photocatalytic degradation of procion bright...

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Indo American Journal of Pharmaceutical Research, 2014 ISSN NO: 2231-6876

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INDO AMERICAN

JOURNAL OF

PHARMACEUTICAL

RESEARCH

PHOTOCATALYTIC DEGRADATION OF PROCION BRIGHT TURQUOISE MX-G DYE

USING BIOGENIC SILVER NANOPARTICLES (AGNPS) SYNTHESIZED FROM ALPINIA

CALCARTA ROSC.

Sachindri Rana

1, K. Ghanapriya

2, K. Priadharsini

2, K. Rajagopal

1 and P. T. Kalaichelvan

2

1 Department of Biotechnology, Vels University, Pallavaram, Chennai-600117, Tamil Nadu, India.

2 Centre for Advanced Studies in Botany, University of Madras, Guindy Campus, Chennai-600025, Tamil Nadu, India.

Corresponding author

Sachindri Rana

Department of Biotechnology, Vels University,

Pallavaram, Chennai-600117, Tamil Nadu, India

[email protected]

Copy right © 2014 This is an Open Access article distributed under the terms of the Indo American journal of Pharmaceutical

Research, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

ARTICLE INFO ABSTRACT

Article history

Received 09/03/2014

Available online

16/03/2014

Keywords

Biogenic Silver

Nanoparticles, AgNps,

Alpinia Calcarata Rosc.,

Procion Bright

Turquoise MX-G,

Reactive Dichlorotriazine

Dye, Photocatalytic

Degradation.

.

In this study, a green approach of synthesizing stable biogenic silver nanoparticles (AgNPs)

using aqueous extracts of rhizomes of Alpinia calcarata Rosc. and silver nitrate has been

reported and is being used in the photocatalytic degradation of Procion Bright Turquoise MX-

G reactive dichlorotriazine dye. Green synthesis biogenic silver nanoparticles using aqueous

extracts of dry rhizomes of Alpinia calcarata Rosc. take place within 30 minutes. The

bioreduced silver nanoparticles have been characterized by Ultraviolet-visible Spectroscopy,

Powder X-Ray Diffraction, Fourier Transform Infrared Spectroscopy, Energy Dispersive

Spectroscopy, Transmission Electron Microscopy, High Resolution Transmission Electron

Microscopy and Atomic Absorption Spectroscopy and have been found to be 2-20 nm in size.

The photocatalytic degradation effect on Procion Bright Turquoise MX-G dye takes place

within 60 minutes and is confirmed by the decrease in absorbance in the concentration of the

dye with increase in time. This method of synthesizing silver nanoparticles is found to be very

cost effective and eco-friendly and thus can be economical and an effective alternative for a

large scale production of biogenic silver nanoparticles. These biologically synthesized

biogenic silver nanoparticles are also very effective in photocatalytic degradation of Procion

Bright Turquoise MX-G dye which is a commercial reactive dichlorotriazine dye. These

biogenic silver nanoparticles can thus be used in degradation of dyes in textile industries

before leaving out the dye effluent into the environment.

Please cite this article in press as Sachindri Rana et al. Photocatalytic degradation of Procion Bright Turquoise MX-G dye using

biogenic silver nanoparticles synthesized from Alpinia calcarata Rosc. Indo American Journal of Pharm Research.2014:4(03).

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Vol 4, Issue 03, 2014. Sachindri Rana et. al. ISSN NO: 2231-6876

INTRODUCTION

The evolutionary boom in Nanotechnology has generated different nanosized materials and of this, metal nanoparticles are

one of the most interesting and promising ones. Recently, metal nanoparticles have been reported as effective photocatalysts for

degrading chemical complexes, under ambient temperature with visible light illumination [1]. This can be achieved by increasing the

optical path of photons leading to a higher absorption rate of nanoparticles in the presence of a local electrical field [2]. These

nanoparticles show new and improved properties based on their morphological structures and characteristics as compared to bulk

materials [3].

