UNIVERSITY OF GUAYAQUIL

FACULTY OF CHEMICAL ENGINEERING

CHEMICAL ENGINEERING
MATERIAL RESISTANCE
Chicaiza Rodríguez Mishel Estefany
6th Semester "6-2"
SEPTEMBER 5, 2018
Green synthesis and characterization of nanoparticles to obtain Zero-Iron Valente from
the Robusta Coffee seed extract.

Resum:

In the present work, the green synthesis of nanoparticles to obtain zero iron Valente
using the aqueous extract of seeds of the robusta coffee plant has been reported. Three
different samples of the coffee seed extract were prepared, to which phytochemical tests
were carried out to make their respective test of organic compounds and to determine
the presence of resins, saponins, reducing compounds, phenolic compounds, flavonoids
and alkaloids. The aqueous solution of ferric chloride was used, after reacting with the
coffee extract, led to the very stable and crystal clear rapid formation of iron
nanoparticles. The nanoparticle rate of the synthesis was very high, which justifies the
use of plants on microorganisms in the biosynthesis of metal nanoparticles through
more ecological and safe methods. The synthesis of iron nanoparticles is described
based on the change in color, change in pH, change in absorbance and the particle size
formed after reduction.

ABSTRACT:

In the present work, the green synthesis of nanoparticles to obtain zero iron Valente
using the aqueous extract of seeds of the robusta coffee plant has been reported. Three
different samples of the coffee seed extract were prepared, to which phytochemical tests
were carried out to make their respective test of organic compounds and to determine
the presence of resins, saponins, reducing compounds, phenolic compounds, flavonoids
and alkaloids. The aqueous solution of ferric chloride was used, after reacting with the
coffee extract, led to the very stable and crystal clear rapid formation of iron
nanoparticles. The nanoparticle rate of the synthesis was very high, which justifies the
use of plants on microorganisms in the biosynthesis of metal nanoparticles through
more ecological and safe methods. The synthesis of iron nanoparticles is described
based on the change in color, change in pH, change in absorbance and the particle size
formed after reduction.
GENERAL PURPOSE:

Obtain nanoparticles from the coffee seed extract and the addition of 0.001 M of ferric
chloride to synthesize and obtain zero iron Valente under atmospheric conditions.

Specific objectives:

• Prepare a coffee seed extract to carry out tests on both organic compounds and
nanoparticle synthesis

• Show a test of organic compounds from phytochemical screening

• Perform a UV analysis to find the diameter of the nanoparticles and the change in
absorbance.

1. Introduction

Nanotechnology involves the creation and use of materials, devices and systems
through the control of matter in the scale of nanometers in length, that is, at the level of
atoms, molecules and supramolecular structures. Nanotechnology refers mainly to the
synthesis of nanoparticles of varying sizes, compositions and controlled dispersity and
their potential to use human benefits [1].

Nanotechnology is reliable and allows the process to be environmentally friendly for the
synthesis of nanoscale particles. The nanometric size results in particular
physicochemical characteristics such as high surface area in relation to volume, which
potentially results in high reactivity. The biosynthesis of nanoparticles is a kind of high
and low focus in which the main reaction that occurs is reduction / oxidation. With the
antioxidant properties of plant extracts is reduced, they are usually responsible for the
reduction of metal compounds in their respective nanoparticles [2].

The green synthesis provides profitable advances, favorable to the environment, easily
extended for large scale, in this method there is no need to use high pressures, toxic
chemicals, among others. Green synthesis offers better manipulation for control over
crystal growth and stabilization [3].

