Production and Characterization Of Ink from Fluid of Warka And Kulkual 2012E.

BAHIR DAR UNIVERSITY

BAHIR DAR INSTITUTE OF TECHNOLOGY
FACULTY OF CHEMICAL AND FOOD ENGINEERING
DEPARTMENT OF CHEMICAL ENGINEERING
Project Topic: Ink Production and Characterization from Ficus Vasta
(Warka) and Euphorbia Abyssinica (kulkual)

Members Name ID

Minale Derseh 0801100

Mulat Degarege 0801122

Surafel Aregahegn 0801275

Advisor: Mr.Mequanint.D
Submission date:16/07/2012E.C

BiT, BDU, Bahir Dar, Ethiopia

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DECLARATION

We declared that this project is entitled to the Production of ink from the fluid of Ficus
Vasta and Euphorbia Abyssinica. The formulation of ink from Ficus Vasta and Euphorbia
Abyssinica has never been published within a degree, diploma, master's, Ph.D., and other
programs. We assure you that the project was done within a group with the help of
Mr.Mequanint (advisor). Generally, the project focused on not only collecting, preparing,
characterizing, and mixing ingredients, but also characterizing the formulated ink too.
Authors have fulfilled the rules, regulations, requirements, procedures, and policies of the
university related to project work.
Name of Authors ID Signature Date

Minale Derseh 0801100 16/07/2012 E.C

Mulat Degarege 08011122 16/07/2012 E.C

Surafel Aregahegn 0801275 16/07/2012 E.C

Advisor approval
This is to certify that the above statement made by the candidates is correct to the best of
my knowledge and belief. This project work has been submitted for presentation with my
approval.

Name of Advisor signature Date

Mr. Mequninet.D 14/07/2012 E.C

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ACKNOWLEDGMENT

First of all, our sincere appreciation goes to God Almighty; help us in every aspect of our
life. We would like to offer our deepest gratitude to our Advisor Mr. Mequanint, the
driving force behind this research, for his constant support, unreserved advice, and
diligent follow-up of our progress, encouragement, patience, and knowledge in guiding
and assisting throughout the research process and editing the project. We are also heartily
thankful to lab assistances for their permission to use the laboratories and for their help
with nearby supervision who all have been of help to us in achieving the project goal.
Special thanks are extended to our faculty of chemical and food engineering and also
Bahir Dar society for giving the raw material directly or showing the direction where it is
found. We will not fail to recognize the endless effort of our honorable BiT for financial,
technical, and other utility support.

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ABSTRACT

Writing ink is a liquid or a paste mainly composed of dyes, pigments, binders, solvents,
and additives. Inks are manufactured from a wide variety of substances that exhibit very
different chemical behaviors. Ethiopia has a variety of plant spices for ink production
ingredients. However, most ink ingredients have been imported and thus, it is necessary
to use locally available raw materials for ink production. This project was aimed at the
production and characterization of ink from the milky fluid of Ficus Vasta and Euphorbia
Abyssinica. The raw materials were collected and prepared. In the experiment, the effect
of solvent (methanol) concentration (50, 75, and 100 %) and mixing ratio (R1, R2, and
R3)of Euphorbia Abyssinica and Ficus Vasta was investigated, and among those
experimental results, the preferable result was found at R3 (102.8:51.4) and solvent
concentration of at 100% methanol. Finally, the formulated ink was characterized
through pH, viscosity, and drying time and found to be 5.53, 0.001 Ns/m2, and 2.16secs
respectively. This showed that Euphorbia Abyssinica and Ficus Vasta has the potential to
produce ink.
Key Words: Milky fluid of Ficus Vasta and Euphorbia Abyssinica, Ink, Binders,
Solvents, Additives

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TABLES OF CONTENTS

DECLARATION ................................................................................................................ 2
ACKNOWLEDGMENT..................................................................................................... 3
ABSTRACT ........................................................................................................................ 4
LIST OF TABLES .............................................................................................................. 7
LIST OF FIGURES ............................................................................................................ 8
CHAPTER ONE ............................................................................................................... 10
INTRODUCTION ............................................................................................................ 10
1.1 Background of the Study .................................................................................... 10
1.2 Statement of the Problem ........................................................................................ 12
1.3 Objectives ................................................................................................................ 12
1.3.1 General objectives ............................................................................................ 12
1.3.2 Specific objectives ............................................................................................ 12
1.4 Scope of the Study................................................................................................... 13
1.5 Significance of the Project ...................................................................................... 13
CHAPTER TWO .............................................................................................................. 14
LITERATURE REVIEW .............................................................................................. 14
CHAPTER THREE ....................................................................................................... 18
MATERIALS AND METHODS ...................................................................................... 18
3.1Materials ................................................................................................................... 18
3.1.1 Equipment and Instrument................................................................................ 18
3.2 Chemicals and Reagents.......................................................................................... 18
3.2.1 Chemicals ......................................................................................................... 18
3.2.2 Reagent ............................................................................................................. 19
3.3 Experimental Design ............................................................................................... 19
3.4 Experimental Setup and Description ....................................................................... 19
3.5 Methods ................................................................................................................... 20