Recently, Silver nanoparticles (AgNPs) have been playing a major role in Nanotechnology. Biologically synthesized AgNPs

or biogenic AgNPs have been a very interesting area of research in the past few years due to their non-requirement of high pressure,

energy, temperature, and toxic chemicals [4]. Presently biogenic AgNPs are being synthesized from microorganisms, yeasts and

plants. Plant extracts are used to synthesize biogenic AgNPs in few minutes. These biogenic AgNPs have received attention due to

high surface plasmon resonance strong absorption in the visible region [5]. Their unique size dependent properties make them superior

and indispensable as they show unusual physical, chemical, and biological properties [6].

Alpinia calcarata Rosc. (Zingiberaceae) is a medicinal plant and is used for several pharmaceutical purposes. It is cultivated

in tropical countries including Sri Lanka, India and Malaysia. The rhizomes of Alpinia calcarata are used for medicinal purposes [7].

Extracts of Alpinia calcarata Rosc. have been found to show antibacterial [8], antifungal [9] and antihelminthic activity [10]. The

extracts of rhizomes have also been used in the treatment of bronchitis, cough, respiratory ailments, diabetics, asthma [11] and arthritis

[11, 12]. The aqueous extracts of rhizomes contain phytochemicals that aid to reduce of silver nitrate to biogenic silver nanoparticles.

This method of production is very cost effective and eco-friendly and thus can be economical and an effective alternative for a large

scale production.

Commercially available textile dyes are rich sources of organic compounds that pose threat to the environment as they are

highly toxic to the ecosystem. The various textile dye effluents enter the water bodies and soil and ultimately effect the ecosystem by

causing environmental hazards. Due to high amount of various organic compounds, the conventional biological methods are

ineffective for their de-colorization and degradation [13]. Procion Bright Turquoise MX-G is a reactive commercial dichlorotriazine

dye used in textile industries. It is a very bright, strong color that has very high reactivity making it suitable dyeing color for textile

even at low temperatures (20◦-30

◦ C). It contains copper at levels of 1 to 5% of the weight of the dye powder.

Sunlight is abundantly available natural energy source and its energy can be conveniently exploited for degradation of commercial

dyes.

Hence, the present study has been aimed to study the photocatalytic degradation of Procion Bright Turquoise MX-G dye; a

commercial reactive dichlorotriazine dye using biogenic AgNPs synthesized using the aqueous extracts of dry rhizomes of Alpinia

calcarata Rosc. that acts both as reducing and stabilizing agents.

MATERIALS AND METHODS

Preparation of Aqueous Rhizome Extract

Rhizomes of Alpinia calcarata Rosc. were cleaned, dried and powdered using a Dry Grinder (Fig. 1a-c). The aqueous

rhizome extract was prepared by adding 1g of dry powder to 100 mL of distilled water and heated at 80° C for 3 minutes. This extract

was then filtered using Whatman 40 filter paper and the filtrate was refrigerated at 4° C for further use.

Biogenic synthesis of Silver Nanoparticles (AgNPs)

5mL of the aqueous rhizome extract was added to 95 mL of 5 mM Silver nitrate (Sisco Research Laboratories Pvt Ltd,

Mumbai, India) and incubated at room temperature for 30 minutes. The solution turned brownish orange in color (Fig. 1d and Fig.

1e).

Fig. 1a – Morphology of Alpinia calcarata Rosc., Fig. 1b – Dry rhizomes, Fig. 1c – Powder of dry rhizomes, Fig. 1d - Silver

nitrate (AgNO3) and Synthesized biogenic Silver nanoparticles (AgNPs), Fig. 1e – Green synthesis of biogenic AgNPs at

different time intervals

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Characterization of biogenic Silver Nanoparticles

Ultraviolet-visible Spectroscopic studies

The synthesized AgNPs were studied at regular intervals using Hitachi U 2900 UV-Visible Spectrophotometer between

ranges of 300 - 800 nm and at a scanning speed of 600 nm/ min.

Fourier Transform Infrared Spectroscopic studies

The functional groups present in the rhizome of the plant and its role in the synthesis of AgNPs was determined by FT-IR

studies. The dried rhizome powder and biogenic AgNPs were mixed with KBr to make pellet and the FT-IR analysis was carried out

in transmittance mode by Schimadzu FT-IR 8300 in the range of 400 - 4000 cm -1

at a resolution of 4 cm -1

Powder X-Ray Diffraction studies

The synthesized dry AgNP powder was analyzed with Cu Kα1 filtered radiation (λ = 1.540598 Å) at a voltage of 40 kV and a

current of 30 mA using Seifert JSO Debye Flex XRD in a range of 10◦ to 70

◦. The peaks were matched with JCPDS file No-04-0783.

