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Vol. 9. Issue 1.
Pages 1119-1128 (January - February 2020)
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Vol. 9. Issue 1.
Pages 1119-1128 (January - February 2020)
Short Communication
DOI: 10.1016/j.jmrt.2019.11.035
Open Access
Photocatalytic degradation of disperse dye Violet-26 using TiO2 and ZnO nanomaterials and process variable optimization
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Aneela Jamila, Tanveer Hussain Bokharia,
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Corresponding author.
, Tariq Javedb, Rahat Mustafac, Muhammad Sajidd, Saima Noreene, Muhammad Zuberc, Arif Nazirc,
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Corresponding author.
, Munawar Iqbalc, Muhammad Idrees Jilanib,
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Corresponding author.
a Department of Chemistry, Government College University Faisalabad, Pakistan
b Department of Chemistry, University of Sahiwal, Sahiwal, Pakistan
c Department of Chemistry, The University of Lahore, Lahore, Pakistan
d Department of Botany, University of the Punjab, Lahore, Pakistan
e Department of Chemistry, University of Agriculture, Faisalabad, Pakistan
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Table 1. Characteristics of dispersive dye V-26.

The degradation of disperse V-26 in solution using UV; UV/H2O2, UV/H2O2/TiO2 and UV/H2O2/ZnO were investigated. The impacts of various key parameters i.e. initial pH, concentration of hydrogen peroxide (H2O2) dose and the dye concentration effect on degradation were studied. The maximum degradation of 93 % was optimized using UV/H2O2/TiO2 at pH 3 in 60min. Fourier transform infrared spectroscopy (FTIR) and gas chromatography-mass spectrometry (GCMS) were applied to check the products obtained after complete degradation. The removal of peaks of certain groups present in dye molecule assured the maximum degradation of dispersive V-26. In biological treatment, cytotoxicity reduction and Ames test were used to check the toxicity level of products. Certain water parameters i.e. dissolved oxygen (DO), chemical oxygen demand (COD) and biological oxygen demand (BOD) were also performed to ensure the maximum degradation of DV-26. DO was increased up to 82 %. The COD and BOD were reduced considerably owing to the treatment of disperse dye Violet 26 at optimum settings of process variables. The degradation of disperse dye V-26 with UV/H2O2/ZnO was 90.1 % which increased up to 93 % with the alternative photo-catalyst UV/H2O2/TiO2.

Disperse V-26
Full Text

The application of dyes and synthetic dyes, which covers almost all areas of life is constantly increasing and developing in many branches i.e. leather tanning industry, textile industry, food technology, paper production, pharmaceuticals and hair colorings [1]. The unwanted effluents which directly produce from unspent dyes are generally discharged without any further treatment [2]. This dyes effluent has major effect on the change of color of water even at low concentrations [3]. Moreover, usage of dyes significantly disperse dyes has been increased from 1970s [4]. Dyes are basically classified according to process of dyeing. The common classes of dyes include acid dyes, reactive dyes and disperse dyes. Reactive and acid dyes are water soluble. Reactive dyes are employed for cotton while acid dyes are used for wool, nylon, silk and some modified acrylic textiles. Finally, disperse dyes are generally partially soluble in water and used for polyesters fibers. They are less water soluble, hence solubility can be increased with the mixing of disperse dye with some water miscible organic solvents. They are largely applied as dispersion in the textile dyeing process [5–7].

Among all the commercial dyes the disperse dyes constitute a major part involved in a vast range of processes in the different industries. The presence of azo group (NN) attached to two substituents is very important characteristic of disperse dyes [8]. Owing to the toxicity of disperse dyes and massive mass production property lead to the requirement of developing new techniques. The difficulty in treating textile wastewater containing disperse dyes is the insufficient of biological processes [9–11]. Disperse dyes are among the persisting class of dyes due to recalcitrant nature and non-biodegradable behavior [12]. In the environmental fraternity the treatment of dye containing wastewater is considered very challenging due to this reason. Oxidation is the best known and most applied treatment to destroy the structure of dyes. In present years, the usage of advanced oxidation processes (AOP’s) have gained much interest especially with UV-H2O2 based system [13–15] which is very good technique to enhance the degradation of dyes. Furthermore, H2O2 decomposes into water and oxygen, hence it is known as friendly oxidant. Presence of ozone in water may arises some difficulties and serious problems [16]. These problems and issues can be resolved and avoided by oxidation with H2O2 stimulated with UV light. This recent work is basically focused to check the comparable photo-catalytic activity of ZnO and TiO2 towards disperse dye degradation. TiO2 and ZnO which are known as semiconductor photo-catalyst have been mostly applied to degrade destructive organic pollutants [17–20] into inorganic compounds like CO2, HCl and water [21–25]. TiO2 and ZnO are often used as catalytic agents since these semiconductors possess great properties like low cost, greater stability, zero toxicity and high efficiency. TiO2 semiconductor photo-catalyst has advantage over ZnO due to its stability under different varying conditions, greater availability of radicals production, and its easy access and economic cost [9,10,26,27].