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3.5.1 Raw Material Collection ................................................................................... 20

3.5.2Raw Material Preparation .................................................................................. 20
3.5.3 Testing for Phenol Compounds ........................................................................ 20
3.5.4 Ink Formulation Procedure ............................................................................... 21
3.5.5Product Characterization ................................................................................... 21
3.5.6 Statistical Data Analysis ................................................................................... 22
CHAPTER FOUR ............................................................................................................. 23
RESULTS AND DISCUSSION ....................................................................................... 23
4.1 Phenolic Test ........................................................................................................... 23
4.2 Drying time ............................................................................................................. 23
4.3 pH value of the ink .................................................................................................. 25
4.4 Viscosity .................................................................................................................. 26
CHAPTER FIVE .............................................................................................................. 29
CONCLUSION AND RECOMMENDATION ................................................................ 29
5.1 Conclusion............................................................................................................... 29
5.2 Recommendation ..................................................................................................... 29
REFFERENCE ................................................................................................................. 31
APPENDICES .................................................................................................................. 33

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LIST OF TABLES

Table 2.1Physical Properties of Standard Ink [4] ............................................................. 17

Table 3.1 Factors and expected experimental results ....................................................... 19

Table 3.2 The formulation of different ratios [10, 12] ...................................................... 21

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LIST OF FIGURES

Figure 3. 1 Experimental set up ........................................................................................ 19

Figure 4. 2 Effect of variation of mixing ratio and methanol concentration on drying time
........................................................................................................................................... 23
Figure 4. 3 Effect of variation of methanol concentration and mixing ratio on drying time
........................................................................................................................................... 24
Figure 4. 4 Effect of variation of mixing ratio and solvent concentration on pH value ... 25
Figure 4. 5 Effect of variation of methanol concentration on viscosity............................ 26

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ACRONYMS
BC Before Christ
Cps Centipoises
Kg Kilogram
o
C degree centigrade
ETB Ethiopian Birr

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CHAPTER ONE

INTRODUCTION

1.1 Background of the Study

The development of the art of writing was growing stepwise with the reformation of
civilization. It is a skill by which a person expresses his thoughts, ideas, feelings, and
emotions. Writing ability makes the human being a pioneer of the ecological system and
sets him apart from this world among the animal kingdom [3].

Writing inks were first manufactured in both ancient Egypt and China in about 2500BC.
These inks were composed of soot bound together with gums. Printing was invented by
the Chinese about 3000 years later. They used a mixture of colored earth, soot, and plant
matter for pigments, again mixed with gums for a binder. By 1440, when Johannes
Guttenberg invented the first printing press with moveable type, the ink was made of soot
bound with either linseed oil or varnish - similar materials to those used for black inks
today. Colored inks were introduced in 1772 and drying agents were first used in the
nineteenth century. Today's printing inks are composed of a pigment (one of which is
carbon black, which is not much different from the soot used in 2500BC), a binder (an
oil, resin, or varnish of some kind), a solvent, and various additives such as drying and
chelating agents[1, 2].

Writing comprises writing tools to make documentation using well-distinguished

language. Chemists, physicists, technologists provided writing tools like colorful inks,
pens, brushes, etc. to write on a substrate like paper, cloth, rock, wooden blocks, plastic
or metal sheet, etc. With the progress of technology, scientists invented superior tools in
modern society. Writing is an advanced mode to make the image comes true that one
would raise preserved, secured, and stable documentation. To achieve this target
magnetic, electric, electronic inks are arising which will provide certainly a step towards
conservative society [5].

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Inks are manufactured from a wide variety of substances that exhibit very different
chemical behaviors. Inks designed for use in different writing instruments or printing
methods have quite dissimilar components. Since the 1950s chromatographic and
electrophoresis methods have played important roles in the analysis of inks, where
compositional information may have bearing on the investigation of counterfeiting, fraud,
forgery, and other crimes [6].

Ink performance can be characterized based on the following parameters: depth of color,
durability, and indelibility.
Depth of Color: Thus the ink must flow from the pen, so that the finest lines and
characters may be formed. It must not be thick or form a hand crust when it dries up on
the rib. This occurs sometimes with perfectively good ink and is hen merely a sign that
the ink has become too concentrated by evaporation and requires dilution with water, if,
however, the addition of water does not put the matter right. It proves either that the
original composition of the ink was wrong or that the ink has decomposed[4].
Indelibility: For certain purposes such as for documents that will possess a historical
interest, the ink must be able to withstand merely the ravages of time and also deliberate
attempts to efface it by chemical means. Certain inks, especially those which contain
dyes as pigments are capable of withstanding ravages of time extremely well [4].
Durability: A good ink should keep its color unchanged for a long time and should not
show any material alteration if the paper becomes damp or wet. A good ink must not go
moldy even after greater dilution. This last condition is easily fulfilled as many inks are
themselves toxic to molds on in any ease antiseptics can always be added to them [4].
The pigments are finely distributed in the ink and are maintained in the suspended state
using a dispersing agent [17].

