IHJPAS. 36 (3) 2023 201 This work is licensed under a Creative Commons Attribution 4.0 International License *Corresponding Author : nsuzaneiaz@gmail.com Abstract Myrtle plant was washed, dried, and powdered after harvesting to produce a fine powder that was used in water treatment. created an alcoholic extract from the myrtle plant using ethanol, which was then analyzed using GC-Mass, Fourier Transform Infrared spectroscopy, and ultraviolet-visible spectroscopy to identify the active components. Zinc nanoparticles were created using alcoholic extract. We used FTIR, UV-Vis, SEM, EDX, and TEM to characterize zinc nanoparticles. Using a continuous processing procedure, zinc nanoparticles with myrtle extract and powder were employed to clean polluted water containing heavy metals. Firstly used 2g with 20ml polluted water and the result was ( Fe 96.20%, Cr 84%, Pb 100%, Sb 93.70, Cd 100%, andCu 90.60%) Secondly, weused Zinc nanoparticles to treat water the result was (Fe 96.20%, Cr 84%, Sb 54%, 64.50%, Cu 64.80). When Comparing between results myrtle powder and zinc nanoparticle we found myrtle plant was prefer in treatment water. Keywords: Myrtle plant, Zinc nanoparticle, pollutant water treatment, Heavy metals. doi.org/10.30526/36.3.3056 Article history: Received 2 October 2022, Accepted 28 November 2022, Published in July 2023. Ibn Al-Haitham Journal for Pure and Applied Sciences Journal homepage: jih.uobaghdad.edu.iq Green Synthesis Zinc Nanoparticles in the Treatment of Heavy Metals in the form of Complexes *uslim AbdullahMSuzan Department of Chemistry, College of Science for Women, University of Baghdad, Baghdad, Iraq. nsuzaneiaz@gmail.com Abbas Ali Salih AL-Hamdani Department of Chemistry, College of Science for Women, University of Baghdad, Baghdad, Iraq. Abbas_alhamadani@yahoo.co.uk Farqad Abdullah Resheed Ministry of Higher Education & Scientific Research & Science and Technology / Directorate of Environment & Water. Hightower3274@gmail.com https://creativecommons.org/licenses/by/4.0/ mailto:nsuzaneiaz@gmail.com mailto:nsuzaneiaz@gmail.com mailto:nsuzaneiaz@gmail.com mailto:Abbas_alhamadani@yahoo.co.uk mailto:Abbas_alhamadani@yahoo.co.uk mailto:Hightower3274@gmail.com mailto:Hightower3274@gmail.com IHJPAS. 36 (3) 2023 202 1. Introduction There was a pressing need to reuse water, particularly in the fields of industry or irrigation, as the sources of clean water over time started to diminish as the demand for it grew[1]. It was crucial creating scientific, practical, and effective ways to treat water because of the growing demand for pure and industrial water, which simultaneously increases water pollution and affects water sources with chemical pollution (both organic and inorganic)[2]. A qualitative and quantitative analysis of the pollutants in the water must come before choosing a treatment procedure, and only then can the optimal course of action be decided. There are therapies that use physical techniques, and there are others that use chemical or biological techniques. However, cost and efficiency[3,4]. are the key factors to consider when comparing various systems. Therefore, researchers looked for affordable and effective therapy options that wouldn't disturb the delicate balance of the environment. Due to their propensity to absorb chemical contaminants, plant residues are used in water treatment, according to many studies. Wastewater has been treated using water hyacinth, water lettuce, duckweed, and vetiver grass. Due to its unchecked development in water bodies, Eichhornia crassipes have been labeled a problematic aquatic free-floating weed. It is also challenging to manage and eradicate this plant from water bodies[5,6]. However, it has been regarded as a bioindicator because of its capacity to absorb heavy metals from aquatic habitats. Only a little amount of study has been done on the phytoremediation method of employing Eichhornia crassipes to clean kitchen wastewater. Chemists have been concentrating on nanotechnology in recent years, particularly nanotechnology connected to plants, or "Green Nano"[7]. In this work, we will investigate the treatment of heavy metals polluted water using zinc nanoparticles in combination with alcoholic myrtle extract using customized columns processing. In order to cleanse water tainted with phenols and aromatic chemicals, silver nanoparticles have already won the use of extracts utilizing specialized capsules[8]. To purify water of inorganic pollutants, another study combined zinc nanoparticles with cumin leaf extract [9]. 