONSENTIRAI A UTILISER MES CONNAISSANCES ET MON

ÉTAT POUR CORROMPRE LES MŒURS ET FAVORISER DES ACTES CRIMINELS.
QUE LES HOMMES M'ACCORDENT LEUR ESTIME SI JE SUIS FIDÈLE A MES

PROMESSES.
QUE JE SOIS COUVERT D'OPPROBRE ET MÉPRISE DE MES CONFRÈRES SI J'Y
MANQUE.
Acknowledgement
First and foremost, I would like to thank Almighty Allah for the courage and the patience he
has provided me to realize this modest work.
It is with great pleasure that I thank my supervisor, Prof. AYACHE Rachid, for his guidance,
help and support provided throughout the entire process.
I would like to acknowledge the jury members Prof. HARKAT Hassina and Dr. MANSOURI
Sakina who honoured me by dedicating their time to review and evaluate my work.
I would also like to thank Dr. ABERKANE Ahlem Hospital university assistant professor in
pharmaceutics. Department of Pharmacy, Faculty of Medical Sciences, University of Batna 2
for her significant assistance and guidance in conducting UV-vis spectroscopic measurements.
My greatest appreciation goes to Dr. Hacini Messaoud, the director of the Saharan Geology
Laboratory in Ouarlga, and his Engueer Mr. GADJA Omar for their invaluable assistance
regarding X-ray Diffraction Spectroscopy.
to Mr. MEGHEZZI Ahmed, Professor in Applied Chemistry, University of Biskra and Ms.
TOURTA Nacira, Engineer at Centre De Recherche Scientifique Et Technique En Analyses
Physico–Chimique CRAPC, Biskra for their precious help concerning Scanning Electronic
Microscopy.
My sincere appreciation and gratitude go to the entire team of the Laboratory for Growth and
Characterization of New Semiconductors (LCCNS), at Ferhat Abbas University of Setif 1 for
their cherished help in conducting Fourier Transform- InfraRed Spectroscopy.
My thanks are also addressed to Mr. LADJEL Segni, Professor and team leader at the
Laboratory of Process Engineering, and Mr. GHERIANI Rachid, Assistant Professor class A
in Material Physics, Kasdi Merbah University of Ouargla, for the kind help and fruitful
discussions that contributed in enriching this work.
Many thanks are also addressed to the teachers of the Pharmacy Department for their
contributions to our education. I would additionally like to thank my parents for their genuine
support and patience, much love. Finally, I would like to thank all those who have shared
their words of advice and contributed in any way to the progress of this work.
Dedication
Because none of this work would’ve been made without your constant reassurance and
availability for my rants:
To family,
To my loving mother, who has always poured me with Dua and overwhelmed me with
blessings each time I flee to her from stress and pressure of life.
To my dear father, who has been and still the primary source of encouragement and support
through the entirety of this journey.
To my two beloved sisters and brother, my lifelong friends.
To friends,
People who aren’t family, yet make us feel just as heard and supported.
To my sleepless nights and endless cups of coffee.
To Bechbouch, my feline pal who accompanied me in my solitude. You were my only

security in my chaos, offering comfort with each tender paw step -R.I.P-
This thesis is dedicated to all of you, for your boundless love, persistent sacrifices, and
unshakable belief in my abilities, you have shaped me into the person I am today, and for that,
from the depths of my soul, I am eternally grateful.
List of abbreviations
AAP: American Academy of Paediatrics NSAIDs: Non-steroidal anti-inflammatory

drugs
AHA: American Heart Association
PLT: Primed lymphocyte test
ALT: Alanine Transaminase
SEM: Scanning electronic microscope
AST: Aspartate aminotransferase
SEs: Secondary electrons
BDA4S: Barium diphenylamine-4-
sulfonate UA : Urinalysis
BSEs: Backscattered electrons UV-vis : Ultraviolet visible
CBS: Concentric Backscattered XRD : X-ray diffraction
CL: Cathodoluminescence XRPD: X-ray powder diffraction
EDS: Energy Dispersive X-

Ray Spectroscopy
EMR: Electromagnetic radiation
FT-IR: Fourier Transform Infrared
GGT: Gamma-glutamyl transferase
HOMO: Highest occupied molecular
orbital
IgG: Immunoglobulin G
IR: Infrared
KD: Kawasaki disease
LCCNS: Laboratory for Growth and

Characterization of New Semiconductors
LDH: Lactate dehydrogenase
LFD: Large Field Detector
LUMO: Least unoccupied molecular

orbital
LYM: Lymphocyte
MON: Monocyte
List of tables
Table 1 : The compound candidates used to construct colorimetric sensor array for KD
discrimination.............................................................................................................................7
Table 2 : Absorption spectrum range and substance characteristics of various substances.. .17
Table 3 : The parameters of reflections, interatomic distances and diffraction angles of
(C12H10NO3S)2Ba.......................................................................................................................35
Table 4 : Elements of (C12H10NO3S)2Ba spectrum....................................................................38
List of figures
Figure 1 : Predictor sensing compound structure.......................................................................8
Figure 2 : Structure of Barium Diphenylamine 4-Sulfonate.......................................................8
Figure 3 : Two-dimensional lattice with translation vector (b) Three-dimensional lattice with
translation vector.......................................................................................................................12
Figure 4 : Various configurations of Bravais lattices ..............................................................13
Figure 5 : An illustration of X-ray diffraction pattern..............................................................14
Figure 6 : Schematic diagram of the Lambert-Beer law...........................................................15
Figure 7 : Molecular orbitals and the energy gap needed to excite the electron energy state.. 17
Figure 8 : Measurement principle in UV/VIS spectroscopy.....................................................18
Figure 9 : Scheme of the optical spectrum, focusing on the infrared region............................19
Figure 10 : The interaction of electron beam with specimen and the signal emitted from the
sample.......................................................................................................................................23
Figure 11 : BTX™ III Benchtop XRD Analyzer......................................................................27
Figure 12 : HighScore Plus Software used...............................................................................27
Figure 13 : Scanning Electronic Microscope brand PHILIPS / FEI QUANTA 250 used........28
Figure 14 : The double-beam spectrophotometer Analytik Jena..............................................29
Figure 15 ; Aspect UV Software used......................................................................................30
Figure 16 : The SHIMADZU Fourier-transform infrared spectrophotometer used.................31
Figure 17 : Conductivity meter WTW LF 320 of physics laboratory at Pharmacy Department-
BATNA-...................................................................................................................................31
Figure 18 : A.KRUSS DR 500 Refractometer used.................................................................32
Figure 19 : XRD Pattern of barium diphenylamine -4- sulfonate............................................35
Figure 20 : SEM micrographs of C12H10NO3S)2Ba powder grains with diameter of 200 nm...36
Figure 21: EDX Elemental Analysis spectrum.........................................................................37
Figure 22 : A x10 000 close-up of the grain sample.................................................................37
Figure 23: UV/vis Spectra of Barium Diphenylamine-4-Sulfonate.........................................38
Figure 24 : FT-IR Spectrum of Barium Diphenylamine-4-Sulfonate.......................................39
Figure 25 : Variation of the electrical conductivity as function of concentration....................41
Figure 26: Variation of Electrical Conductivity as function of Temperature...........................42
Figure 27 : The relationship between concentration and refractive index of (C12H10NO3S)2Ba
solutions....................................................................................................................................43
Contents
Acknowledgment
Dedication
List of abbreviation
List of tables
List of figures
General Introduction
CHAPTER I:
GENERALITIES ON BARIUM DIPHENYLAMINE -4- SULFONET
Introduction.......................................................................................................................
1. Chemical structure of Barium Diphenylamine 4-Sulfonate .........................................
2. Previous studies on Barium Diphenylamine 4-Sulfonate.............................................
CHAPTER II CHARACTERIZATION TECHNIQUES
3. Spectroscopic techniques used in the characterization of Barium Diphenylamine
4-Sulfonate..................................................................................................................
3.1 X-Ray diffraction........................................................................................................
3.1.1 Introduction .............................................................................................................
3.1.2 Crystal structure ......................................................................................................
3.1.3 X-ray diffraction principle.......................................................................................
3.1.4 Applications of PXRD in Pharmaceutical Sciences ................................................
3.2 UV Visible spectrophotometry....................................................................................
3.2.1 Introduction .............................................................................................................
3.2.2 Principles of UV-visible spectrophotometry............................................................
3.2.2.1Lambert–Beer Law ................................................................................................
3.2.2.2Basic Principle of UV-Vis Spectrophotometry......................................................
3.2.2.3Measurement principle ..........................................................................................
3.2.3 Applications of UV-visible
spectrophotometry in pharmaceutical field .............................................................
3.3 Fourier transform-infrared (FT-IR) spectroscopy ......................................................
3.3.1 Introduction .............................................................................................................
3.3.2 Principle of Fourier transform infrared (FTIR) spectroscopy .................................
3.3.3 Application of Fourier transform infrared (FT-IR) spectroscopy
in pharmaceutical field ...........................................................................................
3.4 Scanning Electron Microscopy (SEM) ......................................................................
3.4. Introduction...............................................................................................................
3.4.2 Fundamental Principles of SEM .............................................................................
3.4.3 Application of SEM in pharmaceutical field ...........................................................
Experimental Part
I. Materials and Methods...................................................................................................
1. Preparation method: .....................................................................................................
2. Protocol of the solutions preparation ...........................................................................
3. X- ray diffraction XRD.................................................................................................
4. Scanning Electron Microscopy.....................................................................................
5. UV Visible Spectrophotometry ....................................................................................
6. Fourier transform infrared (FT-IR) spectroscopy ........................................................
7. Electrical Conductivity .................................................................................................
8. Refractive Index ...........................................................................................................
Results & Discussion........................................................................................................
I. X-ray Diffraction...........................................................................................................
1 Structural identification..................................................................................................
2. Indexing and determination of lattice parameters.........................................................
3. Crystal structure ...........................................................................................................
II Scanning Electronic Microscopy ..................................................................................
III. UV/vis Spectroscopy ..................................................................................................
IV. Fourier Transformed-InfraRed....................................................................................
V. Electrical conductivity .................................................................................................
VI. Refractive Index..........................................................................................................
Conclusion & Perspectives................................................................................................
Abstract
General
Introduction
INTRODUCTION
Barium Diphenylamine-4-sulfonate (BDA4S) is a versatile compound that has been