The present study aims to examine the ultraviolet radiation with hydrogen peroxide, hydrogen peroxide/TiO2 and hydrogen peroxide/ZnO to degrade the disperse V-26 (Fig.1a, Table 1) and to produce compounds such as CO2 and H2O. The efficiency of process was gauged on the basis of dye degradation, toxicity reduction and water quality improvement. FTIR and GC–MS analysis was also performed to assure the degradation of end products of disperse V-26.

Fig. 1.

(a) Structural formula of disperse Violet 26 (b) Absorption spectra of disperse Violet 26 dye.

Table 1.

Characteristics of dispersive dye V-26.

Name  Dispersive Violet 26 
Molecular formula  C26H18N2O4 
Molecular weight (g/mol)  422.43 
Chemical nature  Anionic Violet 26 
Colour Index name  violet 
Colour Index number  62025 
λmax (nm)  641 
Reactive group  Amino group 
2Material and methods

All the chemicals and reagents used in this study were of analytical grade. The molecular structure of commercial C.I. disperse V-26 (C26H18N2O4, MW: 422.43g/mol) is shown in Fig. 1. The dye was taken from Khawaja & Company Dyes and Chemicals Faisalabad with no further purification. TiO2 particles were prepared from Degussa (P25). TiO2-P25, hydrogen peroxide and ZnO was purchased from Sigma Aldrich. The pH of the disperse V-26 solutions was adjusted by using dilute HCl (0.1M) and NaOH (0.1M). Disperse V-26 in their aqueous solution was subjected to UV/H2O2/TiO2 and UV/H2O2/ZnO treatment and was examined using spectrophotometer (Cecil 7200). To prepare the disperse dye V-26 samples, distilled water was used. Various parameters including concentration of photo-catalysts, concentration of dye, UV dosage, pH, H2O2 were optimized to check the efficiency of photo-catalytic degradation process.

2.1Irradiation of samples and analysis of disperse V-26 dye

The experiments for degradation using photo-catalytic techniques were performed by stuffing different concentrations (50mg/L, 100mg/L, 150mg/L) of the stock solution (1000mg/L) of given disperse dye solutions in the UV chamber. UV reactor was used having following specifications (wavelength 254nm, power 144W and shaker speed 120rpm). Absorbance of all samples is noted at λmax 641nm before and after treatments. In these concerned experiments, the solution of disperse V-26 was stirred by magnetic stirrer in the presence of TiO2 and ZnO in the absence of light for 60min to extent the adsorption equilibrium before UV radiation treatment. Millipore membrane with pore size 0.45μm was used to filter the solutions of disperse dye V-26, and calibration curve method was significantly used to determine the UV–vis absorbance characteristics by UV–vis spectrophotometer in the University of Agriculture, Faisalabad (UAF). The percentage degradation was calculated by applying formula:

% Degradation=100×(C0C)/C0
Where C0=initial concentration of dye solution, C=concentration of dye solution after photo irradiation.

2.2Toxicological tests and water evaluation parameters

Elimination of H2O2 from irradiated samples was very necessary to avoid its toxic impact. For this purpose, addition of minor quantities of MnO2 (< 1mg/mL) was made to lessen the impact of H2O2. After a given reaction time of 45min. the solution was clarified and uncovered to the toxicity tests such as hemolytic and Ames test. Hemolytic test was performed for cytotoxicity results, while Ames test is used to assess the mutagenicity of tested samples. All the tests were performed at the Biochemistry Laboratory, Department of Biochemistry, UAF. Cytotoxicity assay was evaluated by performing hemolytic experiments against human red blood cells (RBCs). Triton X-100 was used as positive control. To check the mutagenic prospective of chemical compounds the biological assay like Ames test was performed. A positive test shows the carcinogenic nature of chemical, since cancer is frequently related to mutation. However, a number of false-positives and false-negatives are known. The test serves as a quick and advantageous assay to evaluate the carcinogenic nature of a compound.