2. Materials and method 2.1. Materials and instrumentation The following chemical substances were employed, and a Shimadzu-3800 Spectro-meter equipped with a (FTIR) in the range (4000-400) cm-1 was used as a detector: methanol, ethanol, zinc sulphate, sodium hydroxide, ascorbic acid, and polyvinyl alcohol. Shimadzu 160 Spectro- photometer was used to find the electronic spectrum data. Compounds were subjected to mass indication analysis using a GC Mass100P Shimadzu. This study used scanning electron microscopy (SEM) to manage the analysis and describe the size and morphology of nanoparticles. The best technique for determining the NPs' morphology is (TEM). A sample is passed through an intense electron beam during this technique for microscopy, and the outcome of the electrons' interactions with the material is the creation of a picture.A little drop of nanoparticles was applied on a copper grid that had carbon coating, and it was left to dry under a mercury lamp for five minutes. Finally, readings were taken under stable voltage conditions at magnifications of 5000x, 10000x, 20000, and 50000x. To validate the presence of the zinc nanoparticle, EDX measurements were performed using a high-resolution spectrophotometer in a transmission electron microscope. IHJPAS. 36 (3) 2023 203 2.2 Plant harvest and preparation for grinding and extraction Used myrtle plants for this study came from the Kadhimiya District in Iraq's Baghdad Governorate. It was thoroughly cleaned with deionized water many times to get rid of any impurities, dried at room temperature, and then ground into a very fine powder using a special laboratory grinder for 15 seconds. Alcoholic myrtle extract was produced by mixing a solution of 65% methanol, 20% ethanol, and 15% free ionized water, allowing it to sit for a while, and then heating it to 50C. It was condensed simultaneously for eight hours using a laboratory condenser. At 50°C, the extraction procedure is carried out, then evaporation and condensation are used to boost enrichment. Show Figure 1. 2.3 Preparation of zinc nanoparticles The following steps were used to manufacture zinc nanoparticles with myrtle extract, using a modified version of Elumalai's method: placing 10 ml:20% of myrtle extract and 1000 ml of pure water in a round flask. The flask was left to be heated and stirred at different temperatures. After one minute, 17.5 g of zinc sulfate was added gradually while being continuously stirred [10] the mixture's acidity was then equalized by adding pure sodium hydroxide. The mixture was then put into a glass container and heated to 200°C for two hours. The filtered solution separates from the precipitate to complete the separation, and the precipitate is then collected and dried from the remaining water in A furnace set to 70°C will be used to do the drying; after it has been crashed, 17.5g of zinc sulfate will be gradually added to finish the mixing of the components. green powder that was produced is kept in an airtight container for characterization.[11]. Show Figure 2. Figure1.A. myrtle plant after wash B. myrtle plant after dryed C. myrtle plant after grinded IHJPAS. 36 (3) 2023 204 Figure 2: A. zinc nano-particles during prepare B. zinc nano-particles after dry 2.4 Determining the activated compounds of myrtle plant extract The gas chromatography-mass spectroscopy technique (GC-Mass), which is cleaner, quicker, and less expensive than conventional extraction methods, was used to identify the activated compounds in the alcoholic myrtle plant extract. GC-Mass is an analytical technique for a qualitative and quantitative group of a broad domain of compounds[12]. Substances found in the myrtle extract by GC-Mass are shown in Figure 3, Table 1. Table 1.Compounds characterized in the myrtle extract by GC-Mass Peak No. R.T Area % Comp. Name Classification 1 25.145 6.60 Benzoic acid Organic acid Soapy compounds 2 25.817 2.14 Benzoic acid Organic acid 3 33.075 0.92 Cyclopentane-1-thione, 2,3,4,4-2-tetramethyl Thiophen compounds 4 34.898 1.22 Tetradecane Aliphatic compounds 5 39.871 1.53 Durohydroquinone Glycol Soapy compounds 6 43.116 4.28 Hexadecane Aliphatic compounds 7 50.336 1.89 Furazan 2-(dimethyl amino methylene amino)- 4-(1,2,4-trizol-2-yl) Triazol 8 50.518 2.62 Hexa decanal, 2-methyl Aliphatic compounds 9 51.770 13.37 Oxirane undecanoic acid, 3-pentyl methyl ester, trans Alcohol 10 53.999 3.30 n-hexadecanoic acid Alcohol 11 54.759 1.13 Epoxy-1- vinylcyclododecene-1,2 Fatty acid methyl esters Soapy compounds 12 56.062 16.52 Methyl (furan-2-yl)-6- hydroxy x-2-ynoate Fatty acid Soapy compounds 13 57.171 5.23 4-(4-chlorophenyl)-2- diethyl amino-2-cyclo buten-1,2-dione Epoxyd compounds Soapy compounds 14 57.451 3.41 Oleic Acid Methyl esters 15 57.654 2.50 1-cyclo hexylnonene Amino acid mrthyl esters Soapy compounds 16 58.731 1.67 (Octadecanoic acid (Z-1) Fatty acid IHJPAS. 