2. ROBUST COFFEE

Robusta coffee (C. canephora) is native to the equatorial forests of Africa, from the west
coast in Uganda and the southern part of the Sudan, to the part of western Africa, at
elevations from sea level to approximately 1000 meters height. It is a smooth tree or
bush, with broad leaves that sometimes acquire a corrugated or wavy, oblong - elliptic
appearance, short, acuminate, rounded or widely coined at its base, 15-30 cm long and
5-15 cm Wide; the midrib is flat above, prominent below, the lateral ribs are 8-13 pairs;
the petiole is strong 8-20 mm long; the interpeciolar stipules [4]. Robusta has a higher
productivity compared to Arabica, being used for instant coffee and strong toast. This
species shows better results at sea level. It generates considerable amounts of
agricultural waste ranging from 30% to 50% of the total weight of coffee produced, of
which parchment and pulp are the main waste components in coffee processing [5]. The
improper handling of this waste carries a great environmental problem [6].

3. APPLICATIONS:

It has been used to treat contaminated groundwater. Work in recent years has shown
that it is also effective in removing contaminants relevant to drinking water, including
viruses and bacteria, chlorine, disinfection by-products, DBP precursors (eg, natural
organic matter), and metal ions [7] .

4. METHODOLOGY

4.1 Obtaining extract (procedure)

In a beaker, place the coffee seed and wash with distilled water, let the sample dry and
then crush it in a homemade blender, previously ensuring that the materials are
sterilized with alcohol. In a beaker place 150 ml of distilled water and heat with 15g of
the sample for 30 minutes in a range of 65-70 ° C with constant agitation, let the sample
cool. The extract is filtered using filter paper, the filtrate is collected in a test tube and
placed in refrigeration at 10 ° C. Several tests must be done to obtain better results.

4.2 Characterization (Phytochemical screening of coffee extract)

Phytochemical screening or phytochemical screening is one of the initial stages of

phytochemical research, which allows to determine qualitatively the main chemical
groups present in a plant and from there, guide the extraction and / or fractionation of
the extracts for the isolation of the groups of greater interest [8].

Phytochemical screening involves the extraction of the plant with appropriate solvents
and the application of color reaction and precipitation. It must allow rapid evaluation,
with sensitive, reproducible and low-cost reactions [9].

4.2.1 Resin Test

Into a test tube, 2 ml of the aqueous extract was added and diluted in 10 ml of distilled
water. In this test, a precipitate must be observed to determine the results of the test.

4.2.2 Fehling test

1 ml of Fehling A reagent and 1 ml of Fehling B reagent and 1 ml of aqueous extract

solution are added to a test tube. The mixture was stirred and heated for 6 minutes. And
it is possible to appreciate the results by changing the color.

4.2.3 Foam test: Recognition of saponins

Into a test tube, 1 ml of the aqueous extract was added and diluted with 5 ml of distilled
water, stirred for 10 minutes. And if foam was observed, the test was positive.

4.2.4 Ferric chloride test: Recognition of phenolic compounds

An aliquot of the aqueous extract is taken and mixed with 3 drops of a 5% ferric
trichloride solution. A change in coloration should be observed between: red, deep
green or blue.

4.2.5 Dragendorff test

Into a test tube, an aliquot of the aqueous extract is introduced and 1 drop of 1%
hydrochloric acid is added to be taken to a hot water bath for 1 minute. Allow to cool
and the whole is mixed with 3 drops of Dragendorff's reagent. In order to consider the
presence of alkaloids, definite turbidity (++) or precipitate (+++) must be obtained,
since opalescence (+) could indicate incomplete extraction of primary, secondary or
tertiary bases.

4.2.6 Mayer's test

Proceed in the same way as in the previous point until obtaining the acid solution, to
which a small amount of sodium chloride powder will be added, then it is stirred and the
whole is filtered. 2 or 3 drops of Mayer's reagent are added and the results must be
observed: opalescence (+), defined turbidity (++) or precipitate (+++). The presence of
alkaloids is evidenced in the same conditions as Mayer's trial.

Table 1. Results of phytochemical screening on robusta coffee seed extract

Observations: In the Reducing Compounds Fehling test it was observed that in sample 2
and 3 it became yellow. If the crystalline product is yellow, this is an indication of a
saturated carbonyl compound, so the reaction becomes negative.