The determination of the DO was done from Hi-Tech Lab UAF, Pakistan. The samples were taken before and after irradiations and also with additional parameters like H2O2 and TiO2 and ZnO. For COD determination the complete oxidation of the organic matter should be done. The test for the determination of COD was done by dichromate (K2Cr2O7) method. The reduction of the COD values depends upon a number of the factors. The addition of the hydrogen peroxide, ZnO and TiO2 also increased the reduction of the COD.

In the BOD the oxygen used by the bacteria is calculated by comparison of amount of oxygen left behind after five days with the initial oxygen amount which was a known quantity [28]. The amount of dissolved oxygen at room temperature is about 8mg/L. The BOD was calculated by previously reported methods.

3Results and discussion3.1Effect of dye concentration and irradiation time

To design the model of numerous initial dye concentrations is for the basic purpose of inserting the impact of initial dye concentration to the degradation equation. Various concentrations (50mg/L, 100mg/L, 150mg/L) of disperse V-26 was irradiated with UV radiation remaining other parameters constant at various irradiation times (30−60min.) to evaluate degradation efficiency. Fig. 2(a) shows the plot of degradation with respect to various irradiation times. When time taken was 30min. degradation was highly effective at the low concentration of the dye. The degradation efficiency decreases by increasing the initial dye concentration. The reason is that the solution become more intense in color by increasing the disperse V-26 concentration and the dye molecules adsorbed on the surface, hence making the degradation process more difficult. The decrease in degradation was observed at higher initial concentration of dye may be owing to presence of low relative number of OH radicals because by increasing dye concentration, competition between dye molecule and OH radicals is increased [29,30]. These findings are supported by previous studies which show that the concentration of dye has substantial influence on dye degradation (photo-catalytically) e.g. effect on Coralene Red F3BS dye under UV irradiation [31]. It was observed that dye degradation was variable at different dye initial concentration. The same process was repeated by taking different intervals of time i.e. 45min and 60min. It has also been noticed that also by increasing the irradiation time, degradation of disperse V-26 also improved on low dye concentration (50mg/L).

Fig. 2.

(a) Percent degradation efficiency of disperse V-26 as a function of initial dye concentration at various irradiation times (30−60min.) and (b) Percent degradation graph for disperse V-26 at different pH value (3–9).

3.2Effect of pH

The effect of pH on the rate of degradation of different concentrations of disperse V-26 (50ppm, 100ppm, 150ppm) at different pH values of 3, 5, 7, and 9 was checked. pH plays a significant role in the discoloration of dyes by H2O2/UV with different photo-catalyst (ZnO, TiO2) process. In this study TiO2 showed more catalytic activity under UV light irradiation than ZnO, that is why H2O2/UV/TiO2 plays a significant role in degradation efficiency. Degradation and discoloration process is more effective in an acidic medium [32]. Increasing the pH from 3 to 9 led to a noticeable degrease in degradation efficiency from 92 % to 95 % as reference [33] demonstrated. At basic pH the reduction in efficiency can be observed because of the fact that a large part of H2O2 is utilized for the breakdown of alkalis forming oxygen and water rather than producing hydroxyl radicals under UV radiation. Moreover, at higher pH values, the H2O2/UV/TiO2 process is very sensitive to the scavenging effect of carbonate [34]. Hence the instant concentration of hydroxyl radical decreases causing efficiency decrease. Temperature does not have any significant effect on discoloration of the dyes. Fig. 2b Shows the effect of pH on degradation efficiency of disperse V-26.