extensively studied for its potential applications in various fields such as medicine and
industry. BDA4S acts as a Redox Indicator in Spectrophotometric Micro-determination of
Non-Steroidal Anti-Inflammatory Drugs [1] and has also been utilized in the diagnosis of
lung cancer through the analysis of exhaled breath with a colorimetric sensor array [2].
Additionally, BDA4S has demonstrated promise in the determination of volatile reducing
substances in blood and gases [3] as well as in a urinary colorimetric sensor array to
distinguish Kawasaki Disease from other febrile illnesses [4].
Kawasaki Disease (KD) is an acute febrile illness primarily affecting young children and
associated with the risk of coronary artery aneurysms (5). The absence of a specific diagnostic
test for KD presents a significant challenge to accurately diagnose and promptly treat the
disease. Consequently, the development of a simple and cost-effective colorimetric sensor
array employing BDA4S is of great interest to researchers in this field.
The objective of this study is to conduct a comprehensive physic-chemical quality control

analysis of BDA4S to ensure its suitability for further pharmaceutical industry production.
Various spectroscopic approaches, including X-ray diffraction (XRD), Scanning Electron
Microscopy (SEM), Ultraviolet-visible (UV-vis), Fourier Transform Infra-Red (FTIR),
refractive index, and electrical conductivity, will be employed to investigate the physic-
chemical properties of BDA4S. These analytical techniques are widely utilized to determine
the structure, purity, and quality of chemical compounds.
This typescript is divided into three distinct parts, each contributing to a comprehensive
understanding of the subject matter. The first part comprises a literature review, which is
presented in two chapters. The initial chapter provides an overview of general concepts and
knowledge pertaining to barium diphenylamine 4 sulfonate. The subsequent chapter focuses
on various analysis techniques employed for the identification and characterization of this
compound.
The second part of the thesis is condensed into a single chapter, wherein the preparation
methods and a range of analysis techniques for the characterization of barium diphenylamine
4 sulfonate are summarized. The highlighted techniques include UV-vis, XRD, FTIR, SEM,
electrical conductivity measurements, and refractive index analysis.
2
The third and final part of this thesis delves into the results obtained from the aforementioned
analyses and presents their interpretation. This section aims to establish connections between
the experimental findings and the underlying principles of barium diphenylamine 4 sulfonate.
By elucidating the implications of these results, this part serves to enhance our comprehension
and contribute to the overall body of knowledge in this field of study.
3
Literature
Review
CHAPTER I:
GENERALITIES ON BARIUM
DIPHENYLAMINE -4- SULFONET
5
CHAPTER I GENERALITIES ON BARIUM DIPHENYLAMINE -4- SULFONATE
Introduction
In 1967, a Japanese doctor named Kawasaki was the first to describe a syndrome
characterized by mucocutaneous lymph node involvement, now known as Kawasaki disease
[6], is a short-term inflammation of medium-sized blood vessels that predominantly affects
the coronary arteries [7]. It mainly affects children under the age of five and is rare among
older individuals It has experienced a significant rise worldwide, particularly in the last 20
years [8].
It is the primary contributor to acquired heart conditions in developed countries and is
gradually surpassing rheumatic heart disease as a major concern in developing nations [7].
Various theories have been proposed regarding the cause of KD. Presently, it is widely
accepted that there is a genetic predisposition to developing KD, and it is believed that an
unidentified infectious factor also plays a role. Recent evidence indicates that genetic factors
play a significant role in the occurrence of KD. Specific variations in the IgG receptor have
been identified, which can heighten the susceptibility of children to KD and increase the
likelihood of developing coronary artery aneurysms [9].
A reliable method to accurately diagnose Kawasaki disease (KD) in children is by considering

their age and measuring various biomarkers such as % MON, phosphorus, UA, globulin, %
LYM, prealbumin, GGT, AST/ALT ratio, serum chloride, LDH, and PLT. This novel
diagnostic approach proves effective in distinguishing children with KD from those with other
febrile illnesses. Implementing this diagnostic model enables accurate identification of KD
cases [10].
These tests contribute to the high cost and long-time associated with the diagnostic process,
based on the information given in the estimation of the cost of Nonadherence to Kawasaki
Disease Diagnostic Recommendations that have been published by the American Heart
Association (AHA) and American Academy of Paediatrics (AAP) in 2004. The estimated
cost of the diagnostic tests per patient among 113 studied cases with suspected Kawasaki
disease (KD) is approximately $5,868. This cost includes clinical assessment, laboratory tests,
and echocardiograms [11].
6
Hence, there is a strong need and urgency to prioritize the creation of an affordable, quick,
and convenient alternative diagnostic test for Kawasaki disease that can be conducted directly
at the point of care.
The application of colorimetric array-based sensing is a robust approach for quantitatively
detecting a wide range of analytes through the recognition of distinct patterns using multiple
sensing compounds. Various classes of sensing compounds are commonly employed in
colorimetric sensors, including metalloporphyrin, Bronsted acid/base dyes, solvatochromic
dyes, and redox indicators. Redox indicators, encompassing both metal-organic complexes
and true organic redox systems, exhibit a clear and reversible colour change between their
oxidized and reduced forms.
Among the 190 candidate compounds an optimal subset of 11 sensing compounds utilized in
the assembly of colorimetric sensor arrays for diagnosing Kawasaki disease (table 1), one
notable compound is barium diphenylamine 4 sulfonate [4].
Table 1 : The compound candidates used to construct colorimetric sensor array for KD
discrimination [4].
7
Figure 1 : Predictor sensing compound structure [4].
1. Chemical structure of Barium Diphenylamine 4-Sulfonate