The obtained pattern was for fcc cubic crystal structure. The ratio between the intensities of diffraction peaks of the sample were

calculated and matched with the conventional values of JCPDS file No-04-0783. The crystalline size was calculated using the Debye–

Sherrer formula [14]. The lattice constant was calculated according to Bragg’s law [15]. The crystallinity index was calculated using

the formula-

Icry = Dp (SEM, TEM)/Dcry(XRD)

where, Icry is the Crystallinity Index, Dp is the particle size obtained from either SEM or TEM morphological analysis, Dcry is

the particle size calculated according to Debye–Sherrer formula in XRD [16].

Transmission Electron Microscopic studies

A drop of solution containing biogenic AgNPs was placed on the carbon coated grids and kept under vacuo desiccation

before analyzing with Hitachi H 7650 at 100 kV of acceleration.

Energy Dispersive Spectroscopic studies

The dry AgNP powder was used for this purpose using Hitachi S 3400 N operating at 30 kV of acceleration and at a

magnification of 25k and the energy dispersive spectrum (EDS) was recorded.

High Resolution Transmission Electron Microscopic studies

The stable biogenic AgNPs were washed and diluted by distilled water to attain the absorbance range of 0.5. Then one drop

of diluted AgNP sample was placed on Copper grid with Ultrathin Copper on holey carbon disc and was allowed to dry in vacuo.

After drying, the synthesized AgNPs were visualized using Tecnai G2 FEI High Resolution Transmission Electron Microscope

operating at 200 kV of acceleration. The SAED pattern was also obtained.

Evaluation of effect of biogenic AgNPs on the reduction of Procion Bright Turquoise MX-G dye

The photocatalytic degradation of Procion Bright Turquoise MX-G dye was evaluated outdoor with sun as the main source of

light. The intensity of light was measured using an Extech Lightmeter 401025 (Taiwan) Luxmeter. 1 mL of 50 µg/ mL AgNPs

solution was added to 50 mL of 10−4

M Procion Bright Turquoise MX-G dye solution. This mixture was then stirred for a minute in

darkness to ensure constant equilibrium of AgNPs in the dye solution. After this reaction, the mixture was kept under sunlight in a

borosil glass beaker at mean temperature of 32◦C with 60 minutes shine duration.

The absorption spectrum of the suspension mixture was measured using Hitachi U 2900 UV-Vis Spectrophotometer ranging

between 200 - 700 nm at a scanning speed of 600 nm/ min. This was done after centrifuging 2 mL of the reaction mixture at 10000

rpm for 10 minutes to ensure the degradation of the dye solution.

RESULTS AND DISCUSSION

Characterization of biogenic Silver Nanoparticles

Ultraviolet-visible Spectroscopic studies

The formation of biogenic AgNPs was easily detected and characterized by UV-Visible Spectroscopy owing to the reduction

of silver nitrate and due to the Surface Plasmon resonance (SPR), i.e., the interaction of electromagnetic radiation and the electrons in

the conduction band around the nanoparticles [17, 18]. AgNPs were observed strongly in the range of 400 - 450 nm in visible region.

In the present work, the biogenic AgNPs are rapidly formed (at pH 7) after the addition of Alpinia calcarata Rosc. aqueous extract,

evident from the appearance of brownish orange color at 422 nm which is the characteristic wavelength of silver nanoparticles [19]

with increase in absorbance at regular time intervals of 5, 15, 30, 45 and 60 minutes as depicted in Fig. 2.