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1.2 Statement of the Problem

Ethiopia imports most ink ingredients from abroad countries instead of preparing it from
domestic plants spices. There are locally available materials in Ethiopia having a capacity
of producing ink like milky of Euphorbia Abyssinica and Ficus Vasta which are found
abundantly and used as a source of resin for ink production. Both these raw materials
have a milky fluid which has a binding nature. Indeed, the formulations of ink from these
raw materials have not been studied yet. Thereby the motivation of this project was
mainly focused on the investigation of Ficus Vasta and Euphorbia Abyssinica fluid for
ink formulation.

1.3 Objectives

1.3.1 General objectives

The main objective of this project is the production and characterization of ink from the
fluid of Euphorbia Abyssinica and Ficus vasta.
1.3.2 Specific objectives
 To test the phenolic content of milky fluid of Euphorbia Abyssinica and Ficus
Vasta
 To investigate the effects of solvent concentration and mixing ratio of Euphorbia
Abyssinica and Ficus Vasta on ink formulation
 To characterize the product

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1.4 Scope of the Study

This project work ranges from the phenolic test of fluid of Ficus Vasta and Euphorbia
Abyssinica, investigating the effect of solvent concentration and mixing ratio of
Euphorbia Abyssinica, and Ficus Vasta on ink formulation and characterization of
produced ink.

1.5 Significance of the Project

The fluids of Ficus Vasta and Euphorbia Abyssinica are considered the best candidate for
the substitution of synthetic resins to produce ink because of their good binding nature
and ease available in Ethiopia. Using this fluid as a raw material for ink production has
many economic benefits including the reduction of imported raw material cost and unit
price of ink. Generally, it is an attractive alternative to produce ink due to its abundance,
renewable resources, etc.

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CHAPTER TWO

LITERATURE REVIEW

The improvement of technology produced advanced writing instruments which have been
grown progressively. The techniques modernized step by step through quill, fountain,
ball, felt to gel pen and also in use as writing device nowadays. The successive variation
of this technology pens also brought changes in ink composition and again to ink
chemistry. Based on a colorant (dye or pigment) used, inks are classified as a dye and
pigmented inks. Similarly, vehicle (water or solvent) used to manufacture inks also
categorized the inks as aqua based and solvent-based inks. Some additional chemical
reagents are used in pigmented inks which make sure strong adhesion of coarse
molecules of pigment to the substrate and also then ensure prevent from being withdrawn
by mechanical abrasion. These components are typical resin in solvent-based inks or
binding agents in aqua-based inks [5].

According to Sureh and Shah, 1987, writing inks are usually in fluid forms consisting of
suspension prepared from dyes, pigments, binders, solvents, additives, paints, alcohol,
and water. The characteristic of a particular ink being used in writing determine how long
and clear the writing can stay over a while. [4].

Synthetic inks have colorants (titanium dioxide, calcium carbonate, lithol, etc.), resins
(ethylcellulose, acrylic resins, polyvinyl acetate, etc.), solvents (toluene, mineral oil,
acetone, methanol, etc.), additives (phenol, titanium chelates, silicones, cobalt &
manganese compound) while in this study natural agents were used such as colorant
(betanin and vulgaxanthin from beetroot, curcumin from turmeric, tannic acid from amla
powder), resin (gum acacia), solvent (water) and additives (vinegar, salt) [21].

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The ink composition for oil-based ballpoint pens according to the present invention
exhibits a light and soft writing sensation due to low viscosity of 300 to 3,000 cps is free
of variation in ink flow depending on variation (increase or decrease) in surrounding
temperatures and thus exhibits superior stability [15].

Pigments have been used predominantly for coloring. Pigments can be organic or
inorganic. They are insoluble because they consist of molecules larger than that of dye.
Inorganic pigments such as titanium oxide, carbon black, ultramarine blue, cobalt blue,
chromium oxide, iron oxide red, and graphite are used. The most common pigment used
is carbon black because it gives opacity, color permanence, and vibrancy [18].

An organic solvent-based ink that employs a pigment as a colorant is also known to the
art. Since the pigment inherently is not compatible with the organic solvent or a binder
resin, the pigment must be ground with the binder resin or the solvent and dispersed in
the ink. The pigmented ink, however, does not have stability with time and often forms
agglomerates and precipitates. An amount of the dye is not limited and varied by a useful
application of the obtained ink, but generally within the range of 8 to 20% by weight
(preferably 10 to 15% by weight) for ballpoint pens, 3 to 15% by weight (preferably 5 to
10% by weight) for making pens. The ink composition generally contains the dye and an
organic solvent, especially an alcohol or glycol. It may further contain a binder resin that
is dissolved in or compatible with the organic solvent. Typical examples of organic
solvents are monohydric alcohols (e.g. methanol, ethanol, propanol, and benzyl alcohol),
polyhydric alcohols [7].