Barium diphenylamine 4-sulfonate is a chemical compound with the molecular formula
(C12H10NO3S)2Ba. BDA4S is a white, odorless powder with a molecular weight of
approximately 633.88 g/mol. It exhibits a melting point of around 300°C, indicating its
transition from a solid to a liquid state. At 20°C, it exists as a solid, and it is slightly soluble in
water, meaning it can dissolve to a limited extent [12].
8
Figure 2 : Structure of Barium Diphenylamine 4-Sulfonate
2. Previous studies on Barium Diphenylamine 4-Sulfonate

Barium diphenylamine-4-sulfonate, renowned for its unique properties and versatile nature,
holds immense significance in various industrial and scientific applications, particularly in the
pharmaceutical field. Its value extends to cutting-edge diagnostic techniques, where it serves
as a colorimetric sensor array for the diagnosis of lung cancer through the analysis of exhaled
breath. By detecting specific biomarkers, barium diphenylamine-4-sulfonate contributes to the
early detection and monitoring of this devastating disease, offering potential avenues for
improved patient outcomes [2].
Furthermore, this compound plays a crucial role as an indicator in the determination of

volatile reducing substances, such as alcohol or ether, in both blood and gases. Its precise and
sensitive nature enables it to function as a reliable indicator during chromic acid titration,
facilitating accurate measurements in analytical procedures. This application finds relevance
in forensic analysis and various medical investigations [3].
In the field of pharmaceutical research and analysis, barium diphenylamine-4-sulfonate serves

as a redox indicator in the spectrophotometric micro-determination of non-steroidal anti-
inflammatory drugs (NSAIDs). Through its involvement in this analytical technique, it
enables the quantification and characterization of NSAIDs, contributing to the development of
safer and more effective medications [1].
9
CHAPTER II
CHARACTERIZATION
TECHNIQUES
3. Spectroscopic techniques used in the characterization of

Barium Diphenylamine 4-Sulfonate
3.1 X-Ray diffraction
3.1.1 Introduction
In 1912, Max von Laue and his colleagues made the significant discovery that crystalline
materials behave like three-dimensional diffraction gratings when exposed to X-ray
wavelengths that align with the spacing of planes within the crystal lattice (Friedrich et al.,
1912) Currently, X-ray diffraction has become a widely used method for investigating crystal
structures and the distances between atoms [13]. XRD is a non-invasive method of testing that
can be used to analyse a diverse range of substances, such as minerals, polymers, plastics,
metals, semiconductors, ceramics, and solar cells [14]. While X-ray crystallography finds
extensive industrial applications, it continues to be a complex discipline of research. Many
studies have explored the various uses of XRD, but there is a scarcity of comprehensive
reviews focusing on technical details of crystal structures and XRD [15].
3.1.2 Crystal structure
Crystalline structures consist of arrays of atoms arranged in a repetitive and orderly manner.
The fundamental building block of a crystal is called a unit cell, and its size and shape (as
shown in Figure 3) are determined by the angles between the axes (α, β, γ) and the lengths of
the three axes (a, b, c) in a three-dimensional system [16]. Atoms within an array are
methodically arranged by their positions, either through translation or transformation, without
any alteration in terms of orientation or rotation. The translation can occur in one, two, or
three dimensions, depending on the specific type employed [17]. A crystal's regular
arrangement of points is referred to as a lattice. Figure (3a) and (3b) depict the lattice structure
of crystals in two and three dimensions, respectively.
11
Figure 3 : Two-dimensional lattice with translation vector (b)

Three-dimensional lattice with translation vector [17].
In 1848, Bravais introduced the mathematical concept of a space lattice to describe the
arrangement of crystal structures (Figure 4). The space lattice demonstrates the scattering of
an infinite number of points in space, highlighting that the arrangement of points around one
point is comparable to that around any other point [18]. The arrangement of points within a
space lattice is defined using the x, y, and z axes. Figure 4 illustrates 14 lattices that represent
all possible arrangements of points within a three-dimensional space lattice. These 14 Bravais
lattices can be classified into 7 crystal systems based on the angles between the axes, their
lengths, and their symmetry properties.
12
Space groups in crystallography describe the symmetry of crystals, indicating how their
orientation can change without affecting the atomic positions. These changes include
translations, reflections, rotations, and inversions. The combination of these transformations
results in 230 distinct space groups that categorize the inherent symmetry of crystals [19],
[20], [21], [22], [23]
3.1.3 X-ray diffraction principle

X-ray diffraction relies on the constructive interference of monochromatic X-rays with a
crystalline sample. The X-rays are generated by a cathode ray tube, filtered for
monochromatic radiation, and focused onto the sample. When the incident X-rays interact
with the sample, constructive interference occurs, producing a diffracted ray. This
phenomenon follows Bragg's law:
nλ=2dhklsinθ
where n represents an integer, λ is the wavelength of the X-rays, d denotes the interplanar
spacing responsible for the diffraction, and θ represents the angle of diffraction and dhkl is the
spacing of the crystal layers (path difference), which relates the wavelength of X-rays, the
diffraction angle, and the interplanar spacing in the crystal lattice.
The diffracted X-rays are then detected, processed, and counted. By scanning the sample at
various angles, all possible diffraction directions of the lattice can be obtained. The resulting
13
diffraction peaks can be converted into d-spacings, which are unique for each compound and
can be used for compound identification. X-ray diffractometers consist of three main
components: X-ray tube, a sample holder, and an X-ray detector. X-rays are generated by
heating a filament in the cathode ray tube, accelerating electrons towards a target, and causing
characteristic X-ray spectra to be emitted. These spectra typically include components such as
Ka and Kb [24].
3.1.4 Applications of PXRD in Pharmaceutical Sciences

Experimental screening is commonly employed to explore the various possible solid forms
(polymorphs, hydrates/solvates, salts, co-crystals, amorphous) of pharmaceutical compounds.
The properties of different solid forms of the same drug can significantly differ, impacting
crucial factors such as solubility, dissolution, bioavailability, stability, processability, and
shelf life. Therefore, it is crucial to understand the different solid forms and their relationships
for the successful commercialization of a candidate molecule. X-ray powder diffraction
(XRPD) serves as a primary tool for characterizing solid forms and is extensively used during
the drug development process to ensure the reproducibility of the selected form [25].
3.2 UV Visible spectrophotometry

3.2.1 Introduction
UV-visible spectroscopy is a versatile and cost-effective analytical technique that can be used
for a broad range of organic and some inorganic compounds. This non-destructive method is
both simple and flexible. It operates by measuring the absorption or transmission of light
through a medium as a function of wavelength using UV-vis spectrophotometers [26].
3.2.2 Principles of UV-visible spectrophotometry

3.2.2.1 Lambert–Beer Law
The Lambert-Beer law forms the foundation for quantitatively analysing liquid parameters
through UV-Vis spectroscopy.
14
Figure 6 : Schematic diagram of the Lambert-Beer law.

This analytical approach is based on the principle of measuring the interaction between a
beam of monochromatic parallel light and the tested medium's surface [27]. As the light
passes through the medium with a specific thickness, the medium absorbs a portion of the
light energy, resulting in a reduction in the intensity of the transmitted light. The absorbance
of the medium being analysed is directly proportional to its thickness.
The mathematical representation of the Lambert-Beer law can be expressed as follows:
A = log(1/T) = ε · c · l (1)
where A represents the absorbance of the sample, T is the transmittance of light through the
sample, ε is the molar absorptivity or molar absorption coefficient, c is the concentration of
the compound, and l is the path length that the light travels through the sample.
3.2.2.2 Basic Principle of UV-Vis Spectrophotometry
UV-Vis spectroscopy operates on the principle that molecules can selectively absorb light
within the UV-Vis wavelength range. When light of a specific wavelength is absorbed, it
excites electrons from a lower energy orbital (HOMO) to a higher energy unoccupied orbital
(LUMO). The energy of the absorbed light must be equal to the energy gap between the
HOMO and LUMO (HOMO-LUMO energy gap).
In the case of conjugated systems, where there are alternating single and multiple bonds, the
energy gap between the HOMO and LUMO is smaller compared to isolated double [28].
15
Figure 7 : Molecular orbitals and the energy gap needed to excite the
electron energy state.
Different molecules exhibit distinct absorption characteristics, leading to unique spectral

curves. However, a majority of molecules demonstrate light absorption within the UV-Vis
region. By leveraging the Lambert-Beer law as a theoretical framework, it becomes possible
to effectively measure the concentration of molecules in solution. Parameters commonly
utilized in water quality assessment, such as the spectral absorption range for substances like
NO3-N and NO2-N, typically fall within the 200-250 nm range. Organic matter and turbidity,
on the other hand, are typically absorbed within the 380-750 nm range.
Table 2 : Absorption spectrum range and substance characteristics of various substances.
16
3.2.2.3 Measurement principle