4.3 Synthesis of zero-valent iron nanoparticles:

During iron synthesis of nanoparticles both the precursor and the reducing agent were
mixed in a clean sterilized flask 1: 1 ratio. For the reduction of Fe ions, 5 ml of filtrate
of the seed extract was mixed in 5 ml of a 0.001 M aqueous solution of FeCl 3 with
constant stirring at a temperature of 50-60 ° C. For this, 3 samples were made. Within a
certain time it turns from a Brown color to a Brown color obtained by nanoparticles.

Figure 1. Synthesis of iron nanoparticles after leaving the mixture at rest at room
temperature.

4.4 UV-Vis Spectra Analysis:

The reduction of pure Fe ions to Fe ° was monitored by measuring the UV-Vis spectrum
by sampling aliquots (0.3 ml) of Fe nanoparticle sample dilution solution in 3 ml of
distilled water. UV-Vis spectral analysis was performed by using UV-Vis in the range
of 200-600 nm and observed the absorption peaks at 216 nm. It was determined that the
nanoparticles formed had the highest absorption peak at 216 nm, with a value of 1376A,
3.4% of Transmittance and 13.57 ppm of concentration regions due to the excitation of
surface plasmon vibrations in the FeNPs solution, which are identical to the spectrum of
UV-visible characteristics of metallic iron.

Figure 2. Absorption of the nanoparticle solution at 216 nm.

4.5 Reaction Mechanism

Quinic acid: Quinic acid has been used as a standard to determine the composition of
organic acids in bitter gentian tea and in the development of cranberry fruit by HPLC
[12]. It can be used in the preparation of 3,4-O-isopropylidene-3 (R), 4 (S) -
dihydroxycyclohexanone. Quinic acid, a plant metabolite, is a chiral component used in
the chemical synthesis of several steps of natural compounds [10].

Figure 3. Mechanism of reaction of Iron nanoparticle formation from the oxide-

reduction between and the Iron ions.

Quinic acid, 1,3,4,5-tetrahidoxycyclohexane-1-carboxylic acid, is a vegetable acid very

abundant in nature that was found in the cinconarinda and also in the coffee seeds and
leaves of many plants [11]. ]

• The reaction can be represented as:

C15 H12O6 + Fe + 3 → C15H10O6 + Fe0 + 2H + 1

• Formation of metal-organic complex with the release of 2 protons.

C15 H12O6 + Fe + 3 → [C15H10O6] -2 2 [Fe] + 3 → 2 H + 1

• Ionic cloud formation: The nearby atoms of Fe0 will begin to collide to form iron
nanoparticles, which will be stabilized by the polyphenolic components.

RESULT AND DISCUSSION

The seed extract is used to produce iron. The nanoparticles in this experiment are based
on Fe + 3 ions that are reduced in Fe0 when coffee seed extract is mixed with a FeCl3
solution in a ratio of 1: 1. The reduction is followed by an immediate change in color of
brown to brown Black and the change in the pH of the solution. It is well known that
Ferric Chloride has a bright yellow color in distilled water. In the mixture of the seeds
of plant extract with the aqueous solution FeCl3 changed the color of the solution
immediately and the reduction of pH, which may be an indication of the formation of
iron nanoparticles. In this experiment it was observed that the pH changes from a high
acidic pH to a low acid pH.

CONCLUSION

It has been shown that the extract is very effective for the preparation of iron
nanoparticles that shows good stability in solution, by virtue of the UV-Visible
wavelength, nanoparticles show resonance behavior. The ferric chloride with the agent
reduction ie the coffee seed extract has shown a remarkable color change with the
change in question in the pH of the solution. The success of such a rapid time scale for
synthesis of metallic nanoparticles is an alternative to chemical synthesis protocols and
low cost reduction to synthesize iron nanoparticles.

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ANNEXES:

OBTAINING THE EXTRACT

CHARACTERIZATION
Obtaining all the tests carried out Obtaining iron nanoparticles