3.3Effect of hydrogen peroxide

The impacts of H2O2 concentration on disperse V-26 degradation under H2O2/UV was also investigated in the range of 0.3-0.9mL/L and the result is shown in Fig. 3. In the absence of H2O2 the value of %age degradation was 63.1 % but this value was suddenly increased up to 82.7 % by the addition of hydrogen peroxide (0.9mL) with H2O2/UV. By increasing H2O2 concentration the degradation efficacy was increased. This is due to photo irradiation of H2O2 to diminish OH· and the ability of H2O2 for trapping electrons. In the process of radiolysis, production of hydroxyl radicals (OH) favors the oxidative degradation of dyes and this phenomenon can be more enhanced in the presence of H2O2[35]. Results are given below which clearly show that in the absence of electron acceptor such as H2O2 decomposition of disperse V-26 decreases by increasing the dye concentration exhibiting the reason of intense color by increasing concentration. While adding the H2O2 the degradation pattern suddenly increased.

Fig. 3.

(a) Comparison Percent degradation with UV and UV/hydrogen peroxide and (b) Percent degradation of disperse V-26 with different amounts of H2O2 (0.3–0.9mL).

3.4Effect of TiO2, ZnO photo-catalysts dose

In order to get maximum degradation efficiency of disperse V-26, various concentrations of two photo-catalyst TiO2 (0.2g, 0.4g, 0.6g) and ZnO (0.2g, 0.4g, 0.6g) were used (Fig. 4) while keeping all other parameters constant. Maximum degradation efficacy (93 %) was achieved with H2O2/UV/TiO2 as compared to H2O2/UV/ZnO, which was (90.1 %). The decrease in the degradation efficacy was attributed to the reference [27], which clearly indicated the enhanced TiO2 catalytic activity under UV light. The energy band gap of TiO2 is 3.2eV as compared to energy band gap of ZnO, which is 3.3eV. TiO2 is preferred over ZnO due to its stability under various conditions, its easy availability, non-toxic nature and its low cost results are demonstrated in Fig. 6.

Fig. 4.

Comparison between degradation efficiency of photo-catalysts TiO2 (0.6g) and ZnO (0.6g).

3.5Water quality parameters

In water or liquids, gaseous, free and non-bonded oxygen refers as dissolved oxygen. The sample solution of 50ppm with addition of 0.9mL H2O2 + 0.6g TiO2 and 0.9mL H2O2 + 0.6g ZnO was checked for DO, COD and BOD analysis. The DO values increased up to a significant rate after treatment which is the clear indication of degradation of dispersive V-26. (Fig. 5) shows the comparison in the values of DO in mg/L before and after treatment with different parameters. Before treatment the DO value was 2.01mg/L which suddenly increased up to 3.25mg/L with 0.9mL H2O2 + 0.6g ZnO and further increase up to 5.15mg/L with 0.9mL H2O2 + 0.6g TiO2. The BOD values before irradiation were 585mg/L, 490mg/L and 375mg/L. Hydrogen peroxide showed a major role in BOD reduction. After irradiation these values were reduced to 315mg/L, 205mg/L and 105mg/L shown in Fig. 5b. BOD reduction was up to 82.3 % in presence of H2O2 because hydrogen peroxide interacts with aqueous electron and hydrogen radical and may scavenge these species. Actually oxidative degradation of dyes occurs by hydroxyl radicals generated during radiolysis and is facilitated in the presence of hydrogen peroxide [35]. This result is strongly proved by comparing the BOD values already reported in the literature. For example, the initial AR and AY solutions had BOD values equal to 400, 330mg/L, respectively. The UV irradiation caused a decrease in the BOD of the two dye solutions. The reduction in BOD values from 400 to 120mg/L and from 330 to 80mg/L respectively occurred in the presence of H2O2[36]. After irradiation the values of COD reduced to a significant rate due to breakdown of organic matter. It was thought that the hydrogen peroxide may decrease the COD to a significant value but practically it was noted that the value of COD increased by addition of hydrogen peroxide. The 50ppm solution of disperse V-26 has COD value 925.895mg/L before irradiation and was decreased to 515.146 for 50ppm+0.9mL H2O2 +0.6g ZnO. Further decrease up to 397.34mg/L was observed (Fig. 5c). The COD values of disperse V-26 were strongly recommended by giving a comparison of these values with the already reported COD values of two dyes in literature [37–42]. The COD values of two dyes AR and AY solutions were equal to 1200, 1000mg/L respectively before irradiation but suddenly decreased up to 310mg/L and 275mg/L after AOP treatment [36].

Fig. 5.

(a) DO (mg/L), (b) BOD values in mg/L and (c) COD values (mg/L) before and after treatment with different photo-catalyst (ZnO, TiO2).