To determine the intensity of light passing through a sample solution in a cuvette, a UV-vis
spectrophotometer measures it and compares it to the intensity of the light before it passed
through the sample. The main parts of a UV-vis spectrophotometer include a light source, a
sample holder, a dispersive device that separates different light wavelengths (such as a
monochromator), and a suitable detector [29].
Figure 8 : Measurement principle in UV/VIS spectroscopy
3.2.3 Applications of UV-visible spectrometry in pharmaceutical

field
In the process of developing drugs, analysis is an essential component that covers everything
from the initial discovery stage to the quality control of the final products. Depending on the
specific stage of development, different analysis methods are necessary, taking into account
factors such as the amount of material available, the need for speed and accuracy, selectivity
requirements, ease of use, and available resources. During the preformulating phase of drug
development, which focuses on physicochemical profiling, the properties of the active
molecules dictate which methods are appropriate for analysis and characterization. One
widely used method in pharmaceutical analysis is UV-vis spectrophotometry, either alone or
in combination with a separation technique. The reason for its broad usage is that most drug
substances have chromophores that absorb light somewhere between 190-800 nm, which the
UV-vis absorption spectrum can detect. This spectrum is determined by the molecule's
structure and can assist in identifying compounds, as well as determining physical and
chemical properties such as pKa, partitioning, and complexation. However, the primary use of
17
UV-vis spectrophotometry in pharmaceutical analysis is to measure the amount of drug

substances present [30].
3.3 Fourier transform-infrared (FT-IR) spectroscopy

3.3.1 Introduction
Spectroscopic techniques have been used for material analysis in laboratories for many years.
In the past, infrared (IR) spectroscopy was primarily used for qualitative analysis, providing
general information about a wide range of samples. However, advances in chemometrics,
software algorithms, and instrumental technology have enabled efficient artificial intelligence
techniques to be applied to IR spectroscopy, making it a powerful quantitative analytical
method. Fourier transform infrared (FT-IR) spectroscopy is a modern and popular technique
that has revitalized IR spectroscopy as a reliable and powerful analytical tool. IR spectroscopy
involves the absorption of energy from passing electromagnetic radiation in the IR frequency
range, resulting in several excited molecular vibrational and rotational states that produce a
unique and highly characteristic spectrum. Recent developments in FT-IR techniques have
made the tool suitable for both qualitative and quantitative analysis purposes [31].
3.3.2 Principle of Fourier transform infrared (FTIR) spectroscopy

Invisible to the human eye, IR radiation consists of electromagnetic waves (EMR) with
wavelengths longer than visible radiation. The IR portion of the electromagnetic spectrum
spans wavelengths ranging from 0.8–100 µm, and is typically divided into three categories:
near-IR, mid-IR, and far-IR. The mid-IR range, which includes radiation in the wavenumber
interval from 4000 cm−1 to 400 cm−1, is most commonly used in medical applications. The
frequency of the absorbed radiation determines each subatomic vibrational interaction, as
demonstrated in (figure 9).
18
Figure 9 : Scheme of the optical spectrum, focusing on the infrared

region
FT-IR spectroscopy is a technique used to obtain the absorption or emission infrared spectrum
of solids, liquids, or gases. The advantage of FT-IR spectrometry over dispersive
spectrometry is that it simultaneously collects high-resolution information over a broad
spectral range (between 4000 and 400 cm−1). Spectroscopy techniques, such as FT-IR or UV-
vis spectroscopy, aim to quantify the amount of light absorbed by a sample at each frequency.
The dispersive spectroscopy method involves focusing a monochromatic light beam at a
sample, measuring the amount of absorbed light, and recalculating it for each frequency. In
contrast, Fourier transform spectroscopy uses a less intuitive approach to obtain similar data.
This method focuses a beam, or array, that contains multiple frequencies of light and
measures how much of that beam is absorbed by the sample. Then, the wave is changed to
contain a different combination of frequencies, giving a second data point.
This process is repeated many times in a short period of time, and the information is obtained
by a computer. An interferogram, such as the one shown in (Figure 9), is created by applying
a broadband light source containing the entire range of frequencies to be measured. The light
passes through a Michelson interferometer, which consists of a special array of mirrors, one
of which is moved by a motor. As this mirror moves, each light frequency in the array is
occasionally blocked, reflected, refracted, or transmitted by the interferometer. The different
frequencies are modulated at different rates so that the array exiting the interferometer has a
different range at each mirror position or second [32].
19
3.3.3 Application of Fourier transform infrared (FT-IR)

spectroscopy in pharmaceutical field
Different techniques and methods have been used to examine pharmaceutical preparations and
understand changes that occur in order to develop effective drug dosage forms. Among these
techniques, FT-IR has shown to be highly versatile and useful for drug research purposes. It
can provide information on compound structures, confirm drug synthesis, and allow for drug
characterization and microstructure observation. Additionally, FT-IR has been successful in
detecting drug preparations in bio-samples. Due to its various applications in the field of
pharmaceuticals, FT-IR is a valuable tool for drug development and analysis [33].
3.4 Scanning Electron Microscopy (SEM)

3.4.1 Introduction
The SEM is a highly versatile and advanced instrument used to observe surface phenomena of
materials. The sample is bombarded with high-energy electrons in the SEM, and the resulting
outcoming electrons/X-rays are analysed. These provide information on the topography,
morphology, composition, and crystallographic properties of the material. Morphology relates
to the object's shape and size, while topography describes its surface features such as texture,
smoothness, or roughness. Composition refers to the elements and compounds that make up
the material, while crystallography pertains to the arrangement of atoms within the material.
The SEM is the leading instrument that can produce a highly detailed visual image of a
particle with a high spatial resolution of up to 1 nm, and magnifications up to 300,000 times.
Although SEM provides information only on the surface of the material, it is still a powerful
tool for characterizing crystallographic, magnetic, and electrical features of the sample, and
for determining whether any morphological changes have occurred after modifying the
sample surface with other molecules. The SEM can provide qualitative information on the
topography, morphology, composition, and crystallographic properties of the specimen,
making it a versatile instrument for examining and analysing materials with high resolution
[34].
3.4.2 Fundamental Principles of SEM