A dye is a colored, ionizing, and aromatic substance that has an affinity to the substrate to
which it is applied. Dyes are colored because they absorb some wavelengths of light
more than others due to the presence of chromophore [20].
The ink produced does not easily erase, because berry has a little property of permanent
ink [4].

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The berry seeds can be used to develop ink which is a useful material in painting,
drawing, and writing as well as waste management (Druid, 2002). Due to the abundance
of berry trees and lack of the management of its seeds in the environment, this makes it
inexpensive and also considered solid waste in the environment [19].

The previous study had investigated that, phenolic compound is found to be one of the
consistent fluid of Warka and kulkual which is the main components of resin. They used
about 5ml of methanol, an equal volume of water, and 3 grams of the ferric chloride were
mixed and found violet color indicates the presence of phenolic compounds. The effects
of different concentrations of methanol extracts and different extraction times on total
phenolic content for O.stamineus leaf was showed that the highest total phenolic content
was 50% methanol concentration extract and follows by 100% methanol concentration.
However, the lowest value of total phenolic content was 0% methanol concentration
extract [14].

Nwafulugo F.U, 2 Samuel F, et al. (2019) had investigated that, the physical properties of
the sample ink were tested against the standard ink and the results shows that the
produced ink is of high quality, having a pH of 9.3, drying time of 2.3 seconds, and
Viscosity of 9.5× 10-4 Ns/m2 by using gum Arabic as a resin or binder [4].

Kawaguchi et al. (1987) formulated a marker ink and they have got the viscosity of 50
cps ( standard 10 to 50 cps), at room temperature by using ketone resin from 3 to 20% by
weight, preferably from 5 to 15% by weight of the ink composition, organic solvent
having a boiling point ranging between 100 and 180° C and titanium dioxide as a
colorant within the range of from 0.5 to 30% by weight, preferably from 2 to 25% by
weight of the ink composition [6].
The pH of standard ink is 5.5 making it slightly acidic. This is due to the presence of SO3,
an acidic gas that is a precursor of H2SO4. The ink is not highly acidic due to the presence
of other basic substances shown in the XRF analysis such as chlorine and magnesium
oxide. The presence of SO3 and chlorine are responsible for the pH values of the ink [18].

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Table 2.1Physical Properties of Standard Ink [4]

Drying (sec) pH Viscosity (Ns/m2)
1-3 5.5 0.00095-0.00147

Ethiopia imports most ink ingredients from abroad countries. But, there are locally
available materials having the capability of producing ink like milky of Kulkual and
Warka which are found abundantly. Thereby the study of this project was mainly focused
on the investigation of Ficus Vasta and Euphorbia Abyssinica fluid for ink formulation.

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CHAPTER THREE

MATERIALS AND METHODS

3.1Materials

3.1.1 Equipment and Instrument

3.1.1.1 Equipment’s

Types of equipment used were beaker to collect the fluid of Ficus Vasta and Euphorbia
Abyssinica sample handling, plastic to collect blackberry, knife to cut the plant to
generate the fluid, stainless steel pot to handle blackberry for heating, bowl to handle the
strained blackberry, mash for filtering the strained blackberry, mixer to mix the
ingredient, stove for heating purpose, measuring cylinder to measure the volume of
solvent and spoon to take the additives.

3.1.1.2 Instruments

Instruments used for doing this project were, a stopwatch to measure time, a
viscometer(Visco star plus) to measure viscosity, and a pH meter (pH-016) to measure
the pH value and balance to measure raw materials.

3.2 Chemicals and Reagents

3.2.1 Chemicals

Chemicals were vinegar used as a preservative, methanol (CH3OH, 99.95%) as a solvent,

milky fluid of Warka and kulkual to bind the ingredients together and with the surface of
the paper, soot as carbon black and blackberry for coloring.

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3.2.2 Reagent

Ferric chloride (FeCl2) was used as a reagent to check the presence of the phenolic
compound in the fluid.

3.3 Experimental Design

Two factors, mixing ratio, and solvent concentration were used in the experiment with
three levels and a replication constant of k=2. Total run= *k= 2=18. The
numbers of experimental run that needed to be performed in this study were eighteen.

Table 3.1Factors and expected experimental results

Mixing ratios [authors]
Solvent concentration (% v/v) [12] R1(1:2) R2(1:1) R3(2:1)
50
75
100

3.4 Experimental Setup and Description

Figure 3. 1 Experimental setup

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First, the varnish was prepared from the mixture of solvent, fluid of Warka and kulkual
(resin), blackberry, and additive. Following this, pigment (soot as carbon black) was
added to varnish and well mixed in the mixer to produce the desired ink.