Fig. 6.

(a, b) FTIR bands of dispersive dye V-26 before and after UV irradiation and (c) GCMS profile of disperse violet 26 treated by UV in the presence of H2O2 and TiO2.

3.6FTIR and GC–MS analysis

FTIR was used for un-treated and treated samples to identify the degraded end products. FTIR spectrometer (U-2001, Schimadzu, Japan) at HI-TECH lab Government College University Faisalabad (GCUF) was used in the range of 4000−400cm−1for analysis. Spectrum of un-treated sample showed different vibrational peaks due to different functional groups present in disperse V-26. Spectrum of treated sample of sample dye has shown great variation by breakage of different functional groups and destruction of aromatic rings. After irradiation with UV/H2O2/TiO2, the characteristics bands of dye molecule were vanished, which showed clear indication of destruction of DV-26 [43]. Results are demonstrated in Fig. 6. To assure the results obtained after UV irradiation treatment, toxicity profiling and water parameters analysis, the treated sample was further subjected for gas chromatography–mass spectroscopy (GCMS). The GCMS was performed for maximum degraded DV-26 sample treated with UV in the presence of H2O2 and TiO2. The GCMS analysis clearly indicates the complete breakdown of disperse violet 26 into lower molecular weight inorganic compounds and ions as well i.e. (H2O, CO2, NO3- etc). The GCMS spectrum is shown in (Fig. 6c).

3.7Toxicological tests (Hemolysis, Ames)

Hemolysis is caused by microbes and other parasites like the plasmodium falciparum, hence known as infectious disease [44]. The cytotoxicity parameter was observed for untreated and treated samples of dispersive V-26. The cytotoxicity of un-irradiated 50ppm was 16.1 % and it was reduced to 10.3 % when irradiated with UV radiation. Further reduction up to 7.6 % was noticed with the addition of photo-catalyst (TiO2). The Hydrogen peroxide and photo-catalyst TiO2 also showed a major effect on the reduction of cytotoxicity of the disperse V-26 (Fig. 7a). Ames test was performed to evaluate the mutagenic nature of DV-26. 50ppm solution of disperse violet-26 was analyzed before and after UV irradiation for the mutagenicity using TA98 and TA100 strains, which are very sensitive to frame-shift and base-substitution mutagens respectively [45–47]. The disperse V-26 solution contained the mutagenicity about 8 (91.6 %) and 6(88.5 %) before irradiation. The 50ppm solution was irradiated by UV radiations and mutagenicity was reduced to a significant rate as 2 (98.9 %) and 2 (98.9 %) plates were affected by dye solution which is a clear evidence of reduction in the mutagenicity due to hydrogen peroxide. It was known that the UV radiation was not considered to be effective in the reduction of mutagenicity but with addition of hydrogen peroxide the mutagenicity was reduced to maximum level (Fig. 7b).

Fig. 7.

(a). Hemolysis and (b) mutagenicity reduction of DV-26 with the help of UV radiation and Hydrogen peroxide and TiO2.


The degradation of disperse V-26 was done using UV/H2O2 assisted with various photo-catalysts (ZnO, TiO2). The photo-catalytic method was found more efficient for the degradation of DV-26. Because of the high catalytic effect, greater stability and non-toxic nature of TiO2 photo-catalyst, the degradation was achieved up to 93 % with UV/H2O2/TiO2. The energy band gap of TiO2 (3.2eV) is less than energy band gap of ZnO (3.3eV) which makes it more efficient photo-catalyst and comparable to ZnO. Toxic effect of disperse dye V-26 was decreased by toxicity profiling tests (Hemolysis, Ames). The decrease in the toxicity of DV-26 assured the degradation of dye. The DO, COD and BOD were also improved significantly as a result of UV/ H2O2/TiO2 treatment for DV-26. The physico-analytical techniques like FTIR and GCMS were also performed to check the degradation of disperse dye V-26 and the removal of certain peaks in the molecule of dye confirmed the degradation of dye.

Conflicts of interest

The authors declare no conflicts of interest.


Authors appreciatively acknowledge the Higher Education Commission Pakistan for monetary support of this research work (Project No. 5626/Punjab/NRPU/R&D/HEC/2016).

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Journal of Materials Research and Technology

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