20
In order to use SEM, a sample must be fixed onto a stub using double-sided carbon tape. A
thin layer of material should then be added on top of the carbon tape to reduce charging and
improve image quality. However, non-conductive samples such as polymers must be sputter-
coated with a conductive material like carbon or metal to avoid overcharging. Once the
sample is prepared, it is placed in the sample holder within the vacuumed specimen chamber.
SEM operates under a vacuum to prevent interactions between electrons and gas molecules
that would reduce resolution. The primary electrons produced by the electron gun are
accelerated to a high energy level and focused into a monochromatic beam using magnetic
field lenses and metal slits. The beam is scanned across the sample surface by scanning coils
in a raster pattern. When the primary electrons hit the sample surface, they interact with the
near-surface area of the sample in several ways, generating signals from both elastic and
inelastic scattering.
The interaction volume and scattering of electrons in SEM depend on several factors. The
concentration of atoms and atomic number of the element in the sample, as well as the
accelerating voltage, can affect the interaction volume and scattering. Increasing the
accelerating voltage leads to an increase in the interaction volume and scattering, while higher
atomic number materials absorb or stop more electrons, resulting in a smaller interaction
volume. The angle of incidence of the electron beam also plays a role, with a greater angle of
incidence resulting in a smaller interaction volume. In summary, the angle of incidence,
atomic number, and accelerating voltage are the primary factors that determine the volume of
the specimen in which interactions occur.
As a result of the interaction between incoming electrons and the specimen's nucleus and
electrons through Coulomb field, various signals are emitted such as secondary electrons
(SEs), backscattered electrons (BSEs), photons (X-rays used for elemental analysis) and
visible light (Cathodoluminescence - CL). These signals are collected by detectors and
processed by a computer to form the desired image. Different information about the sample
can be observed depending on the detected signal, with secondary electrons being the most
important for indicating sample morphology and topography, while backscattered electrons
are used for demonstrating contrasts in multiphase samples. X-rays are generated when
incident electrons collide with electrons in the orbitals of sample atoms, causing them to be
excited to higher energy levels and then emit X-rays with a specific wavelength when they
return to lower energy levels. Each element generates a characteristic X-ray, which allows for
21
elemental analysis. SEM is a non-destructive technique, and repeated analysis of the same
material can be done as the generation of X-rays does not lead to any loss in the specimen's
volume.
The interactions that occur between the electron beam and the specimen atoms can be broadly
classified into two types: inelastic and elastic interactions. In inelastic interactions, the beam
electron interacts with the electric field of a specimen atom electron, transferring energy to the
atom and potentially ejecting a secondary electron (SE) with an energy of less than 50 eV.
The creation of vacancies by the ejected electrons leads to the emission of X-rays, which are
characteristic of the energy transition involved.
Elastic interactions occur between the primary electrons and the electric field of the nucleus
of a specimen atom, causing the direction of the primary electrons to change with minimal
energy loss (less than 1 eV). When these elastically scattered electrons deflect out of the
specimen, they are called backscattered electrons (BSEs) and typically maintain at least 50%
of the incident beam energy. These interactions cause the beam electrons to distribute over a
three-dimensional "interaction volume", with secondary and backscattered electrons escaping
from different depths of the sample, resulting in different energies.
SEs generally escape from depths of approximately 5-50 nm, while BSEs escape from several
times greater depths, and X-rays from even greater depths. This means that greater escape
depths can result in wider lateral dimensions for signal generation and lower potential
resolutions. However, the actual size and shape of the interaction volume depend on several
factors, including the accelerating voltage, atomic number, and tilt [35].
22
Figure 10 : The interaction of electron beam with specimen and the signal emitted from the
sample
3.4.3 Application of SEM in pharmaceutical field

In the dynamic landscape of pharmaceutical research, the demand for comprehensive
information has spurred the adoption of advanced tools like scanning electron microscopes
(SEMs), revolutionizing the field and unlocking new possibilities. These sophisticated
instruments have proven to be indispensable powerhouses, empowering scientists to explore
intricate cellular interactions with unprecedented precision and unravel the mysteries of
pharmaceutical compounds.
Within the realm of pharmaceutical research, SEMs have emerged as vital tools for acquiring
invaluable insights into the complex world of cells when exposed to novel drugs. By
harnessing the remarkable resolution capabilities of SEMs, researchers can capture highly
detailed images of cellular structures, allowing them to examine the profound effects of
pharmaceutical compounds on cellular behaviour. These visualizations enable scientists to
23
decipher drug mechanisms, optimize formulations, and design more targeted and efficient
treatment strategies.
Moreover, SEMs have catalysed breakthroughs in the most challenging area of

pharmaceutical research: cancer treatments. Given the multifaceted nature of cancer,
understanding the intricate dynamics within tumour microenvironments is essential for
developing effective therapies. SEMs provide researchers with a transformative perspective,
enabling them to study cancer cells at a remarkably detailed level. By visualizing
morphological changes, investigating drug-target interactions, and scrutinizing cellular
responses, SEMs facilitate the discovery of novel therapeutic approaches, paving the way for
personalized medicine and improving patient outcomes.
The significance of SEMs extends beyond cellular exploration, as they also play a pivotal role
in powder imaging and analysis in the pharmaceutical industry. Precise characterization of
powders is paramount in drug manufacturing, as it directly impacts critical factors such as
dissolution rate, stability, and bioavailability. SEMs excel in this domain, delivering accurate
measurements of particle size, shape, and distribution. Armed with this knowledge,
researchers can optimize formulation processes, evaluate product quality, and ensure
consistent and predictable therapeutic outcomes [36], [37], [38].
24
Experimental
Part
MATERIALS AND METHODS
I. Materials and Methods

1. Preparation method
In this section, we describe the preparation protocol employed for the synthesis of the target
compound. A balloon equipped with a refrigerant was utilized as the reaction vessel. Initially,
5g of diphenylamine and 4ml of concentrated sulfuric acid were introduced into the balloon.
The resulting mixture was then agitated at a temperature of 100°C for a duration of 30
minutes to ensure thorough reaction progress. Subsequently, 10ml of water was carefully
added to the mixture, followed by an additional agitation period of 20 minutes. To facilitate
further processing, the mixture was transferred to 80ml of hot water, and 20ml of 50% weight
concentration barium hydroxide solution was added. This addition resulted in the formation of
a white precipitate. The precipitate was subsequently subjected to filtration, thorough
washing, and drying procedures to obtain the desired product.
2. Protocol of the solutions preparation

The preparation of six solutions of barium diphenylamine 4-sulfonate was conducted
following a meticulous protocol. A precisely measured amount of 100 mg of barium
diphenylamine 4-sulfonate was dissolved in 90 ml of distilled water. The solid was added to
the water and stirred vigorously using a stirring rod until complete dissolution was achieved.
The resulting solution was then divided equally into six separate containers, ensuring each
container contained approximately 15 ml of the solution. To obtain a series of dilutions, each
container underwent a 50% dilution by adding 7.5 ml of distilled water and thorough mixing.
This dilution process was repeated for the remaining five containers using fresh distilled
water for each dilution step. The containers were properly labelled to indicate the respective
dilution factors.
26
3. X- ray diffraction XRD

The X-ray diffraction analysis was carried out within Geology Laboratory, Kasdi Merbah
University of Ouargla using a brand diffractometer the BTX™ III XRD analyser (figure 11)
offers reliable quantitative mineralogy of major and minor components in a compact,
benchtop design. Powerful software is paired with an improved X-ray detector for increased
speed and sensitivity.
Figure 11 : BTX™ III Benchtop XRD Analyzer
A complete full powder pattern analysis Software HighScore Plus is used to identify the XDR
patterns of the compound (figure 12).
27
Figure 12 : HighScore Plus Software used
4. Scanning Electron Microscopy

The CRAPC's scanning electron microscope (figure 13) comes with two types of sensors: the
CBS and the LFD. The CBS, known as Concentric Backscattered, functions in a high vacuum
mode and produces an image with chemical contrast. On the other hand, the LFD, or Large
Field Detector, detects secondary electrons and enables working at pressures up to 2 mbar. It
is particularly useful for capturing images of both secondary and backscattered electrons at
the same time.
28
Figure 13 : Scanning Electronic Microscope brand PHILIPS /

FEI QUANTA 250 used
5. UV Visible Spectroscopy
The double-beam spectrophotometer Analytik Jena (Figure14) at the level of the Galenic
Pharmacy Laboratory, Department of Pharmacy BATNA, was used to analyse the absorption
spectra of BDA4S. It is equipped with two lamps; the first one is a halogen lamp used for
measuring optical density in the visible range, while the second one is a deuterium lamp used
for measuring optical density in the ultraviolet range. In our experiments, BDA4S at specific
intervals were placed in a quartz cuvette to monitor their photodecomposition. The
29
characteristic absorption peak (λmax) was measured within a range of 900 nm and speed of
5nm/s, with respect to distilled water used as a reference.
Figure 14 : The double-beam spectrophotometer Analytik Jena
To operate a spectrophotometer, first, a blank measurement is taken by adding the solvent

(such as water) into a transparent cuvette and passing a light beam through it. The transmitted
light at different wavelengths is then measured by a detector positioned after the cuvette,
which serves as a reference for later measurements.
To measure a sample, it is dissolved in the solvent and added to the cuvette. The light beam is
then passed through the cuvette containing the sample, and the sample molecules absorb some
of the light at different wavelengths.
The transmitted light is then measured by the detector, and the intensity change at different
wavelengths is calculated by dividing the transmitted intensity of the sample solution by the
corresponding values of the blank. This ratio is then recorded by the software ASpect UV
(figure 15) for the recording and analysis of UV-vis data.
30
Figure 15 ; Aspect UV Software used
6. Fourier transform infrared (FT-IR) spectroscopy