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Fig. 2 - UV Visible spectrum of biogenic AgNPs using 95 mL of 5mM Silver nitrate and 5 mL aqueous extract of dry rhizomes

of Alpinia calcarata Rosc. incubated at room temperature (pH 7) with gradual increase in time

Fourier Transform Infrared Spectroscopic studies

FT-IR spectroscopy studies were carried out to identify the biomolecules that not only capped, but also helped in reduction

and stabilization of synthesized biogenic AgNPs. FT-IR spectrum of dry powder aqueous extract and synthesized AgNPs are shown in

Fig. 3. The absorption bands that appear in the IR spectrum of the dry rhizome powder (sample) could also be seen in the IR spectra of

phytocapped synthesized AgNPs. This shows that the phytoconstituents present in the aqueous extract protect the AgNPs from

aggregation.

Fig. 3 - FT-IR spectrum of sample (powder of dry rhizome) and synthesized biogenic AgNPs

The IR-spectrum of the silver nanoparticles showed absorption bands at 1038.1, 1380.4, 1635.2 and 3430.3 cm−1

. The

absorption bands at 1038.1 cm−1

correspond to C-N stretching vibrations of the amine. The absorption bands at 1635.2 cm−1

correspond to amide 1 band of proteins due to carbonyl stretch in proteins and absorption bands at 3430.3 cm−1

are due to the O-H

stretching in alcoholic compounds [20]. The sharp band at 1380.4 cm−1

is due to C-H stretching vibrations of aromatic and aliphatic

amines. IR spectroscopic study thus confirmed that the carbonyl group form amino acid residues and proteins has the stronger ability

to bind metal indicating that the proteins could possibly form a layer covering the metal nanoparticles (i.e., capping of silver

nanoparticles) to prevent agglomeration and thereby stabilize the medium. This suggests that the biological molecules could possibly

perform dual functions of formation and stabilization of silver nanoparticles in the aqueous medium [20].

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Powder X-Ray Diffraction studies

XRD studies were carried out to identify the crystalline nature of the synthesized biogenic AgNPs. Diffraction peaks were

observed at 2θ values of 38. 2°, 44.4° and 64.1° that can be indexed to (111), (200) and (220) reflection planes of face centered cubic

(fcc) as shown (Fig. 4).

Fig. 4 - XRD pattern of biogenic AgNPs

This study confirms that the resultant particles are (FCC) silver nanoparticles [21]. The ratio between the intensities of

diffraction peaks of (200) - (111) and (220) – (111) of the sample values were calculated to be 0.45 and 0.27 which were in agreement

with the conventional values of JCPDS File No. 04-0783 (0.40 and 0.25) [21]. The mean size of the biosynthesized AgNPs was

determined by Debye–Sherrer formula [14] and found to be in the range of 2-10 nm. The lattice parameter was calculated according to

Bragg’s law [15] and was found to be 4.077Å which was also in agreement with the conventional value of JCPDS File No. 04-0783

(4.08Å) [22]. The crystallinity index was calculated to be 1.3604 and was confirmed that synthesized silver nanoparticles were

monocrystalline in nature and the fcc structure was well indexed [16].

Electron Microscopy/ Energy Dispersive Spectroscopic studies

Electron Microscopy studies were carried out to view the size of the synthesized biogenic nanoparticles. The HR-TEM image

of synthesized AgNPs (pH 7) depicted in Fig. 5 (a) gives clear indications regarding size, shape and size distribution of nanoparticles.

The size of the synthesized biogenic AgNPs is approximately 2-20 nm. The SAED pattern of AgNPs reveals that the particles are

crystalline in nature as shown in Fig. 5 (b).

Fig. 5

(a) - HR-TEM studies of biogenic AgNPs

(b) – SAED pattern of biogenic AgNPs

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From TEM images, (Fig. 6) it can be seen that the AgNPs are capped with phytoconstituents of rhizome of Alpinia calcarata Rosc.

[23]. The figure also shows the synthesized AgNPs to be 5.63 to 13.85 nm in size.

Fig. 6 - TEM image of biogenic AgNPs

The result of EDS gives a clear idea about the elements present in the nanoparticles (Fig. 7).

Fig. 7 - EDS studies of biogenic AgNPs

As shown in the figure, the strong signal of the silver (Ag) atoms indicates the crystalline property. The carbon (C) and oxygen (O)

peaks in the EDS analyses can be attributed to the surrounding residual material and/or the carbon tape used for SEM grid preparation

[24, 25].