3.5 Methods

3.5.1 Raw Material Collection

First, the fluid of Ficus Vasta and Kulkual was generated by peeling the bark of steam
using a knife and collected in the glass beaker. Ripe blackberry fruit and vinegar were
bought from the supermarket and soot used as carbon black had been collected from the
kitchen house.

3.5.2Raw Material Preparation

Before using the fluid of Kulkual and Warka unwanted materials were separated
manually. 448.8 gram of ripe and fresh blackberry was collected and put into a stainless
steel pot and subjected to 30 oC. In the process of heating, the berry was continuously
mashed and stirred using a masher. The pot of the berry was removed from the heater and
allowed to cool at atmospheric temperature by exposing it to the air. After cooling, the
liquid was strained by using a mash into a clean bowl repeatedly until the liquid became
too clean and free from any unwanted particles.

3.5.3 Phenolic compound test

The previous study had investigated that, phenolic compound is found to be one of the
consistent fluid of Ficus Vasta and kulkual which is the main components of resin. To
test it, about 5ml of methanol and an equal volume of water were added and 3 grams of
the ferric chloride was also added as a reagent. The appearance of violet color indicated
the presence of phenolic compounds [14].

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3.5.4 Ink Formulation Procedure

Water-based gravure ink formulation contains pigment 6-17%, binding agents 10-30%,
and solvent 1-12%, and water 45-66% [11].

Table 3.2 The formulation of different ratios

Ingredients Ratio 1 Ratio 2 Ratio3 Standard References

(1:1) (1:2) (2:1) values
Warka (g) 77.1 51.4 102.8
Kulkual (g) 77.1 102.8 51.4
Black carbon (g) 210 210 210 [10]
Vinegar (ml) 10 10 10 5-10
Black berry (g) 250 250 250
Methanol (ml) 18 18 18 [12]

The liquid obtained from the straining process was mixed with 154.2gm of milky fluid,
10 ml vinegar, and 18 ml of methanol in a mixer bowl to produce a homogenous mixture.
After that, 210gm of soot as carbon black was added to the varnish as a colorant and
stirred for 10 minutes continuously to achieve perfect homogeneity. Finally, the viscosity,
drying time, and pH of the ink produced were characterized and tested.

3.5.5 Product Characterization

3.5.5.1Viscosity

The ink should flow easily and not clog the marker or pen tip. By using the Visco star
plus-viscometer it was measured directly.

3.5.5.2 Drying time

After the ink is applied on the writing surface, the solvent should vaporize and leaving
the colorant and the binder so that the ink is bind to the surface. The ink was used to write

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on white paper at room temperature and the drying time was measured and recorded
using a stopwatch.

3.5.5.3 pH value

A pH meter is a scientific instrument that measures the hydrogen-ion activity in water-

based solutions, indicating its acidity or alkalinity expressed as pH. A typical pH meter
has two basic components: the meter itself which can be a moving coil meter or a digital
meter one which a numeric display. When the probe was inserted into the ink, the pH
was displayed.

3.5.6 Statistical Data Analysis

The experimental results were analyzed with one sample test in IBM SPSS statistics 20
and Microsoft excel.

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CHAPTER FOUR

RESULTS AND DISCUSSION

4.1 Phenolic Test

The violent color was obtained from the phenolic test of fluid of Warka and kulkual. This
result showed that the existence of phenolic compounds in the fluid of Ficus Vasta and
kulkual which indicates the presence of resin in the fluid. The previous study had
investigated that, the phenolic compound was tested by using ferric chloride reagent and
they found violet color which indicates the presence of phenolic compounds [14].
Therefore, a similar experimental result was found. The result obtained is reasonably fit
with the standard set of pH colors shown in the appendix C5 (violent color).

4.2 Drying time

3.4

3.2

3
Drying time (sec)

2.8
50%
2.6
75%
2.4 100%

2.2

2
0.25 0.75 1.25 1.75 2.25
Mixing ratio

Figure 4. 1 Effect of variation of mixing ratio and methanol concentration on drying time

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3.4

3.2

Drying time (sec) 3

2.8
R1
2.6
R2
2.4 R3

2.2

2
40 50 60 70 80 90 100 110
Methanol concentration (%)

Figure 4. 2 Effect of variation of methanol concentration

and mixing ratio on drying time

Prefer drying time is necessary for neither easy erasable nor high depth of color so that
the ink components will being absorbed beyond stick to the surface. After the ink is
applied on the writing surface, the solvent should vapourize within the standard drying
time and then leaving the colorant and the resin, so that the ink is bind to the surface. The
drying time of the ink is a function of the viscosity [18]. The viscosity of the ink affects
the drying time, therefore, the more viscous the ink, the longer the drying time [4]. From the
above graph, The drying time is decreasing with increasing methanol concentration. As
the solvent concentration increase, the volume of water in the solution decrease and the
tendency of methanol to evaporate is higher than that of water at normal condition. The
drying time also decreases with increasing in Ficus Vasta to kulkual mixing ratio.
Because Ficus Vasta is high soluble than E. abyssica this makes the ink to be less
viscous. Since viscosity decrease with an increase in solubility. Low viscosity results in a
short drying time. The graph clearly shows that the solvent concentration of 100% and
the mixing ratio of R3 have the shortest drying time within the standard ranges. From the
total experimental results, and found to be 2.16 secs. This result is in the range of
standard value (1-3 second) [4]. Previous studies like Nwafulugo F.U, 2 Samuel F, et al.

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(2019) had investigated, the drying time of the sample ink and found it to be a time of 2.3
seconds by using Arabic gum as a resin [4]. Thus, almost the same experimental result is
obtained.
Therefore, the variations of mixing ratio and methanol concentration have a significant
effect on the drying time of the ink at (p < 0.05) [appendix 9A].

4.3 pH value of the ink

6.1
5.9
5.7
5.5
pH value

5.3 50%
5.1 75%
4.9 100%
4.7
4.5
0.25 0.75 1.25 1.75 2.25
Mixing atio

Figure 4. 3 Effect of variation of mixing ratio and solvent concentration on pH value

The above graph was selected for discussion. The other experimental results for the
effects of solvent concentration and mixing ratio on pH are not selected to discuses due to
its strictly increasing behavior as solvent concentration increases so it was shown in
tabular form [appendix 6A].
From the selected graph, the value of pH is small at a low solvent concentration (50%)
and high at a higher solvent concentration (100%) due to the pH value of methanol
ranges from 7-8.3 which results in the pH value of formulated ink increase, as the
concentration of methanol increases in the solution.

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The standard pH value of the writing ink is 5.5 [4]. So from the above graph, it is
investigated that the graph at R3 and solvent concentration of 75% are reasonably fitted to
the standard value.
From the total experimental results, pH = 5.3 was nearest to the standard value as shown
in the above graph. This is the best result because; it approaches the standard value
(pH=5.5). previous studies likeNwafulugo F.U, 2 Samuel F, et al. (2019) had investigated
that, the physical properties of the sample ink were tested against the standard ink and the
results shows that the produced ink is of high quality, having a pH of 9.3 using gum
Arabic as a resin or binder [4].
Therefore, the variations of mixing ratio and methanol concentration have a significant
effect on the pH value of the formulated ink (p <0.05) [appendix 10A].

4.4 Viscosity

0.002
0.0019
0.0018
Viscosity (Ns/m2)

0.0017
0.0016
0.0015 R1
0.0014 R2
0.0013 R3
0.0012
0.0011
0.001
40 50 60 70 80 90 100 110
Methanol concentration (%)

Figure 4. 4 Effect of variation of methanol concentration on viscosity

Were, R1, R2, and R3 are Warka to kulkual mass ratios with the value of 0.5, 1, and 2
respectively.

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The above graph was selected to discuss. The other experimental results for the effects of
mixing ratio and methanol concentration on viscosity are not selected here to discuss due
to its strictly increasing behavior as mixing ratio increases. So, it is better to show it in
tabular form [appendix 5A].
From the above graph it is clearly shown that as the concentration of methanol increases,
the viscosity of the ink is decreasing. This is because of the following three main reasons;
The viscosity of methanol (0.000545Pa.s) is less than the viscosity of water
(0.001Pa.s) at room temperature [16]. This implies that, as the amount of
methanol volume increases in the solution, the viscosity of formulated ink
becomes to decreases.
The addition of methanol towards water results in an exothermic reaction which
increases the amount of temperature release and makes the molecules found in
the ink becomes far apart and finally result in low viscosity.
The solubility increases while methanol concentration increases and thus the
viscosity decrease. Because the viscosity decreases as solubility increases.
The standard viscosity value of the writing ink is from 0.00095-0.00147 (Ns/m2) [4]. So,
from the above graph, it is investigated that the graph at R1 and solvent concentration of
100% are reasonably fitted to the standard value. From the total experimental results,
0.001 Ns/m2 was selected and it is in the range of standard value. The writing friction was
greatly reduced when inks of lower viscosity were used. Low viscosity ink has good
writing experience. The ink should flow easily and not clog the pen tip.
Previous studies like NwafulugoF.U, 2 Samuel F, et al.(2019) had investigated that, the
physical properties of the sample ink were tested against the standard ink and the results
shows that the produced ink is of high quality, having a Viscosity of 9.5× 10-4 Ns/m2 by
using gum Arabic as a resin or binder [4]. Similarly, another previous study was
investigated that, the ink composition for oil-based ballpoint pens according to the
present invention exhibits a light and soft writing sensation due to low viscosity of 300 to
3,000 cps [15]. So, from this project, the lowest viscosity is selected to get a good writing
performance.

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The variations of mixing ratio and methanol concentration seem to have a significant
effect on the viscosity of the formulated ink at (p <0.05) [appendix 10A]. Warka is more
soluble than kulkual with methanol solvent during the experiment and makes the
viscosity to be decreased. However, as the mixing ratio was increasing, the viscosity was
increasing instead of decreasing. This is due to different factors such as instrumental
error, personal error, etc.

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CHAPTER FIVE

CONCLUSION AND RECOMMENDATION

5.1 Conclusion

From this project the following points have been concluded;

The fluid of Ficus Vasta and kulkual is investigated to be resin containing an organic
compound and one of the principal components of ink formulation. The characteristics of
the formulated ink are examined and gives a positive response. The characteristic values
are reasonably closed to the standards and comparable with the previous studies. The best
results of drying time, pH, and viscosity are obtaining at the mixing ratio and solvent
concentration of (R3, 100%), (R3, 75%), and (R1, 100%), respectively. All in one, the
formulated ink is characterized through the best points of mixing ratio of Ficus Vasta and
kulkual at R3 (102.8:51.4 wt by wt) and solvent concentration of 100%. Generally, the
preferable experimental results are investigating with the drying time of 2.16 sec, pH
value of 5.53, and viscosity of 0.001Ns/m2.

5.2 Recommendation

The phenolic content test, drying time, pH value, and viscosity were examined under this
project. And, measurable results were recorded when compared to the standards and
previous researchers' results. The remaining parameters that need to be done further are
recommended below.

 Other properties of raw materials like viscosity, pH, specific gravity and the
quantity of Ficus Vasta and kulkual fluids.
 Other properties of formulated ink like flowability, penetration time
The interested researcher can better use the surfactant for improving the surface
properties of the ink and undergo X-ray fluorescence analysis to know the impact of ink
on the environment. The fluid of kulkual is less soluble with methanol, so the aspiring

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researcher can find another solvent that soluble well to minimize the effects of viscosity
on drying time.

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REFERENCES

[1] Kirk-Othmer, Encyclopedia of Chemical Technology (3rd Edition), V.13 (374-397) &
V. 19 (110-175), Wiley & Sons, New York, 1981.
[2] Color Index (3rd Edition), American Association of Textile Chemists and Colorists,
London, 971.
[3]Sakayanagi M., Komuro J., Konda Y., Watanabe K., Harigaya Y., (1999) Analysis of
ballpoint pen inks by field desorption mass spectrometry, J. for. Sci., 44(6) 1204-1214.
[4]Nwafulugo F.U,2 Samuel F, 3NyamTobias,4S.OOmale, 5Nwosibe P . O (2019),”
Marker Ink Production from Berry Seed Extract”, International Journal of Scientific &
Engineering Research Volume 10, Issue 5, May-2019 698 ISSN 2229-5518
[5]Agarwal, A., et al. "Techniques for the Characterization of Inks."
[6] Keizo Kawaguchi; TakafusaAndo(1987), “INK FOR MARKING PEN”, May 12,
1987
[7] Ono, T. (1991). Organic solvent-based ink composition, Google Patents.
[8] Zlotnick, J., et al. (1999). "Chromatographic and electrophoretic approaches ink
analysis." 733(1-2): 265-272.
[9] McCabe et al. (1986).Momentum Heat and Mass Transfer Fundamentals edited by
Robert Greenhorn.85800004725.
[10]Lokendra pal and dr. Paul d. Fleming (2006), the study of ink pigment dispersion
parameters, volume 2, 2006
[11] Thompson, B., Printing Materials: Science and Technology, PIRA, p. 329-330
(1998).
[12] Powar P. V, Lagad S B, AmbikarR.B, Sharma P. H., Herbal Ink: Safe, Easy and
Eco-friendly Alternative, International Journal of Pharmacognosy and Phytochemical
Research, Vol 6, Issue 2, June-August 2014, 146-150
[12] NoorhaslinaHashim1,*, Abdul RazakShaari1, AwangSohMamat1,
andSyarhabilAhmad1, Effect of Differences Methanol Concentration and Extraction

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 Production and Characterization Of Ink from Fluid of Warka And Kulkual 2012E.C

Time on the AntioxidantCapacity, Phenolics Content and BioactiveConstituents of

OrthosiphonStamineusExtractsMATEC Web of Conferences 78, 01004 (2016)
[14] Samuel Tadesse1, Kumar Ganesan2, Suresh Kumar P. Nair2,
NeethuLetha3andSharmilaBanuGani4*, preliminary phytochemical screening of various
solvent extracts of ficus vasta. (Family: Moraceae), an Ethiopian fig plant, world journal
of pharmacy and pharmaceutical sciences, volume 5, issue 3, 1184-1193, 2016.
[15] https://patentimages.storage.googleapis.com/76/8c/9f/e8b567ea5f1a58/EP2787047A
1.pdf
[16] http://en.m.wikipedia.org
[17] Loftin R (1993) Erasable ink. Retrieved 9th December 1993.
[18] Nwosibe PO*, Nwafulugo FU and Iliyasu N, Erasable Ink Production for White
Board Marker Using Locally Sourced Dye, Medicinal & Analytical Chemistry
International Journal, Volume 2 Issue 2, July 23, 2018
[19] Druid Philips (2002), Berries Production and Processing Products 2nd edition.
Pp.219-231.
[20] Carrol, Clifford C (1997) “US patent US6031023A”.
[21] Nishan Singh1, Vishal Sharma2, DETAIL STUDY OF INK FORMULATION
FROM NATURAL COLOURANTS, International Journal For Technological Research
In Engineering Volume 4, Issue 9, May-2017, ISSN (Online): 2347 - 4718]

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APPENDICES

Appendix A
1A. Effect of mixing ratio and methanol concentration on drying time
Mixing Methanol concentration
ratio 50 75 100
0.5 3.195 2.58 2.405
1 3.11 2.47 2.265
2 2.935 2.37 2.16

2A. Effect of mixing ratio and methanol concentration on drying time

Mixing ratio
Methanol
0.5 1 2
concentration
50 3.195 3.11 2.935
75 2.58 2.47 2.37
100 2.405 2.265 2.16

3A. Effect of mixing ratio and methanol concentration on pH value

Mixing Methanol concentration
ratio 50 75 100
0.5 4.85 5.25 5.45
1 5.25 5.65 5.9
2 5.35 5.53 5.65

4A. Effect of mixing ratio and methanol concentration on pH value

Methanol Mixing ratio
concentration 0.5 1 2
50 4.85 5.25 5.35
75 5.25 5.65 5.53
100 5.45 5.9 5.55

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5A. Effect of mixing ratio and methanol concentration on viscosity

Mixing ratio
Methanol
0.5 1 2
concentration
50 0.0016 0.00175 0.00186
75 0.00135 0.00144 0.00147
100 0.00115 0.00123 0.00142

6A. Effect of mixing ratio and methanol concentration on viscosity

Mixing Methanol concentration
ratio 50 75 100
0.5 0.0016 0.00135 0.00115
1 0.00175 0.00144 0.00123
2 0.00186 0.00147 0.00142

7A. Overall average experimental results

Mixing ratios

Solvent R1(1:2) R2(1:1) R3(2:1)

concentration
Drying Viscosity pH Drying Viscosity pH Drying Viscosity pH
(% v/v)
time(sec) time(sec) time(sec)
(Ns/m2) (Ns/m2) (Ns/m2)
50 3.11 0.00175 5.25 3.195 0.0016 4.85 2.935 0.00186 5.35

75 2.47 0.00144 5.65 2.58 0.00135 5.25 2.37 0.001465 5.53

100 2.265 0.00123 5.9 2.405 0.00115 5.45 2.16 0.00142 5.55

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Where, R is Warka to kulkual mass ratio

8A. Overall experimental results

Mixing ratios

Solvent R1(1:2) R2(1:1) R3(2:1)

concentration
Drying viscosity pH Drying viscosity pH Drying Viscosity pH
(% v/v)
time(sec) time(sec) time(sec)
50 3.18 0.0017 4.9 3.12 0.0018 5.2 3.00 0.00192 5.3

3.21 0.00175 4.8 3.10 0.0016 5.3 2.87 0.0018 5.4

75 2.54 0.0014 5.3 2.41 0.0014 5.6 2.35 0.00148 5.4

2.62 0.00148 5.2 2.53 0.0013 5.7 2.39 0.00145 5.6

100 2.50 0.00012 5.5 2.37 0.00125 5.9 2.21 0.00142 5.5

2.31 0.00011 5.4 2.16 0.00121 5.9 2.11 0.00142 5.6

9A. Statistical data of drying time

One-Sample Test

Test Value = 0

t df Sig. (2-tailed) Mean Difference 95% Confidence Interval of the

Difference

Lower Upper

Drying_time 38.385 5 .000 2.27667 2.1242 2.4291

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10A. Statistical data of pH value

One-Sample Test

Test Value = 0

t Df Sig. (2-tailed) Mean Difference 95% Confidence Interval of the

Difference

Lower Upper

pH 68.097 5 .000 5.4667 5.260 5.673

11A. Statistical data of viscosity

One-Sample Test

Test Value = 0

t df Sig. (2-tailed) Mean Difference 95% Confidence Interval of the

Difference

Lower Upper

viscosity 3.482 5 .018 .00109333 .0002863 .0019004

Appendix B
1B. analytical balance

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2B. Visco star plus viscometer

3B. pH meter

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4B. stopwatch application on mobile

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Appendix C

C1. Ingredients of ink formulation (blackberry, methanol, vinegar, fluid of kulkual and
Warka, carbon black)

C2. Ferric chloride reagent

C3. Collection of fluid of Warka, fluid of kulkual and blackberry

C4. Blackberry after preparation

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C5. Phenolic test

C6. Formulated ink

Appendix D

Experimental setup

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