The purpose of this technique is to gather information about the analysed product by studying
its interaction with radiation. Molecules absorb infrared radiation within the frequency range
of 4000 to 400 cm-1 as a result of molecular vibrational energy. The analysis of the studied
products was carried out at the Laboratory for Growth and Characterization of New
Semiconductors (LCCNS) at Ferhat Abbas University of Setif 1, using a SHIMADZU
Fourier-transform infrared spectrophotometer (Figure 16). The infrared spectra were recorded
in transmittance mode, covering the frequency zone of 3500-500 cm -1, which facilitates the
identification of different functional groups present in the compounds.
31
Figure 16 : The SHIMADZU Fourier-transform infrared spectrophotometer used
7. Electrical Conductivity
The electrical conductivity of each solution was measured using a conductivity meter WTW
LF320. All experiments were conducted at room temperature (25°C) and atmospheric
pressure in the Laboratory of Physics at Pharmacy Department (figure 17).
Figure 17 : Conductivity meter WTW LF 320 of physics laboratory at Pharmacy Department-

BATNA-
32
Before using the conductometer, it is calibrated using a standard solution of known

conductivity. This ensures that the device is accurate and provides reliable results.
The conductometer probe, which contains two electrodes, is then immersed into the solution.
The electrodes are completely submerged and do not touch the sides or bottom of the
container.
Once the probe is immersed, the conductometer will display the conductivity value of the
solution on the screen. The reading can be recorded or stored for further analysis.
After taking the measurement, the probe is thoroughly rinsed with distilled water to prevent
any contamination between readings.
8. Refractive Index
the refractive index of (C12H10NO3S)2Ba solutions are measured using Automatic Digital
Refractometer branded A.KRUSS DR 500 (figure 18). at the Laboratory of Physics in
Pharmacy Department-BATNA-
Figure 18 : A.KRUSS DR 500

Refractometer used
33
Results
&
Discussion
RESULTS & DISCUSSION
I. X-ray Diffraction
X-ray diffraction is a technique employed to determine the composition and structure of
crystalline materials, as well as to confirm the non-crystalline state of certain substances. In
the case of crystalline materials, where atoms are arranged in an orderly and periodic manner,
lattice planes designated by Miller indices (h k l) are formed. When a crystal is illuminated
with X-rays, a diffraction pattern emerges, consisting of distinctive peaks associated with the
diffracting lattice planes. The position of each peak, known as the diffraction angle θ, relies
on the orientation and interplanar distance of the diffracting planes, following Bragg's law.
The synthesized products underwent analysis using X-ray diffraction (XRD) with a copper
anticathode apparatus (λkα=1.54060 Å). The voltage acceleration was set at 40 kV and the
current at 40 mA. The detector scanned the angular range from 5° to 90°, with a fixed step
size of 0.019° and a scanning speed of 9.4 seconds per step.
1. Structural identification
Structural identification is the primary use of the powder method, which involves determining
the specific crystalline species being studied. It can also be employed to qualitatively analyse
the presence of multiple crystalline species within a material. This identification process relies
on accurately determining the positions of peaks and estimating their relative intensities based
on their heights.
2. Indexing and determination of lattice parameters

Indexing involves the assignment of Miller indices (hkl) to each diffraction peak, which
depends on the knowledge of the crystallographic lattice type (e.g., cubic, hexagonal,
tetragonal, etc.). To accomplish this, the crystal system must be determined first, followed by
the definition of the appropriate indices (hkl). This search is typically conducted using
dedicated calculation programs and tailored algorithms, such as High Score.
35
3. Crystal structure
The compound was prepared in the form of a white powder, stable in air. The data collection
was performed using an automated diffractometer in Geology Laboratory, Kasdi Merbah
University of Ouargla. For the record, we hold the distinction of being the initial adopters of
this technique for examining (C12H10NO3S)2Ba.
X-ray diffraction (XRD) analysis of the compound (C12H10NO3S)2Ba reveals the presence of 6
characteristic diffraction peaks that correspond to the compound (figure19).
Figure 19 : XRD Pattern of barium diphenylamine -4- sulfonate.
The parameters of reflections, interatomic distances and diffraction angles of

(C12H10NO3S)2Ba are shown in table 3.
Pos. [°2Th.] Height [cts] FWHM Left [°2Th.] d-spacing [Å] Rel. Int. [%]
7,2215 1001,84 0,2952 12,24143 100,00
10,8300 877,31 0,2460 8,16936 87,57
18,2564 180,45 0,4920 4,85954 18,01
20,4468 529,89 0,3936 4,34363 52,89
24,4967 105,41 0,2952 3,63393 10,52
25,4744 455,33 0,3936 3,49664 45,45
Table 3 : The parameters of reflections, interatomic distances and diffraction angles of

(C12H10NO3S)2Ba
36
NB: the Bravais lattice parameters are still unknown for this region thus we couldn’t calculate
the crystallographic plans. Also, the symmetric of BDA4S is unknown.
The average size of barium diphenylamine 4- sulfonate nanopowder was determined from the
0.9 λ
width of the reflection according to the Debye-Scherrer equation D= , where β is the
βCOSθ
full width at half maximum (FWHM) of the peak in radians, θ is the angle of diffraction and λ
is the wavelength of the X-ray, by considering the FWHM (β= 0.45°) of the dominant
diffraction peak (θ=7.22°) of BADA4S nanoparticles, the crystalline size of BDA4S
nanopowder was around 200 nm.
II. Scanning Electronic Microscopy

The SEM method has been used to identify several particles of different molecules. However,
the observation of (C12H10NO3S)2Ba using SEM has never been done before.
In figure (20) showing SEM micrographs of abrasives powders: (C12H10NO3S)2Ba powder

grains with medium diameter of 200 nm.
The result is in a good agreement with that found by Scherrer formula in X-ray diffraction.
Figure 20 : SEM micrographs of C12H10NO3S)2Ba powder grains with diameter of 200 nm
37
Figure (21) below shows the EDS spectrum obtained from the selected area of the grain
(figure 22). There are several dominant elements, namely C, O, S, N, and Ba.
Fig
ure 21: EDX Elemental Analysis spectrum
Figure 22 : A x10 000 close-up of the grain sample
The weight percentages of the different elements normalized to 100% total are shown in
Table 4 below:
38
Table 4 : Elements of (C12H10NO3S)2Ba spectrum
Table 4 shows the composition of the elements in the (C 12H10NO3S)2Ba samples in the
selected section of the grain.
III. UV/vis Spectrophotometry
The spectral properties of barium diphenylamine 4 sulfonate were studied using an analytical
UV-vis absorption spectrophotometer (Analytik Jena) in diluted solutions in distilled water at
different concentrations. All concentrations exhibited similar absorption spectra with a
maximum absorption wavelength (λmax) in the range of 200-330 nm (Figure 23).
Figure 23: UV/vis Spectra of Barium Diphenylamine-4-Sulfonate

39
IV. Fourier Transformed-InfraRed

The use of Fourier-transform infrared spectroscopy (FT-IR) is essential in identifying the
functional groups present in (C12H10NO3S)2Ba synthesis products (figure 24).
Figure 24 : FT-IR Spectrum of Barium Diphenylamine-4-Sulfonate
Figure 24 displays the FT-IR spectra of these various synthesis products within the frequency
range of 2500-500 cm-1.
The characteristic bands of Barium Diphenylamine-4-Sulfonate are 597,742, 1054, 1172,