36 (3) 2023 205 17 59.709 5.16 Iron, tricarbonyl (2,3,4,5- tetrahydroxy-2,4- cyclopentadien-1-one) Aliphatic compounds 18 60.332 1.48 1,3-cyclopentadiene, 5-(1- methylpropylidene) Fatty acid Soapy compounds 19 60.526 1.26 Octadic-9-enoic acid 20 61.183 1.49 1,3-cyclopentadiene,5- (1-methylpropyldene)- Cyclic compounds Soapy compounds 21 61.606 17.77 Octadic-9-enoic acid Fatty acid methyl esters 22 62.326 6.41 Thiosulfunic acid (H2S2O2), S- (minoethyl) ester 23 62.778 1.83 9-octadecenoic acid, (E)- Fatty acid methyl esters Soapy compounds Figure 3. GC-Mass for the myrtle extract 3. Results and discussion This section describes the results of treating water that has been contaminated with inorganic elements including Cd, Sb, Fe, Cr, and Cu either using myrtle plants or with zinc nanoparticles and evaluates the effectiveness of the treatment. The water treatment technique that was used was the m. processing research. contrasting the standards for standard water adopted by the WHO and treated water. 3.1 Ultraviolet visible (UV-Vis) Ultraviolet-visible spectroscopy is the main part to distinguish active compounds in the myrtle plant by studying the absorptions that are visible in spectra due to the colors of the myrtle plant, which has been screened as an alcoholic extract and zinc nanoparticle with myrtle extract then absorbed peaks inthe first one appear at 307,676nm and in nano292nm this peakrefers to the ultraviolet area belong (n→ σ*), (π→π*) [13]. 307 and 676nm these peaks belong to (n→π*) and (π→π*) in the UV area, 676 nm refers to myrtle plant plus organic and inorganic compounds. When comparing the alcoholic extract to the green myrtle plant and the zinc nanoparticle with the alcoholic extract, alcoholic extract peak shifted towards a shorter longer wavelength 10 nm red shift, and another peak in visible area refers to zinc nanoparticle [14,15], as shown Figure4. IHJPAS. 36 (3) 2023 206 Figure 4. Ultraviolet-Visible for two samples 3.2 Fourier Transform-Infrared (FTIR) Infrared Fourier transform is a key method. When comparing alcoholic extract with myrtle plant and alcoholic extract with nanocomposite, the method for defining organic components in alcoholic extract refers to the creation of nanoparticles. It is employed to identify active chemicals and test whether they can be joined with another element to create new complexes. A peak may be seen at 3371 cm-1, and at 3417 cm-1 zinc nanoparticles can be seen. The (O-H) group has altered in two compounds at around 46 cm-1 in these peaks, which are then followed by further peaks on 2929 cm-1 in alcoholic extract and 2926 cm-1 in zinc nanoparticle. These peaks correspond to the (CH) aliphatic group (1612 cm-1), the carbonyl group (1552 cm-1), the (CH) group (1037 cm-1 in the myrtle alcohol extract), and the (CH) group (1116 cm-1 in nanoparticle) [16,17]show Figure 5,6. Figure 5. FT-IR Spectrum of myrtle alcoholic extract IHJPAS. 36 (3) 2023 207 Figure 6. FT-IR Spectrum of zinc nanoparticle with alcoholic myrtle 3.3.Scanning Electron Microscope (SEM) Scanning Electron Microscope for zinc nanoparticles shows spherical crystal shape in average particles (122.8 nm), which refers to zinc element, this indicates that it has granules size includes a range of nano, this result is consisted [18] Other nanoparticles appear on (55.96, 63.93, 60.66, 85.32,97.20, 100.1, 122.8) nm, which refer to hydrocarbon group range of nano except for hydrogen because the small size of it[19]. Figure7. Show SEM for zinc nanoparticle with alcoholic extract of myrtle 3.4. X-Ray diffraction spectroscopy X-Ray technique was used to identify the arrangement of the crystal atoms, where the X- RAY hit the crystal to show certain directions according to the angles and strength of reflected rays, where 3D images are formed for the Electrondensity inside the crystal. This technique measure the diffraction of X-RAY, the nano-crystals are inserted into the angle meter and transformed while targeting the X-RAY on it, which shall result in random diffraction called measurements. All directions image of angles is taken for 2D dimensions in order to be transformed to 3D images representing the electronic density inside the crystal. In the study of X- RAY diffraction used for identifying the crystal molecular weight,the result of X-ray testing, where IHJPAS. 