Effect of biogenic AgNPs on the reduction of Procion Bright Turquoise MX-G dye

Photocatalytic degradation of Procion Bright Turquoise MX-G dye was investigated using synthesized biogenic AgNPs [26]

by solar irradiation technique at different time intervals of 15 minutes for an hour [27]. The characteristic absorption peak of Procion

Bright Turquoise MX-G dye solution was found to be at 660 nm. Degradation of Procion Bright Turquoise MX-G dye at light

intensity of 45000-49000 Lux was visualized by decrease in peak intensity within 60 minutes of incubation time. There is no

considerable shift in peak position for Procion Bright Turquoise MX-G dye solution without exposure to biogenic AgNPs [28]. The

degraded samples were used for determining the possible changes in the absorption spectra of the dye in the UV -Vis range (Fig. 8)

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350 400 450 500 550 600 650 700

0.00

0.05

0.10

0.15

0.20

0.25

60 mins

30 mins

15 minsA

bso

rba

nce

Wavelength

Control

Fig. 8 – UV-Visible spectrum of photocatalytic degradation of Procion Bright Turquoise MX-G dye using biogenic AgNPs at

different time intervals

Compared to other irradiation techniques, solar light was found to be faster in decolorizing dye in the presence of metal

catalyst [29]. The adsorption of biogenic AgNPs on to the Procion Bright Turquoise MX-G dye solution increased with constant

increase in time. Altogether, the photocatalytic properties of Ag nanoparticles in visible light may well be due to excitation of surface

plasmon resonance (SPR), which is nothing but oscillation of charge density that can propagate at the interface between metal and

dielectric medium. AgNPs are good, highly efficient and stable photocatalysts under ambient temperature with visible light

illumination for degrading organic compounds and dyes [30]. Thus this study also reveals that biogenic AgNPs are stable and efficient

photocatalysts that actively degrade Procion Bright Turquoise MX-G dye which is a reactive commercial dichlorotriazine dye used in

textile and dyeing industries. This ensures that the treated dye effluent may be reused in the industries and also ensures environment

safety if the treated water is let out into the ecosystem.

CONCLUSION

In this study, a facile, environmental friendly and simple method has been adopted to synthesize silver nanoparticles

biologically using Alpinia calcarata Rosc., in room temperature within 30 minutes of incubation time and were characterized by UV

spectra, FT-IR, XRD, EDS, TEM, HR-TEM and AAS studies. The synthesized nanoparticles were found to be highly active in

degrading Procion Bright Turquoise MX-G reactive dichlorotriazine dye solution with visible light illumination within 60 minutes.

Thus, large volume of low concentration textile effluents could be treated with AgNPs in the industries in tanks open to sunlight, left

to stand for few hours, allowing efficient photocatalytic dye degradation and centrifuged to settle down the AgNPs before reusing this

treated water free from AgNPs and dye in the dyeing process or letting this treated water into the environment. These findings suggest

that, biogenic silver nanoparticles synthesized from Alpinia calcarata Rosc., can degrade dyes in the presence of sun light and paves

way for a cost effective treatment of textile industrial effluents.

ACKNOWLEDGEMENTS

We are thankful to Prof. R. Rengasamy, Director, Centre for Advanced Studies in Botany, University of Madras, Guindy

campus for providing lab facilities. We would like to show gratitude to the Head, Department of Nuclear Physics, University of

Madras for providing XRD facility and the Head, National Centre for Nanoscience and Nanotechnology, University of Madras, for

providing Electron microscopy facilities. We would also like to show appreciation towards the Head, Department of Chemistry, Anna

University for providing FT-IR facility.

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List of abbreviations

S. No Abbreviation Meaning S. No Abbreviation Meaning

1 Rosc. Roscoe 4 cm Centimeter

2 ◦ C degree Centigrade 5 mA Milliampere

3 % Percentage 6 kV Kilovolt

7 g Gram 13 µg Microgram

8 mL Milliliters 14 M Molar concentration

9 mM Millimolar 15 rpm Revolutions per minute

10 nm Nanometer 16 C Carbon

11 O Oxygen 17 H Hydrogen

12 N Nitrogen

Authors’ statements

Competing interests

The authors declare of having no conflict of interest.

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