1233, 1334, 1508, 1602 and 3383 cm-1 which was in good agreement with other previous
studies [39].
V. Electrical conductivity
The self ionisation of water results in H 3O+(aq) and OH-(aq) always being present in any
aqueous electrolyte solution. The measured resistance, or conductance, is therefore a
composite quantity made up from the contribution made by the ions of the electrolyte and the
H3O+(aq) and OH-(aq). The contribution from the H 3O+(aq) and OH-(aq) can be obtained
by measuring the resistance, or conductance, of the H 2O used in preparing the electrolyte
40
solutions under study. The conductivity of the water can then be found from this measured
conductance and the cell constant. For an ionic compound, with the formula AB2, we may
consider the following equilibrium in its saturated solution at a given constant temperature.
2+ −
( aq ) (aq )
AB 2 ( s )⇔ A +2 B
The current is carried through a solution by the movement of the ions of the solution.
It is likely that the more ions there are present, the lower will be the resistance of the solution
to the passage of the current and the greater will be the conductivity, . For the ideal case the
conductivity, , would be expected to be strictly proportional to the concentration of ions
actually present (figure 25)
For homogeneous single-phase insolating liquids, a binary ionic system is often used
to express the specific electrical conductivity  of the solution [40]
 = F(Z ++c+ + Z --c- ) ………………..(1)

where F is the Faraday’s constant,  is the ionic mobility, c the ionic concentration, and the
subscripts ± refer to positive and negative valances. In most practical applications, the source
of ions is the dissociation of the impurities and/or an introduction of ionic doping agents in
the liquid. In both of these cases, the concentration of charged species in insulating liquids is
small enough such that one can ignore ionic interactions. As a result, the electrical effect in
the liquid is expected to induce negligible changes in ionic concentrations or other charging
effects such as formation of micelle structures. The mobility of a charged particle in the
solution depends on its diffusion coefficient D and the temperature T.
±
± D
μ =
RT …………………….(2)
where R is the universal gas constant. Ionic diffusion in polymeric systems can be written
using a Stokes-Einstein relationship in the form:
KB T
D=
αη⟨ R⟩ …………………….(3)
with <R> being the root mean square radius of gyration, the common measure of the size of
41
the charged molecules in the solution, α a constant and kB the Boltzmann constant. α is 6π for
ideal solutions. Combining Equations (1)-(3), the conductivity expression can be reduced to
σ=
(
1 Z + c+ Z− c−
+
6 πη ⟨R+ ⟩ ⟨ R− ⟩ )
Figure 25 : Variation of the electrical conductivity as function of concentration
where η is the solvent viscosity.
Figure 25 shows that σ is almost exactly proportional to the concentration of Barium

Diphenylamine-4-Sulfonate (BDA4S), as expected.
As can be seen, when the concentration of ions in an electrolyte solution (BDA4S) increase,
there are more charged particles available to carry electric current. As a result, the
conductivity  of the electrolyte (BDA4S) increases. This relationship is described by the
Nernst-Einstein equation, which states that the molar conductivity is directly proportional to
the concentration of ions in the solution.
Figure (26) demonstrates the variation of electrical conductivity with temperature. As it can
be seen, an increase in a solution’s temperature will cause a decrease in viscosity and increase
in the mobility of the ions in the solution of BDA4S. An increase in temperature may also
cause an increase in number of ions in the solution due to the dissociation of the molecules.
As a result, there will be increase in conductivity of the solution.
42
It is concluded that parameters such as impurities (dissolved solids BDA4S) and temperature
play an important role for the determination of the electrical conductivity.
Figure 26: Variation of Electrical Conductivity as function of Temperature

VI.
Refractive Index
Refractive index is defined as the ratio of the speed of light in a vacuum to its speed in a
specific medium.
Refractive index is also referred to as refraction index or index of refraction. The speed of
light in a medium depends on the properties of the medium. In electromagnetic waves, the
speed is dependent on the optical density of the medium. Optical density is the tendency of
the atoms in a material to restore the absorbed electromagnetic energy. The more optically
dense material is, the slower the speed of light. One such indicator of the optical density of a
medium is the refractive index.
The refractive index is dimensionless. It is a number that indicates the number of times slower
than a light wave would be in the material than it is in a vacuum. The refractive index,
represented by symbol n, is the velocity of light in vacuum divided by the velocity of light in
a medium. The formula of the refractive index is as follows:
43
n=c/v
Where,
 n is the refractive index
 c is the velocity of light in a vacuum (3 × 108 m/s)
 v is the velocity of light in a substance
The vacuum has a refractive index of 1. The refractive index of other materials can be
calculated from the above equation. Higher the refractive index, the higher the optical density
and slower is the speed of light [41].
Figure (27) shows the relationship between refractive index and concentration of
C12H10NO3S)2Ba solutions.
Figure 27 : The relationship between concentration and refractive index of

(C12H10NO3S)2Ba solutions
From (figure 27) the refractive index is directly proportional to the concentration, as
concentration of guiding liquid increases refractive index increases.
44
Conclusion
&
Perspectives
CONCLUSION
Conclusion
In this study, we investigated the interaction between barium diphenylamine sulfonate

(BDA4S) and water using electrical conductivity and optical properties across different
concentrations and temperatures. By analysing the absorption spectra of BDA4S in the UV-
Vis range, we observed that all solutions exhibited similar absorption spectra, with an
absorption maximum (λmax) ranging from 190 to 340 nm.
To determine the functional groups, present in BDA4S, we employed infrared spectroscopy

(FT-IR) and found characteristic bands in the range of 3383-597 cm-1, which aligned well
with previous studies.
The X-ray diffraction (XRD) analysis of BDA4S revealed significant peaks indicative of
crystallinity.
To examine the sizes and morphologies of the samples, scanning electron microscopy (SEM)
was employed. The results exhibited the presence of microcrystals in the form of micro-
grains, with an average length of 200 nm for BDA4S.
The dominant elements identified through Energy-Dispersive X-ray Spectroscopy (EDS)

analysis of the selected grain area were carbon (C), oxygen (O), sulfur (S), nitrogen (N), and
barium (Ba).
The question of determining whether Barium Diphenylamine-4-Sulfonate is useful in the

composition of the urinary colorimetric sensor array to distinguish Kawasaki disease from
other febrile illnesses: - Developing processing techniques to produce BDA4S as biomaterial,
determining the thermodynamic parameters, activation free energies and its related
thermodynamic parameters will definitely will uncover additional valuable insights
concerning it stability.
Laue Symmetry experiment will consistently reveal more information, whether in regards to
structure, and space group, all while extracting the Bravais lattice parameters and the
crystallographic plans, but the measurement is somewhat of a lengthy and complicated
process compared to other optical characterization techniques, such as Spectrophotometry.
The answer therefore depends on the limitations of the equipment and, most importantly, on
the desired results. As the goal set for this work has been reached, it is noteworthy to
46
CONCLUSION
conclude that the
47
CONCLUSION
absorbance, transmittance, and conductivity of the sample make it a good

candidate for the suggested application.
48
BIBLIOGRAPHY
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49
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Abstract
Barium Diphenylamine-4-Sulfonate physic-chemical and optical properties are the area of investigation
in this work. The given synthesised powder and solutions of our specimen have been analysed using X-
ray Diffraction (XRD), Scanning electronic microscopy (SEM), UV-visible spectrophotometry (UV-vis),
Fourier Transform- InfraRed (FT-IR), Electrical Conductivity and Refractive Index techniques. The
compound has an absorption maximum range from 190 to 340 nm in the UV-vis range to all tested
solutions. Our sample showed characteristic peaks in the range of InfraRed at 597,742, 1054, 1172,
1233, 1334, 1508, 1602 and 3383 cm-1. The X-ray diffraction (XRD) analysis of BDA4S manifested
significant peaks indicative of crystallinity. The Scanning Electronic Microscope revealed micrographs
of microcrystals in our sample of an average length of 200 nm. Energy- Dispersive X-ray Spectroscopy
(EDS) analysis displayed the dominant elements in our specimen which are carbon (C), oxygen (O),
sulfur (S), nitrogen (N), and barium (Ba). Electrical Conductivity and Refractive Index parameters were
further extracted, charted and discussed.
Keywords: Barium Diphenylamine-4Sulfonate (BDA4S), Ultraviolet-Visible Spectrophotometry (UV-