36 (3) 2023 208 the three readings between were 30-40 due to Zinc elements presence in more readings due to the size of nano-molecule with Zinc elements, while the remaining values show the presence of Hydrocarbon compounds except for the Hydrogen which does not appear because of its small size[20]. show Figure 8. Figure 8. XRD-diffraction of Zinc nanoparticles 3.5 Energy dispersive X-Ray spectroscopy X-ray spectroscopy uses EDX, a form of X-ray emission, to determine the chemical compounds of the samples; on the other hand, each element has a unique atomic structure and set of values. Three peaks in a zinc nanoparticle examined verified it. (1,8.6, 9.8) keV and they were crystal spherical structures[21]. Show Figure 9. Figure 9. Energy-dispersive X-ray spectroscopy for zinc nanoparticle (EDX) 3.6 Transmission electron microscopy (TEM) is the greatest method for figuring out how nanoparticles are shaped. A sample is run through a powerful electron beam in this sort of microscopy, and the outcome of the electrons' interactions with the material is the creation of an image. After that, the image is magnified and focused onto IHJPAS. 36 (3) 2023 209 an imaging medium, such as a charge-coupled device, a fluorescent screen, or a sheet of photographic film[22]. a smaller magnification Because of differences in the material's composition or thickness, contrast can be seen in TEM pictures of that substance, When using a sample of zinc nanoparticles with myrtle extract, high-resolution transmission electron microscopy (HRTEM) revealed that the sample was smooth and spherical on the outside[23]. show Figure 10. Figure 10. Transmission Electron Microscope of zinc nanoparticles (TEM) 4. Treatment of heavy metals The polluted water was identified using a specific ratio of (Ag, Cd, Cr, Sb, Fe, and Pb) 2g to each element. Thereafter, a continuous technique of treatment was used. Ten milliliters of polluted water were added along with two grams of myrtle powder and the same method with zinc nanoparticles. After that, the shaking and mixing process was completed by placing the ingredients onto a magnetic stirrer. A portion of the sample was pulled out after the end flowrate, and the treatment % was calculated. The subsequent myrtle powder percentages are 62%. Comparatively, 72%, 82%, 54%, 64.50%, and 64.80% of the components were found. [24,25]. Show schemes 1,2.Show tables 2,3,4,5. Table (2). Treatment percentages by continuous process by use zinc nanoparticle with extract myrtle plant Metal (ppm) 2gm Before After Percentage 1. Fe 10 3.8 62% 2. Cr 10 2.8 72% 3. Pb 10 1.8 82% 4. Sb 10 4.6 54% 5. Cd 10 3.55 64.50% 6. Cu 10 3.52 64.80% IHJPAS. 36 (3) 2023 210 Table (3). Treatment percentages by continuous process by use zinc nanoparticle with extract myrtle plant 4gm Before After Percentage 1. Fe 10 B.D.L 100% 2. Cr 10 B.D.L 100% 3. Pb 10 B.D.L 100% 4. Sb 10 B.D.L 100% 5. Cd 10 B.D.L 100% 6. Cu 10 B.D.L 100% Figure 11. Using zinc nanoparticle to treatment water from some heavy metals Table 4. Treatment percentages by continuous process by use myrtle powder Metal (ppm) 2 gm Before After Percentage Fe 10 0.38 96.20% Cr 10 1.6 84% Pb 10 B.D.L 100% Sb 10 0.63 93.70% Cd 10 B.D.L 100% Cu 10 0.94 90.60% 0% 20% 40% 60% 80% 100% 120% Fe Cr Pb Sb Cd Cu zinc nano particles 2gm 4gm IHJPAS. 36 (3) 2023 211 Table 5. Treatment percentages by continuous process by use myrtle powder Metal (ppm) 4 gm Before After Percentage 1. Fe 10 0.3 97% 2. Cr 10 0.18 98% 3. Pb 10 B.D.L 100% 4. Sb 10 B.D.L 100% 5. Cd 10 0.18 98% 6. Cu 10 0.26 97% Figure 12. myrtle plant to treatment water from some heavy metals 5. Conclusion By utilizing zinc nanoparticles, which were in turn manufactured using zinc sulfate as a starting material and whose creation was proven by the following methodology, we were able to successfully treat water in this study using ecologically acceptable techniques: SEM, TEM, EDX, FTIR, UV -Visible. Then, we treated the contaminated water due to heavy metals using continuous process by flowrate polluted water with myrtle powder and zinc nanoparticle with extract myrtle plant, We found that myrtle powder waspreferred to zinc nanoparticle. 6. Acknowledgments Department of Chemistry, College of Science for Women, University of Baghdad, Prof. Dr. Abbas Ali Salih Al-Hamdani, and Ministry of Higher Education & Scientific Research & Science and Technology / Directorate of Environment & Water. 75.00% 80.00% 85.00% 90.00% 95.00% 100.00% 105.00% Fe Cr Pb Sb Cd Cu Myrtle powder 2 gm 4 gm IHJPAS. 36 (3) 2023 212 7. Conflicts of Interest - I hereby confirm that all the Figures and Tables in the manuscript are mine. Besides, the Figures and images, which are not mine, have been given the permission for re-publication attached with the manuscript. - Ethical Clearance: The project was approved by the local ethical committee in University of Baghdad. 8. 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