Vis), Fourier Transform Infrared Spectroscopy (FT-IR), X-Ray Diffraction (XRD), Scanning Electron
Microscopy (SEM), Energy-Dispersive X-ray Spectroscopy (EDS), Electrical Conductivity & Refractive
Index.
Résumé
Les propriétés physico-chimiques et optiques du diphénylamine-4-sulfonate de baryum sont le domaine

d'investigation de ce travail. La poudre et les solutions synthétisées données de notre échantillon ont été
analysées par diffraction des rayons X (XRD), microscopie électronique à balayage (SEM),
spectrophotométrie UV-visible (UV-vis), Infrarouge à transformée de fourier (FT-IR), conductivité
électrique et techniques d'indice de réfraction. Le composé a une plage d'absorption maximale de 190 à
340 nm dans la plage UV-vis pour toutes les solutions testées. Notre échantillon a montré des pics
caractéristiques dans la gamme de l'infrarouge à 597,742, 1054, 1172, 1233, 1334, 1508, 1602 et 3383
cm-1. L'analyse par diffraction des rayons X (XRD) de BDA4S a manifesté des pics significatifs
indiquant la cristallinité. Le microscope électronique à balayage a révélé des micrographies de
microcristaux dans notre échantillon d'une longueur moyenne de 200 nm. L'analyse par spectroscopie à
rayons X à dispersion d'énergie (EDS) a montré les éléments dominants de notre échantillon qui sont le
carbone (C), l'oxygène (O), le soufre (S), l'azote (N) et le baryum (Ba). Les paramètres de conductivité
électrique et d'indice de réfraction ont ensuite été extraits, cartographiés et discutés.
Mots-clés : Baryum diphenylamine-4-sulfonate (BDA4S), Spectrophotométrie ultraviolette-visible (UV-

Vis), Spectroscopie infrarouge à transformée de Fourier (FT-IR), Diffraction des rayons X (XRD),
Microscopie électronique à balayage (SEM) Rayons X à dispersion EDS, Conductivité électrique, et
Indice de Réfraction.
‫ملخص‬
‫ تم تحليل عينة من‬.‫ هي مجال بحث هذه المذكرة‬Diphenylamine-4-Sulfonate Barium ‫تعتبر الخصائص الفيزيائية والكيميائية والبصرية‬
‫ مطيافية األشعة فوق البنفسجية و‬،)SEM( ‫ الفحص المجهري اإللكتروني الماسح‬،)XRD( ‫المسحوق ال ُمحضر باستخدام انعراج األشعة السينية‬
‫ يحتوي المركب على أقصى مدى لالمتصاص من‬.‫ الناقلية الكهربائية وقياس قرينة االنكسار‬،)FT-IR( ‫ األشعة تحت الحمراء‬،)UV-vis( ‫المرئية‬
‫ و‬1508 1602‫ و‬3383 ‫ عند‬InfraRed ‫ أظهرت عينتنا قمم مميزة في نطاق‬.‫ لجميع المحاليل المختبرة‬UV-vis ‫ نانومتر في نطاق‬340 ‫ إلى‬190
‫ كما‬.‫ قم ًماـ كبيرة تشير إلى التبلور‬BDA4S ‫) لـ‬XRD( ‫ أظهر تحليل حيود األشعة السينية‬.1- ‫ سم‬597‫ و‬743‫ و‬1054‫ و‬1172‫ و‬1233‫ و‬1334
‫ عرض التحليل الطيفي لألشعة‬.‫ نانومتر‬200 ‫كشف المجهر اإللكتروني الماسح عن صور مجهرية من البلورات الدقيقة في عينتنا بمتوسط طول‬
.)Ba( ‫) والباريوم‬N( ‫) والنيتروجين‬S( ‫) والكبريت‬O( ‫) واألكسجين‬C( ‫) العناصر السائدة في عينتنا وهي الكربون‬EDS( ‫السينية المشتتة للطاقة‬
.‫كما تمت دراسة الناقلية الكهربائية و قرينة االنكسار لمختلف المحاليل‬
‫ الناقلية الكهربائية وقياس‬،‫ المجهر اإللكتروني الماسح‬،‫ انعراج األشعة السينية‬،‫ األشعة تحت الحمراء‬،‫ مطيافية األشعة فوق البنفسجية و المرئية‬b:‫الكلمات المفتاحية‬
‫قرينة االنكسار‬

Study of Barium Diphenylamine 4-Sulfonate

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Democratic and Popular Republic of Algeria

Ministry of Higher Education and Scientific Research

Serie N°: ....../FM/DP/2023

Study of Barium Diphenylamine-4Sulfonate

Defended publicly in ……, 2023

Thesis Supervisor: Pr. AYACHE Rachid Professor in Applied Physics

- HARKAT Hassina Professor in Organic Chemistry Chair

- MANSOURI Sakina Assistant Professor Class A in Physics Examiner

University Year : 2022-2023

Mémoire de fin d’études

Étude de Barium Diphenylamine-4-Sulfonate

-AYACHE Rachid Professeur en Physique Appliquée Rapporteur

- MANSOURI Sakina Maitre Assistante (A) en Physique Examinatrice

Année universitaire : 2022-2023

LE VICE DOYEN A LA GRADUATION Pr. LAHMAR Mourad

LE VICE DOYEN A LA POST GRADUATION Pr. DERDOUS Chawki

LE PRÉSIDENT DU CONSEIL SCIENTIFIQUE Pr. HARKAT Hassina

LISTE DES RESPONSABLES DU DEPARTEMENT DE PHARMACIE.

ADJOINTE DU CHEF DU DÉPARTEMENT Dr. MAKHLOUF Youcef

ADJOINT DU CHEF DU DÉPARTEMENT Dr. ZAITER Thamer

PRÉSIDENT DU COMITÉ SCIENTIFIQUE Pr. BEN MOUSSA Mohammed Tahar

N° Nom &Prénom Spécialité Module(s)

JE JURE, EN PRÉSENCE DES MAITRES DE LA FACULTÉ, DES CONSEILLER DE

D'EXERCER, DANS L'INTÉRÊT DE LA SANTÉ PUBLIQUE, MA PROFESSION

DE NE JAMAIS OUBLIER MA RESPONSABILITÉ ET MES DEVOIRS ENVERS LE

EN AUCUN CAS, JE NE CONSENTIRAI A UTILISER MES CONNAISSANCES ET MON

QUE LES HOMMES M'ACCORDENT LEUR ESTIME SI JE SUIS FIDÈLE A MES

To my two beloved sisters and brother, my lifelong friends.

To my sleepless nights and endless cups of coffee.

To Bechbouch, my feline pal who accompanied me in my solitude. You were my only

AAP: American Academy of Paediatrics NSAIDs: Non-steroidal anti-inflammatory

BSEs: Backscattered electrons UV-vis : Ultraviolet visible

CBS: Concentric Backscattered XRD : X-ray diffraction

CL: Cathodoluminescence XRPD: X-ray powder diffraction

EDS: Energy Dispersive X-

EMR: Electromagnetic radiation

FT-IR: Fourier Transform Infrared

GGT: Gamma-glutamyl transferase

HOMO: Highest occupied molecular

KD: Kawasaki disease

LCCNS: Laboratory for Growth and

LDH: Lactate dehydrogenase

LFD: Large Field Detector

LUMO: Least unoccupied molecular

Barium Diphenylamine-4-sulfonate (BDA4S) is a versatile compound that has been

The objective of this study is to conduct a comprehensive physic-chemical quality control

A reliable method to accurately diagnose Kawasaki disease (KD) in children is by considering

Figure 1 : Predictor sensing compound structure [4].

1. Chemical structure of Barium Diphenylamine 4-Sulfonate

Figure 2 : Structure of Barium Diphenylamine 4-Sulfonate

2. Previous studies on Barium Diphenylamine 4-Sulfonate

Furthermore, this compound plays a crucial role as an indicator in the determination of

In the field of pharmaceutical research and analysis, barium diphenylamine-4-sulfonate serves

3. Spectroscopic techniques used in the characterization of

3.1.2 Crystal structure

Figure 3 : Two-dimensional lattice with translation vector (b)

3.1.3 X-ray diffraction principle

3.1.4 Applications of PXRD in Pharmaceutical Sciences

3.2 UV Visible spectrophotometry

3.2.2 Principles of UV-visible spectrophotometry

Figure 6 : Schematic diagram of the Lambert-Beer law.

The mathematical representation of the Lambert-Beer law can be expressed as follows: