wastewater treatment for plant urea fertilizer using

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Proceedings of the 2nd International Conference on Natural and Environmental Sciences (ICONES) September 9-11, 2014 , Banda Aceh, Indonesia ISSN 2407-2389 129 Wastewater Treatment for Plant Urea Fertilizer Using Fenton Reagent Thanthawi Imam a , Marlina a , Saiful a , Hizir b , Darmadi c a Department of Chemistry, Faculty of Mathematics and Natural Sciences, Syiah Kuala University, Indonesia; b Department of Mathematics, Faculty of Mathematics and Natural Sciences, Syiah Kuala University, Indonesia; c Department of Chemical Engineering, Faculty of Engineering, Syiah Kuala University, Indonesia Abstract. The research on Urea Waste Water Treatment using Fenton Reagent has been done . The results of theanalysis indicate that the initial conditions of waste water urea fertilizer industry has different propertiesto the standards set by the indonesian government (PP.51/MENLH/10/1995) ie BOD and TSS below the standard while COD , NH 3 -N and pH is above the quality standards set by the Indonesian government . Industrial wastewater treatments of urea has been done by advanced oxidation processes (advanced oxidation process) using Fenton reagent, which is a mixture of a solution of hydrogen peroxide (H 2 O 2 ) and ferrous sulfate (Fe 2 SO 4 ) at 222:6 composition (g/L). The optimum processing conditions was achieved in the pH value of 3 and Fenton reagent volumes as much as 10 mL , the percent reduction in COD is 94.56 . Fenton reagent used to degrade and reduce almost all of the impurities present in the urea fertilizer industrial wastewater, industrial wastewater so that it is secure in the waste to the environment as the result of a process that processed small molecules such as N 2 , CO 2 and H 2 O. Keywords: waste water, urea, Fenton, advances oxidation processes and COD. INTRODUCTION Water is an essential component in a urea fertilizer industry, beside natural gas which is the main raw material. PT. Pupuk Iskandar Muda is one of the synthetic urea fertilizer industry in Indonesia. The fertilizer plant requires water in a very large number, amounting to 700-800 tons per hour with a hardness level between 40-100 ppm. This plant utilizes water from Krueng Peusangan in North Aceh as the source of water, and then it processed in the utility unit. Some functions of the water produced in the utility unit are as portable water, process water, and demineralized water for steam boilers. Some factors have contributed to the limitation and pollution of the clean water such as the increase of water production costand suppression by regulatory environment. At this point, the industry sector needs to re-evaluate the management of the wastewater processes for re-usable purposes. Waste water in a fertilizer plant produced from the utility,ammonia and urea units. Wastes derived from the utility, ammonia and urea in the form of anion and cation, condensate containing ammonia and urea as well as the former compressor oil. Waste water is supplied into ponds and sewage treatments, further treatment with stripping system and neutralization using sulfuric acid (H 2 SO 4 ). So that waste water discharges from ponds and sewage treatment is expected having the quality standards set forth in KEP-51/MENLH/10/1995 on waste water quality standard for industrial activities of urea, ie pH 6-9, a maximum of COD 250 ppm , TSS 100 ppm, NH 3 -N 50 ppm, and a maximum of waste discharge 15 m3/ton-produk. Contamination can occur because the water treatment process is not perfect or the equipment do not have maximum performanceeither in or out of the pipe plant. Treatment using sulfuric acid and water stripping not giving optimal results in PT. PIM fertilizer industry. Analysis of urea and Ca-Hardness of waste water at the inlet and outlet KPPL, showed that the wastewater contained in the disposal at high level [17]. The urgency of the reduction of water pollution and waste water from the plant is essential to decrease the level of environmental pollution, so that the water will notcontaminate the ecosystem or even can be reused. One of the treatment process that can reduce environmental pollution is an advanced oxidation process (AOP) using Fenton solution (FeSO 4 /H 2 O 2 ) as a reagent. Fenton reagent is a mixture of hydrogen peroxide compound and the catalyst Fe 2 + (FeSO 4 ), generate hydroxyl radical (•OH) that effectively oxidize organic compounds. Fenton has been developed to treat domestic waste, industrial and raw water, i.e. by taking into account several parameters ,

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Page 1: Wastewater Treatment for Plant Urea Fertilizer Using

Proceedings of the 2nd International Conference on Natural and Environmental Sciences (ICONES)September 9-11, 2014 , Banda Aceh, Indonesia

ISSN 2407-2389

129

Wastewater Treatment for Plant Urea Fertilizer Using Fenton Reagent

Thanthawi Imama, Marlinaa, Saifula, Hizir b, Darmadic

aDepartment of Chemistry, Faculty of Mathematics and Natural Sciences, Syiah Kuala University, Indonesia;bDepartment of Mathematics, Faculty of Mathematics and Natural Sciences, Syiah Kuala University,

Indonesia; cDepartment of Chemical Engineering, Faculty of Engineering, Syiah Kuala University, Indonesia

Abstract. The research on Urea Waste Water Treatment using Fenton Reagent has been done . The results of theanalysisindicate that the initial conditions of waste water urea fertilizer industry has different propertiesto the standards set by theindonesian government (PP.51/MENLH/10/1995) ie BOD and TSS below the standard while COD , NH3-N and pH is above thequality standards set by the Indonesian government . Industrial wastewater treatments of urea has been done by advancedoxidation processes (advanced oxidation process) using Fenton reagent, which is a mixture of a solution of hydrogen peroxide(H2O2) and ferrous sulfate (Fe2SO4) at 222:6 composition (g/L). The optimum processing conditions was achieved in the pH valueof 3 and Fenton reagent volumes as much as 10 mL , the percent reduction in COD is 94.56 . Fenton reagent used to degradeand reduce almost all of the impurities present in the urea fertilizer industrial wastewater, industrial wastewater so that it issecure in the waste to the environment as the result of a process that processed small molecules such as N2 , CO2 and H2O.

Keywords: waste water, urea, Fenton, advances oxidation processes and COD.

INTRODUCTION

Water is an essential component in a urea fertilizer industry, beside natural gas which is the main raw material. PT.Pupuk Iskandar Muda is one of the synthetic urea fertilizer industry in Indonesia. The fertilizer plant requires waterin a very large number, amounting to 700-800 tons per hour with a hardness level between 40-100 ppm. This plantutilizes water from Krueng Peusangan in North Aceh as the source of water, and then it processed in the utilityunit. Some functions of the water produced in the utility unit are as portable water, process water, anddemineralized water for steam boilers. Some factors have contributed to the limitation and pollution of the cleanwater such as the increase of water production costand suppression by regulatory environment. At this point, theindustry sector needs to re-evaluate the management of the wastewater processes for re-usable purposes.

Waste water in a fertilizer plant produced from the utility,ammonia and urea units. Wastes derived from theutility, ammonia and urea in the form of anion and cation, condensate containing ammonia and urea as well as theformer compressor oil. Waste water is supplied into ponds and sewage treatments, further treatment withstripping system and neutralization using sulfuric acid (H2SO4). So that waste water discharges from ponds andsewage treatment is expected having the quality standards set forth in KEP-51/MENLH/10/1995 on waste waterquality standard for industrial activities of urea, ie pH 6-9, a maximum of COD 250 ppm , TSS 100 ppm, NH3-N 50ppm, and a maximum of waste discharge 15 m3/ton-produk.

Contamination can occur because the water treatment process is not perfect or the equipment do not havemaximum performanceeither in or out of the pipe plant. Treatment using sulfuric acid and water stripping notgiving optimal results in PT. PIM fertilizer industry. Analysis of urea and Ca-Hardness of waste water at the inletand outlet KPPL, showed that the wastewater contained in the disposal at high level [17]. The urgency of thereduction of water pollution and waste water from the plant is essential to decrease the level of environmentalpollution, so that the water will notcontaminate the ecosystem or even can be reused.

One of the treatment process that can reduce environmental pollution is an advanced oxidation process (AOP)using Fenton solution (FeSO4/H2O2) as a reagent. Fenton reagent is a mixture of hydrogen peroxide compound andthe catalyst Fe2

+(FeSO4), generate hydroxyl radical (•OH) that effectively oxidize organic compounds. Fenton hasbeen developed to treat domestic waste, industrial and raw water, i.e. by taking into account several parameters ,

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Proceedings of the 2nd International Conference on Natural and Environmental Sciences (ICONES)September 9-11, 2014 , Banda Aceh, Indonesia

ISSN 2407-2389

130

such as Biological Oxygen Demand / Chemical Oxygen Demand (BOD/COD), Total Suspended Solid ( TSS ), color,nitrogen, phosphorus and some metals contained in water. Utilization Fenton in laboratory able to reduce COD by92.3 % with the composition ratio of Fe2

+ : H2O2 is 1 : 4.5 at pH 4 (Benatti et al., 2005) . Using of Fenton reagent fortreatment of industrial waste in India can reduce COD up to 95 %, with the composition Fenton 222 g/LH2O2/FeSO4 6 g/L and pH 3 . Therefore, this study was conducted in wastewater treatment of urea fertilizer plantsusing variation of Fenton reagent volume and pH, and its effect on the COD number. Determination of COD donewith effective conventional methods are bichromate methods of using the compounds ferrous ammonium sulfate(FAS) as titrant (Mandal et al., 2010). This method can be used for the reduction of urea fertilizer waste water anddoesn't cause environmental pollution, both air and water pollution. Expected, the treated waste water reusableto save on the cost of water treatment from primary sources.

METHODS

This research has been done in the laboratory of Chemistry Department of Mathematics and Natural Sciences ofSyiah Kuala University, Banda Aceh, starting from April to June 2013. Samples in the form of fertilizer plantwastewater of PT. Pupuk IskandarMuda, Lhokseumawe, i.e the wastewater in the unit inlet KPPLs. The tools usedin this study are glassware, analytical balance, pH meter, a set of tools reflux, DO meter and turbidymeter. Thematerials used in this research was H2SO4, FeSO4, H2O2 30%, a standard solution of dichromate 0.25 N, silversulphate (Ag2SO4), a standard solution of ferrous ammonium sulfate (FAS) 0.1 N, fenantrolin ferrous sulfate(ferroin), mercury sulfate (HgSO4), NaOH, phenantroline monohydrate, and distilled water. The sample took atsecond week in April,2013, from urea fertilizer plant PT. Pupuk Iskandar Muda, Lhokseumawe. The sample wastaken at 3 points in the unit inlet KPPLs (before processed and discharged into a body of water) and then mixed ina place.

Initial Characterization of Urea Liquid Waste. Characterization of physical and chemical properties of waste waterfrom PT. PIM has done according to existing standard methods (Clesseri et al., 1998).

Waste TreatmentPreparation of Fenton Reagent. Six grams of FeSO4 dissolved into 1 liter of distilled water and 222 grams of H2O2

also dissolved into 1 liter of water. Then both mixed (Mandal et al., 2010).

AOP (Advanced Oxidation Process). Sample as much as 100mL inserted into a 250 mL flask and the pH hasadjusted using H2SO4 as needed. Then fenton reagent was added (6 g/L FeSO4 H2O2 222g / L), and stirredcontinuously and maintained up to 30 minutes. The resulting supernatant was added to the flask and the pH wasraised up to 7 with NaOH. Furthermore, the supernatant was analyzed (Mandal et al., 2010).

TABLE 1. Composition of Fenton Reagen

Concentration (H2O2 : FeSO4) pH Fenton Volume

222 : 6 (gram/liter)

2

10 mL3

4

5

Final Waste Characterization. The finalcharacterization of the waste has done on samples at optimum conditions,ie pH and volume on the right. Characterization includes BOD, COD, TSS, NH3-N, and pH. The analysis wasperformed as Initial Characterization of Urea Fertilizer Waste Water2.

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RESULT AND DISCUSSION

Initial characterization of waste. The initial condition of the urea plant wastewater is characterized to determinethe nature of the wastewater and the efficiency of wastewater treatments by using fenton solution. Wastewater istaken before treatment processing in landfills. This waste is a mixture of all the waste in the production process,which is derived from the cooling tower, demineral unit, urea plant and ammonia plant flowed through the sewerto the storage. The results of wastewater characterization of PT PIM can be seen in table 3.1 below :

TABEL (2). Initial conditions of urea industrial wastewater

Based on the table above, we see that the parameters BOD and TSS has a value below the standards set, while thevalue of COD, NH3-N concentration and pH above the allowed threshold. Results of analysis of BOD analysisshowed values below the allowed standard, ie 74.3 ppm. This value indicates the amount of oxygen demand byliving organisms in the waste water for the destruction of organic matter (C, H, O, N, S, and P), at a specified timeand temperature at 20 0C analysis shows BOD value is still in the allowable range, means the number ofmicroorganisms in the urea fertilizer industry wastewater is unobtrusive production process and environment ifthe waste is disposed. The number of microorganisms in the water a lot of the process can lead to corrosion thusmaking the process inefficient, whereas in the environment can cause disruption of the ecosystem due to lack ofoxygen.

COD is an important parameter in determining the characteristics of the waste, which indicates the chemicals,both organic and inorganic, in the waste water. The analysis showed that the COD value of the effluent urea abovethe quality standards set, ie. 332 ppm. The COD value is associated with TSS parameter, which indicates theamount of the suspended solids of 24.4 ppm and NH3-N is the levels of urea in wastewater at 97.2 ppm. Based onthe results of this analysis can be concluded that the COD value is strongly influenced by organic chemicals, ureawhich is the main product of this industry. Highlevels of urea indicate that the urea production process was notgoing well. Wastewater pH value is determined by thecontent of the materials in the waste water.

Waste Treatment. Waste treatment is intended to remove pollutants or impurities contained in waste water, sothe water is released into the environment safe. Waste water treatment of urea plant PT PIM has been done withthe AOP (advanced oxidation), that is by using Fenton solution as a reagent. Advanced oxidation processes haveproven successful doing in several types of wastewater treatment, for example in destruction of organic pollutantssuch as color [8]. The main drawback of this is Fenton treatment on large concentrations of H2O2 and FeSO4 wereused during the treatment process, which the ratio of H2O2 /Fe2+ is the key to efficiency in the Fenton treatmentprocess. Therefore, in this study the optimal ratio between H2O2 / Fe2 + obtained by8 maintained to achievemaximum degradation efficiency of urea fertilizer plant waste water. Several factors affect the processing ofFenton, are:

Effect of pH. Effect of pH on the chemical reaction system is very important, because the pH plays a role in theproduction of OH [10,11,164]. In this research, the wastewater is treated with Fenton reagent at different pH, from

ParametersResult Maximum value

BOD 74,3 ppm 100 ppm

COD 332ppm 250 ppm

TSS 24,4 ppm 100 ppm

NH3-N 97,2 ppm 50 ppm

pH 10,13 6,0- 9,0

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2-5, while the other experimental conditions kept constant. Figure 1.shows the degradation pattern of the ureaplant wastewater at different pH from 2 to 5. The optimum pH value is 3, which the optimum reduction in CODreached 94.56%. This value resembles the resulting value on the degradation of some mixture of industrial waste[8]. Figure one shows that at pH level above 3 the degradation process is decreased gradually, which is indicatedby a small percent reduction in COD. This is likely due to an increase in the formation of hydroxyl radicals (OH *),then the formation of the iron complex hidokso {Fe (HO)4} at higher pH (Oller, 2011). The results also showed thatat a pH below 3 degradation of waste is also reduced. This may be caused by the formation of complexes{Fe(HO)6}2+ which reacts more slowly with peroxide compared to the {Fe (HO) (H2O)5}2 +. Thus, a pH of 3 isconsidered as the optimum pH and selected for further research condition.

FIGURE 1. Effect of pH on reduction of COD of water treatment in urea plant

Visually result of urea wastewater treatment using Fenton reagent at various pH of the solution can be seen inFigure 2. In this figure, it is clear that the waste is treated with a Fenton solution with a pH of 3 clearer than thewaste solution with a pH above and below 3, which still has a brownish yellow and sediment.

FIGURE 2. Reagent Fenton reaction with wastewater

Fenton reaction mechanism between the solution with liquid waste such as urea is estimated at equation 1.to5.thefollowing:

Fe2+ + H2O2 Fe3+ + ·OH + OH .......... 1Fe3+ + H2O2 Fe2++ ·O2- + 2H+ .......... 2Fe3+ + ·O2- Fe2+ + O2(g) + 2H+ .......... 3·OH + CO (NH2)2 N2 + CO2 + 2H2O .......... 4·OH + H2O2 ·HO2 + H2O . .......... 5

From equation 4. it can be seen that the end result is the small molecules that are safe for the water, and can bedischarged into the water because it is notwill disrupt the ecosystem. Other results obtained during the process of

82,1194,56

64,68

57,63

0

20

40

60

80

100

2 3 4 5

% P

enur

unan

CO

D

pH

pH2 pH3 pH 4 pH 5 pH neutral

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ISSN 2407-2389

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wastewater treatment plant fertilizer use is the pH affects the Fenton reaction temperature increase, which in turnwill affect the rate of reaction. Figure 3.2 shows the effect of temperature and pH on the reaction rate. From theseresults it can be concluded that the reaction is exothermic because it produces heat and lasts a long time, which isabout 2 to 3 hours. The temperature rise is directly proportional to the rate of reaction invitation OH * formationresults from H2O2 and FeSO4 (equation 3. 1). The rate of reaction between H2O2 and FeSO4 more slowly belowpH 3 and above, which have an impact on the overall COD reduction.

FIGURE 3. Effect of pH on Thermal and rate of Reaction

Effect of reagents amount. The amount of reagents or materials used in a chemical reaction will determine theoutcome of the reaction. In this study the amount of Fenton reagent used varies from 6-10 mL, with a pH value of3 that the optimum pH. Figure 3.2 shows the effect of the amount (volume) of the Fenton reagent in CODreduction percent, where the highest decrease occurred in Fenton volume of 10 mL, which is 94.56%. The analysisshowed that the value of COD from 6 mL of Fenton reagent differs only slightly from the initial of COD, so the useof Fenton reagent under 6 mL was not done because it is not efficient. Similarly, for the amount of Fenton reagentabove 10 mL was discontinued for economic reasons, where the use of 10 mL of Fenton's enough to lower allwastewater parameters.

FIGURE 4. Effect of Fenton Reagent volume to percent reduction of COD

Characterization of Final Waste. The final condition industrial wastewater urea after Fenton treatment werecharacterized to determine the nature of the waste and the efficiency of wastewater treatment processes. Analysisof the waste is taken to the optimum processing conditions, ie pH at 3 and 10 mL volume of Fenton. The results ofthe final wastewater characterization PT PIM can be seen in table 2 below:

TABLE 3. Final Characteristic of urea waste water

Parameter Result % of Reduction

BOD 5,6 ppm 92,5

COD 18,13 ppm 96,37

0

50

100

Proceedings of the 2nd International Conference on Natural and Environmental Sciences (ICONES)September 9-11, 2014 , Banda Aceh, Indonesia

ISSN 2407-2389

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wastewater treatment plant fertilizer use is the pH affects the Fenton reaction temperature increase, which in turnwill affect the rate of reaction. Figure 3.2 shows the effect of temperature and pH on the reaction rate. From theseresults it can be concluded that the reaction is exothermic because it produces heat and lasts a long time, which isabout 2 to 3 hours. The temperature rise is directly proportional to the rate of reaction invitation OH * formationresults from H2O2 and FeSO4 (equation 3. 1). The rate of reaction between H2O2 and FeSO4 more slowly belowpH 3 and above, which have an impact on the overall COD reduction.

FIGURE 3. Effect of pH on Thermal and rate of Reaction

Effect of reagents amount. The amount of reagents or materials used in a chemical reaction will determine theoutcome of the reaction. In this study the amount of Fenton reagent used varies from 6-10 mL, with a pH value of3 that the optimum pH. Figure 3.2 shows the effect of the amount (volume) of the Fenton reagent in CODreduction percent, where the highest decrease occurred in Fenton volume of 10 mL, which is 94.56%. The analysisshowed that the value of COD from 6 mL of Fenton reagent differs only slightly from the initial of COD, so the useof Fenton reagent under 6 mL was not done because it is not efficient. Similarly, for the amount of Fenton reagentabove 10 mL was discontinued for economic reasons, where the use of 10 mL of Fenton's enough to lower allwastewater parameters.

FIGURE 4. Effect of Fenton Reagent volume to percent reduction of COD

Characterization of Final Waste. The final condition industrial wastewater urea after Fenton treatment werecharacterized to determine the nature of the waste and the efficiency of wastewater treatment processes. Analysisof the waste is taken to the optimum processing conditions, ie pH at 3 and 10 mL volume of Fenton. The results ofthe final wastewater characterization PT PIM can be seen in table 2 below:

TABLE 3. Final Characteristic of urea waste water

Parameter Result % of Reduction

BOD 5,6 ppm 92,5

COD 18,13 ppm 96,37

8,1326,74

94,56

0

50

100

6 8 10

Proceedings of the 2nd International Conference on Natural and Environmental Sciences (ICONES)September 9-11, 2014 , Banda Aceh, Indonesia

ISSN 2407-2389

133

wastewater treatment plant fertilizer use is the pH affects the Fenton reaction temperature increase, which in turnwill affect the rate of reaction. Figure 3.2 shows the effect of temperature and pH on the reaction rate. From theseresults it can be concluded that the reaction is exothermic because it produces heat and lasts a long time, which isabout 2 to 3 hours. The temperature rise is directly proportional to the rate of reaction invitation OH * formationresults from H2O2 and FeSO4 (equation 3. 1). The rate of reaction between H2O2 and FeSO4 more slowly belowpH 3 and above, which have an impact on the overall COD reduction.

FIGURE 3. Effect of pH on Thermal and rate of Reaction

Effect of reagents amount. The amount of reagents or materials used in a chemical reaction will determine theoutcome of the reaction. In this study the amount of Fenton reagent used varies from 6-10 mL, with a pH value of3 that the optimum pH. Figure 3.2 shows the effect of the amount (volume) of the Fenton reagent in CODreduction percent, where the highest decrease occurred in Fenton volume of 10 mL, which is 94.56%. The analysisshowed that the value of COD from 6 mL of Fenton reagent differs only slightly from the initial of COD, so the useof Fenton reagent under 6 mL was not done because it is not efficient. Similarly, for the amount of Fenton reagentabove 10 mL was discontinued for economic reasons, where the use of 10 mL of Fenton's enough to lower allwastewater parameters.

FIGURE 4. Effect of Fenton Reagent volume to percent reduction of COD

Characterization of Final Waste. The final condition industrial wastewater urea after Fenton treatment werecharacterized to determine the nature of the waste and the efficiency of wastewater treatment processes. Analysisof the waste is taken to the optimum processing conditions, ie pH at 3 and 10 mL volume of Fenton. The results ofthe final wastewater characterization PT PIM can be seen in table 2 below:

TABLE 3. Final Characteristic of urea waste water

Parameter Result % of Reduction

BOD 5,6 ppm 92,5

COD 18,13 ppm 96,37

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TSS 4,83 ppm 80,2

NH3-N 12,5 ppm 87,13

pH 3 50-33,3

From the table it can be seen that nearly all the parameters (except pH) are required for the fertilizer industrywastewater discharges have been under the range set by the government (PP 51, 1995). Based on the analysisresults, we can conclude that the AOP process uses highly efficient Fenton reagent used for industrial wastewatertreatment urea, in which the percent efficient process reaches above 80, except the pH value. Thus, urea fertilizerplant wastewater that has been processed safely discharged into the environment, or may be reused as processwater after the pH of pH adjusted by using Chemical that do not damage the environment again

CONCLUSION

1. Urea fertilizer industry wastewater PT. IskandarMuda fertilizer has the properties below the standards set by thegovernment, namely PP 51 / MENLH / 10/1995.

2. Advanced oxidation process (AOP) uses the Fenton reagent can be applied to urea industrial wastewatertreatments.

3. The treatmentproccess with Fenton reagent reached the optimum conditions achieved at pH values 3 and theamount of total volume 10 mL, with a COD reduction of 94.56 %

4. Fenton Reagents amount can reduce almost all the impurities present in the urea industry wastewater,industrial

waste water so that it is secure in the exhaust into the environment.

REFERENCES

1. Alaerts dan Sumestri Sri.(1987), Metoda Penelitian Air. Usaha Nasional, Surabaya.2. Clesceri L. S., Arnold E.G and Andrew D. E (1998), Standard Method for The Examination of Water and Wastewater, 20

th Edition, APHA – AWWA – WEF, United Stated of America.3. Douglas, A. S., and Donald, M. W. (1980).Principles of Instrumental Analysis 2nd Edition. Holt-Saunders Japan, Ltd.

Tokyo, Jepang.4. Guedes, A. M.F.M., Madeiraa, L.M.P., Boaventuraa, R. A.R., Costa, C.A.V.(2003). Fenton Oxidation of Cork Cooking

Wastewater-Overall Kinetic Analysis. WaterResearch.37 : 3061–3069.5. Huling, S., Arnold, R., Sierka, R., Jones, P., and Fine, D. (2000), Contaminant Adsorption and Oxidation Via Fenton

Reaction. J.Environ. Eng. 126 (7) : 595-600.6. Kayaalp N., et al., (2010). A New Approach for Chemical Oxygen Demand (COD) Measurement at High Salinity and Lor

Organic Matter Samples. Environ SciPollut Res, 17: 1547-1552.7. LaGrega M. D et al., (2001), Hazardous Waste Management 2nd Edition, McGraw-Hill International Edition, Singapore.8. Mandal, T. (2010), Advanced Oxidation Process and Biotreatment: Their Roles in Combined Industrial Wastewater

Treatment. Desalination, 250: 87-94.9. Marlina, Darmadi dan Hizir. 2012. Penanggulangan dan Pemanfaatan LimbahCair PT. Pupuk Iskandar Muda. Laporan

Penelitian. FMIPA Unsyiah. Banda Aceh.10. Mert, K. (2010), Pre-treatment Studies on Olive Oil Millffluent using Physicochemical, Fenton and Fenton-like

Oxidations Processes, Journal of Hazardous Materials, 174: 122-128.11. Oller, I. (2011), Combination of Advanced Oxidation Processes and Biological Treatments for Wastewater

Decontamination. Science of Total Environmental, 409: 4141-4186.12. Othmer, K. (1992), Encyclopedia of Chemical Technology 5th ed, Interscience, Encylopedia Inc., New York.13. Pemerintah RI. (1997), Pengelolaan Lingkungan Hidup, Undang-Undang Republik Indonesia Nomor 23 Tahun 1997.14. Raymakers E. Steve (2001), 1 st International Ballast Water Treatment, R & D Symposium, http:/www. globallast.

Imo.org/15. Shiying. (2009), A Novel Advanced Oxidation Process to Degrade Organic Pollutants in Wastewater: Microwave-

activated Persulfate Oxidation. Journal of Enviromental Sciences, 100: 1175-1180.16. Shukla. (2010), Activated Carbon Supported Cobalt Catalysts for Advanced Oxidation of Organic Contaminants in

Aqueous Solution.Applied Catalyst B.Enviromental, 100: 529-524.

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17. Thanthawi, I. (2012), Laporan Kuliah Kerja Praktek Efektivitas KPPL Terhadap Penurunan pH dan Kadar Urea dalam AirLimbah dan Pengaruhnya Terhadap Kadar CaCO3 dalam Air Limbah PT. PIM, Unsyiah, Indonesia.

18. Zhu Y. et al., (2005), Multyelement Determination of Trace Metals in River Water (Certified Reference Material, JSAC0301 – 1) by High Efficiency Nebulization ICP after 100-fold Preconcentration with a Chelating Resin-PackedMinicolumn, Analytical Sciences, Volume 21, 199 – 203.

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Implementation of Geoportal Server for Disseminating and Sharing HugeGeographic Information Generated in 2004 Tsunami Recovery Process for Aceh

Province, Indonesia Nizamuddina and Ardiansyahb

aInformatics Department, bElectrical Engineering Department, Syiah Kuala University, Banda Aceh, Indonesia

Abstract. The proprietary and open source Geographical Information System (GIS) technologies including desktop GIS,server GIS and geographic database have significantly grown along with the rapid development of computer andinternet technologies. In this paper, we proposed free and open source Geoportal Server for disseminating and sharinghuge geographic information produced during Rehabilitation and Reconstruction (RR) process available at AcehGeospatial Data Center (AGDC). In addition to easily sharing the huge geographic information, we integrated GeoportalServer with server GIS, geographic database and desktop GIS. The RR process (April 2005 to March 2009) following the2004 Earthquake and Tsunami has successfully built-back the better Aceh province, Indonesia. During the RR phase, GIShave turned out to be necessary and useful, and played an important role in many sectors e.g. humanitarian,infrastructure, transportation, social and economic, etc. A huge amount and variety of geographic information havebeen compiled and produced with a large budget from international and national agencies to support the RR-process.After RR-process, the geographic information, including many map documents or project, and GIS applications havebeen handed over to AGDC established in 2006 whose one of the task was to facilitate the transfer of all geographicinformation and GIS applications to Aceh government from Bureau, international and national agencies/NGOs thatworked in Aceh. This valuable and important geographic information generated in the RR-process will be useful forusers/decision-makers for the study or for the future sustainable development of Aceh province. AGDC and Acehprovince have faced a serious problem in disseminating and sharing the huge geographic information. Therefore, weproposed this system.

Keywords: Tsunami recovery, Rehabilitation and Reconstruction process, GIS, Geoportal Server, Aceh-Indonesia.

INTRODUCTION

Rehabilitation and Reconstruction BureauOn April 15th, 2005, the Indonesian government declared the establishment of National Bureau for theRehabilitation and Reconstruction (BRR) for Aceh-Nias. Its main tasks were formulating strategies, preparingbudgets, developing the detailed plans and coordinating, controlling, and monitoring the RR activities in Aceh-Nias[1]. One hundred thirty-three countries have provided assistance to the humanitarian mission [2], committingabout 6.72 billion USD3. At the end of the four-year RR process of Aceh - Nias, around 500 agencies haveimplemented 2.200 projects [1]. These projects included the building of 140.300 permanent houses, 1.759 schools,1.115 health facilities, 996 government buildings and 363 bridges. Construction of around 2.696 kilometers ofroad, 23 ports, and 13 airports or airstrips has also been completed [3,4].

Aceh Geospatial Data Center in Aceh ProvinceMany GIS centers had involved in RR process in Aceh such as Indonesia National Agency for Survey and Mapping(BAKOSURTANAL, The United Nations Information Management System (UNIMS), BRR-Spatial Information andMapping Centre (SIM-C), BRR - Geospatial Task Force (GTF) center and Aceh Geospatial Data Center (AGDC). AcehGeospatial Data Center (AGDC) was established by BRR, SIM-C, GTF and other agencies at the Aceh DevelopmentBoard Office (BAPPEDA).

The objectives after the RR process was finished was that AGDC would be a center that handle the transfer processof geographic information and GIS applications from BRR and other agencies to the Aceh government [5]. Themain tasks are to (a) provide access to spatial data and information easily and quickly, (b) encourage the utilizationand the integration of data and information to support the decision-making systems, and (c) improve theunderstanding about the use of data of geospatial information [6].

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Geographic Information in Aceh ProvinceIn 2004, the only available and consistent digital base maps that could be used for the beginning emergency phasewere the Topographic Line Maps (TLM) at scale 1:50,000 and 1:250.000 produced in the 1970s by BAKOSURTNAL7.In July 2005, the NORAD (The Norwegian Agency for International Development) has funded a geospatial dataproject to support the acquisition of high-resolution aerial photography over the Aceh province [8]. The projectwas undertaken by BLOM (Norwegian Geographical Information Company) and BAKOSURTAL. It produced highresolution Orthophoto Imagery, Digital Elevation Model (DEM) and TLMs in tsunami-affected areas [7]. Thisgeospatial data has been widely utilized by many agencies in their RR activities. During the RR activities, due to thepartial lack of availability of geospatial data in some areas, BRR and other agencies, which utilized GIS in theirprojects, sometimes had to carry out individual mapping to generate and compile relevant geospatial data.

Several large amounts of geographic information projects were active over the course of the 4 years RR programsuch asBAKOSURTANAL’s Topographic line map, NORAD- BLOM - BAKOSURTANAL’s Aerial imagery andTopographic Line Map, JICA - study team in Aceh province’s Topographic line map and ARRIS thematic map,World Bank - BPN RALAS program’s Land parcel maps, LAPAN supported by EUROSAT/UN disaster chapter’sSPOT5, LANDSAT 7, ASTER and IKONOS, BGR’s Airborne electromagnetic map and ground water map, AusAID-BAKOSURTANAL’s IFSAR DEM (Digital Elevation Model), BRR’s Barrack geodatabase, BRR’s Housing geodatabase,AusAID-GTZ AMAP’s Asset mapping spatial data and UNDP-BRR Technical Team’s Asset geodatabase [9]. SIM-Crecorded a significant geographic information distribution from 2006 to 2008 at BRR, including around 2,773 hardcopy maps, 706 digital copies of spatial data and 90 aerial imageries requested by users. SIM-C has produced inexcess of 9,000 maps and other information [10]. [11] reported that they discovered 30,000 ESRI shapefiles,received from many agencies, when they did a quick data audit of the SIM-C’s data server.

The GIS applications implemented at BRR during RR-processIn 2004, the only available and consistent digital base maps that could be used for the beginning emergency phasewere the Topographic Line Maps (TLM) at scale 1:50.000 and 1:250.000 produced in the 1970s by BAKOSURTNAL[7]. In July 2005, the NORAD (The Norwegian Agency for International Development) has funded a geospatial dataproject to support the acquisition of high-resolution aerial photography over the Aceh province [8]. The projectwas undertaken by BLOM (Norwegian Geographical Information Company) and BAKOSURTAL. It produced highresolution Orthophoto Imagery, Digital Elevation Model (DEM) and TLMs in tsunami-affected areas [7]. Thisgeospatial data has been widely utilized by many agencies in their RR activities. During the RR activities, due to thepartial lack of availability of geospatial data in some areas, BRR and other agencies, which utilized GIS in theirprojects, sometimes had to carry out individual mapping to generate and compile relevant geospatial data.

RELATED WORK

Several applications had been implemented during RR-process [8] and are being used at ADGC [6] and previousstudy about prototype of an integrated information system [9] has been proposed to AGDC. The implementedapplications used during rehabilitation and reconstruction process were to satisfy each group of user and specificpurposes during RR-process and they were not designed to easily handle huge amount of geographic information.Several disadvantages of existing applications [6] being used by AGDC have been investigated in detail and clearlyexplained in the previous study [9]. Several advantages of a prototype of an integrated information system, thatincluded the implementation of the ArcIMS Metadata Explorer for disseminating and sharing Geographicinformation, have also been explained in the previous study [9]. The main advantages of previous study [9] includethe effectiveness and efficiency of work process for AGDC to manage geodatabase, publish map services includingArcIMS Feature, Image, ArcMap Image services and ArcGIS Server map service as well as easily develop the customWeb mapping Application. AGDC has evaluated several advantages of the prototype of an integrated informationsystem and concluded that the system suitable to be implemented in Aceh [9]. However, AGDC also stated anobstacle of the information system during their evaluation, this obstacle is the high cost of purchasing the ESRIserver products including both ArcIMS and ArcGIS Server. On the basis of several problems of existing application,an obstacle in the previous study [9]and the issues relating to the huge geographic information including a lot ofArcMap documents, the GIS users in Aceh province as well as the emergence of the latest FOSS ESRI Geoportal

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Server [12]. Therefore, these motivated us to implement an effective and efficient method for disseminating andsharing geographic information produced during RR-process using ESRI Geoportal Server integrated/combinedwith other ESRI products version 10 such as ArcGIS Server, ArcSDEGeodatabase connection for PostgreSQL8.4.7/PostGIS 1.4.2 and ArcGIS Desktop.

SYSTEM OUTLINE

In this section, we will describe software components that are used as the data layer, server layar and applicationlayer inthe system.

(1) Data layer:(a) Geospatial data,(b) ArcSDEGeodatabase,(c) PostgreSQL/PostGIS spatial database,

(2) Server layer:(a) ESRI Geoportal Server(b) ArcGIS Server and their services,

(3) Application layer:(a) GIS Desktop software:

(i) ArcGIS Desktop 10,(ii) ArcExplorer,(iii) QuantumGIS (QGIS),etc,

(b) Web applications:(i) ESRI Geoportal Server Application(ii) ArcGIS Server 10 Manager,(iii) ArcGIS Server 10 REST API

SYSTEM FUNCTIONALITIES AND FACILITIES

System facilities for AGDC StaffCreate and publish ArcGIS Server ServicesArcGIS Desktop 10 or ArcGIS Server Manager 10 is used to publish ArcGIS Server Map Service and manage thepublished ArcGIS Server Map Services. ArcMap from version 9.3.1 has the Map Service Publishing toolbar, which isused to (a) analyze and preview map before publishing the ArcGIS Server Map Service, (b) directly publish MapServices from ArcMap and (c) create a MSD file. ArcGIS Server Manager 10 or ArcCatalog 10 uses the MSD file as aninput to publish high performance ArcGIS Server Map Services [13,14]. ArcGIS Server Manager or ArcCatalog 10also uses a MXD file to publish ArcGIS Server Map Service [13]. In our system, REST URLs of ArcGIS Server MapService is utilized to provide online linkage in the metadata document (Identification | Citation | General) or bothREST and SOAP URLs of ArcGIS Server Map Services is used to directly register a resource using “Register resourceon the network [15]” in the ESRI Geoportal Server application.

Create metadata documents and resources descriptionWe use ArcCatalog for creating metadata document and use both the ArcGIS server manager and the ArcMapDocument Properties in ArcMap for creating the description of the resources. The metadata document must becreated before resources can be published to Geoportal Server Metadata Service using “Geoportal Server Publishclient [15]” in ArcCatalog. The description or information relating to of the resources is needed when one directlyregisters a resource through the “Register a resource on the network[15].”

Publishing resourcesWe use either the “Geoportal Publish Client [15]”, an extension for the ArcCatalog or the Add page ofAdministration Tab in ESRI Geoportal Server application for publishing the resources. The three methods are asfollow:

a. Register a resource on the network,

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There are seven main categories of protocol types in the Registered Resource, i.e. URL, ArcGIS, Esri MS,OAI, WAF,CSW, THREDDS. Since the main map services in this system are ArcGIS Server Services, we prefer to use TheRegister Resource, select The ArcGIS protocol type and register the REST and SOAP URL of ArcGIS Server Servicesinto Geoportal Server Metadata Service [15,16].

b. Upload or validate metadata file from the local disk, andc. Use dedicated editor to create metadata manually

System facilities for decision maker and end-usersThe system allows local government decision-makers and end users to find geographic information by searchingand browsing through the contents of ESRI Geoportal Server Metadata Service using either ArcMap or ESRIGeoportal Server application. Users can directly bring/open the geographic information services found in the ESRIGeoportal Server Metadata Service into their ArcMap [16].

Finding geographic information resources using ESRI Geoportal Server applicationESRI Geoportal Server application is used to search and browse content of Geoportal Server Metadata Servicethrough a Web browser [16]. After finding the geographic information in ESRI Geoportal Server application, userscan directly bring/open an ArcGIS Server Map Services by firstly opening ArcGIS Services Directory relating thepublished ArcGIS Map service and then by clicking View in: “ArcMap” link

RESULT

This section shows the Geoportal web application produced by the system that is used as user interface foradministrator and user. The Geoportal user interface shows the list of geographic information already publishedand registered to our system.

FIGURE 4.1.ArcGIS Services Directory relating the published ArcGIS Map service9

DISCUSSION AND CONCLUSION

ESRI Geoportal Server was latest server product technology form ESRI. Since first generation of ESRI GeoportalServer open source 1.0, it does not need ArcGIS Server and/or ArcSDE license or ArcGIS server and/or ArcSDE that

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is installed on the same machine to develop the ESRI Geoportal Server application. It can use the offline geographicinformation resources or other online resource of Map Services, such as ArcGIS Online services resources, toprovide online resource in metadata element for sharing geographic information [12,16]. However, to share hugeorganization’s geographic information, ESRI Geoportal Server must be integrated with ArcGIS server and/orArcSDE. This integration will allow administrator to easily publish and manage ArcGIS Server Service such as Mapservice, Feature service, OCG standard-WMS/WFS. This integration also will also allow users or decision makers toeasily search geographic Information through ESRI Geoportal Server application and directly bring/open the ArcGISserver map services of geographic information found at ESRI Geoportal Server application to their ArcGIS desktop.Therefore, ESRI Geoportal Server open source has been implemented along with ArcGIS Server and ArcSDE todisseminate and share huge geographic information available at the AGDC.

REFERENCES

1. BRR,“Building a Land of Hope: One Year Report Executing Agency of the Rehabilitation and Reconstruction Agency forAceh and Nias April 2006”, Banda Aceh, BRR-NAD-Nias, 2006.

2. Masyaraf, Harry and McKeon, Jock MJA,“Post-Tsunami Aid Effectiveness in Aceh: Proliferation and Coordination inReconstruction”,Wolfhen Center for Development Working Paper, No.6, Washinton DC,2008.http://www.brookings.edu/~/media/Files/rc/papers/2008/11_aceh_aid_masyrafah/11_aceh_aid_masyrafah.pdf(accessed 2012-2-2),

3. Agusta, Margaret (ed.), Surbakti, Amin and Ul-Aflaha, Aichida,“BRR Book Series,Finance: The Seven Keys to Effective AidManagement(ISBN 978-602-8199-48-3)”,Banda Aceh, BRR NAD-NIAS and UNDP, 2009.

4. Darajat, Eddie, et al.,“Book Series, MAP: Spread of Effort and Achievements”, (ISBN 978-602-8199-60-5), Banda Aceh,BRR-UNDP, 2009.

5. AGDC,“LaporanAkhir: PeningkatanKapasitasdankapabilitasPusat Data Geospasial-NAD (Final Report: The Capacity andcapability Building of the Geospatial Data Center-NAD) (AGDC Stage II) (In Indonesian)”, Banda Aceh, AGDC, 2007.

6. AGDC-b. “AGDC Info”, Aceh, AGDC, 2012, http://www.gdc.acehprov.go.id/info.php7. Australia Indonesia Partnership for Reconstruction and Development(AIPRD), “Assessment of Priority Mapping Needs

Nanggroe Aceh Darussalum and Nias Island, Northern Sumatra”,Canberra,2005http://reliefweb.int/sites/reliefweb.int/files/resources/93207D195480658C49257090001F890F-ausaid-idn-25aug.pdf(accessed 2012-2-2)

8. Mindy, Agusta (Ed.),“SIM-Centre Two Years Report: Activity Summary from February 2006 - August 2008”, Banda Aceh,SIM-Centre BRR NAD - NIAS, 2008

9. Nizamuddin, Ishizuka Hidehiro, “A prototype of an integreted information system for geographic information producedduring Rehabilitation and reconstruction process following the earthquakes and tsunami in Aceh province, Indonesia”,Journal of Japan Society of Information and Knowledge, Vol. 23, No. 1, 2013, Japan

10. Harris, Paul. “The Role of Spatial Information in Rebuilding a Sustainable Future for Aceh.Trinidad”, 10th InternationalConference for Spatial Data Infrastructure, http://www.gsdi.org/gsdiconf/gsdi10/papers/TS18.1paper.pdf, 2008.

11. Suwandy, N., Haris, P.M and Mollison, M.,“Patince and perseverance: Building and SID in Aceh”,South East Asian SurveyCongres (SEACS), BAKOSURTANAL, 2009.

12. ESRI, “Geoportal Server” - http://www.esri.com/software/arcgis/geoportal/index.html (accessed 2012-2-2).13. ESRI-b,“Publishing optimized map services”

http://webhelp.esri.com/arcgisdesktop/9.3/index.cfm?TopicName=Publishing_optimized_map_services (accessed 2012-2-2). USA : ESRI, 2012.

14. ESRI-c,“Using ArcIMS 9.3: Publishing a map”http://webhelp.esri.com/arcims/9.3/General/arcims_help.htm (accessed 2012-2-2)

15. ESRI-d,“GeoportalServer : How to Publish Resources”http://help.arcgis.com/en/geoportal_extension/10.0/help/index.html#//00t00000000n000000.htm(accessed 2012-2-2).

16. ESRI-e,“How to Set Up an EsriGeoportal Server”http://www.esri.com/news/arcuser/0611/how-to-set-up-an-esri-geoportal-server.html.

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Improvement of Purity Silicon Obtained from Natural Sand by Antioxidant andAntimicrobial Activities from Leaves of Coleus atropurpureus Benth

Sovia Lenny, Cut Fatimah Zuhra, and Lamek Marpaung

Department of Chemistry FMIPA USU, Email: [email protected]

Abstract. The antioxidant and antimicrobial activities of Coleus atropurpureus Benth leaves extracts were determined. LeavesC.atropurpureus Benth were extracted with methanol, ethylacetate and n-hexane. Test of antioxidant activity by using DPPHmethod. All tested extracts showed strong antioxidant activity. Ethylacetate extract were found to be the most active fractionswith IC50 values of 21.86 mg/L and methanol and n-hexane extracts with IC50 values of 51.2 and 54.38 mg/L. The C.atropurpureus leaves extracts were tested against Shigella SP, Streptococcus mutan, Escherichia coli, Staphylococcus aureus,Candida albicans, Saccharomycess cerevisia and salmonella thypii by the agar diffusion method showed antimicrobial activityagainst all tested microorganisms except n-hexane extracts was not active against E. coli. Research results showed that leavesextracts of C. atropurpureus Benth possess strong antioxidant and antimicrobial properties.

Keywords: Coleus atropurpureus, diffusion method, antioxidant activity.

INTRODUCTION

Coleus atropurpureus Benth is a species of the genus Coleus Lamiaceae family who are scattered throughout thetropics. The specialty of this plant is the diversity of its kind and color. This plant has been growing ornamentalplants with beautiful varieties. The style, shape and color of plants is diverse, but the drug is efficacious as abrownish red. Indonesian people used this plant as a medicine Ambein, abdominal pain, fever, constipation,diabetes mellitus, laxative menstruation, boils, abscesses and wound ulcers [2,11,12]. C. atropurpureus Benth leafextract (syn: C. scutellarioides) has been tested for antibacterial activity against Staphylococcus aureus and thepotential to suppress bacterial infections of the ear [3]. Ethanol extract of leaves Coleus atropurpureus Benth hasantibacterial activity because it can inhibit gram-positive and gram-negative bacteria[6].

Based on phytochemical screening showed that Coleus atropurpureus Benth leaf contains flavonoids and isolationof ethyl acetate extract of the plant as well as UV-Vis spectrum analysis, FT-IR and 1H-NMR spectrum analysisshowed that the isolated compounds flavonoid class of flavon [7]. Flavonoid compounds are one of the manygroups of secondary metabolites analyzed, because flavonoids are the largest constituent of plant pigments, suchas anthocyanin which is a subclass of flavonoids that give red, orange, blue and purple in the leaves, flowers andfruit. Flavonoids are also used as a drug or dietary supplement because it has strong antioxidant activity [5].Flavonoid compounds also showed biological activity such as hypo-allergenic, antiviral and anti-inflammatory[9,10], anti-aging effects caused by the presence of antioxidant compounds, especially phenolic compounds suchas flavonoids13 and effective reduce the risk of cancer, where some of the flavonoid compounds effective as ananticancer and cancer chemopreventive [8]. In this study, antioxidant and antimicrobial activity testC.atropurpureus Benth leaf extracts by solvent extraction variations.

METHODS

Extraction. The leaves of C.atropurpureus Benth (900 g) were dried and powdered. The powder was extracted withmethanol at room temperature for 72 h. Solvent was evaporated under reduced pressure to afford a methanolextract. The extract was partitioned with ethylacetate and H2O (1:1). The ethylacetate extract was partitioned withn-hexane. The ethylacetate and n-hexane solution was concentrated under reduced pressure to afford aethylacetate and n-hexane extract.

Antioxidant activity. The effect on antioxidant on DPPH radical-scavenging is thought to be due to their hydrogen-donating ability. DPPH is a stable free radical and accepts ab electron or hydrogen radical to become a stable

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molecule. The reduction capability (on the DPPH radical) is determined by the decrease in its absorbance at itsabsorption maximum at 517 nm that is induced by antioxidant. This is visualised as a change in colour from violetto yellow. DPPH is usually used a subtrate to evaluate antioxidant activity. Extract solution were prepared bydissolving of dry extract in ethanol (10, 20, 40 and 80 mg/L). 2.5 ml 0f extract solution were mixed with 1 ml DPPHsolution 0.3 mM in the flask. The sample were kept in the dark for 15 min at room temperature and thenabsorbance was measured at 515 nm (changes in colour from viole to light yellow). Radical-scavenging activity wascalculated by the following formula:

% Inibition = [(AB – AA) / AB ] x 100Where AB, absorption of blank sample (t = 0 min); AA, absorption of tested extract solution (t = 15 min).

Antimicrobial activity. The antimicrobial activities of the methanol, ethylacetate and n-hexane extracts wereevaluated by means of the agar disc diffusion method. The media used were Mueller-Hinton agar for the bacteriaand Sabouraud Dextrose agar for the fungi. Filter paper disc (6 mm in diameter) were individually impregnatedwith extract (0.5 g/ml), then placed on the inoculated plates, they were incubated at 370C for 24 h for bacteria andat 300C for 48 h for yeast. The potency of extracts was determined againts Shigella SP, Streptococcus mutan,Escherichia coli, Staphylococcus aureus, Candida albicans, Saccharomycess cerevisia and salmonella thypii. Theantimicrobial activity was measured as the diameter (mm) of clear zone of growth inhibition.

RESULTS AND DISCUSSION

Extraction. The leaves of C. atropurpureus (900 g) were dried and powdered. The powder was extracted withmethanol at room temperature for 72 h. Solvent was evaporated under reduced pressure and yielded 148 g of amethanol extract. The methanol extract was partitioned with ethylacetate and H2O (1:1) at room temperature. Theethylacetate extract was partitioned with n-hexane. The ethylacetate and n-hexane solution was concentratedunder reduced pressure to afford 11.42 g a ethylacetate extract and 58.17 g n-hexane extract.

TABLE 1. Extraction of leaves C.atropurpureusSolvent Extraction yield (gram)Methanol 62.9Ethylacetate 11.42n-hexane 58.17

Antioxidant activity. The relatively stable organic radical DPPH has been widely used in the determination ofantioxidant activity of single compounds as well as of different plant extract [4]. The IC50 values for DPPH assay ofthe samples have been given in Table 2.

TABLE 2. Antioxidant activity of the various extracts from leaves C.atropurpureusSample IC50 (mg/L)Methanol extract 51.2Ethylacetate extract 21.86n-hexane extract 54.38

The ethylacetate extract of C.atropurpureus Benth was able to reduce the stable free radical 2,2-diphenyl-1-picrylhydrazyl (DPPH) to the yellow coloured with an IC50 of 21.86 mg/L. Other extract had antioxidant values 51.2and 54.38 mg/L, measured by the DPPH method. The mechanism of the reaction between antioxidant and DPPHdepens on the stuctural conformation of the antioxidant. Some compounds react very quickly with DPPH, reducinga number of DPPH molecules equal to the number of the hydroxyl groups [1].

As it is shown, all the tested samples showed antioxidant activity in this method. Among the tested samples, theethylacetate extract showed the most antioxidant activity, which may be attributed to the collective antioxidant

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effects of flavonoids present or the other compounds such as phenolics which may potentiate the antioxidantactivity of flavonoids. These secondary metabolites antioxidant activity have been reported in this plant7.

Antimicrobial activity. The growth inhibition zone diameter for the agar disc diffusion method of the sampleshave been given in Figure 3.

FIGURE 3. Grafic antimicrobial activity of the various extracts from leaves C.atropurpureus

The plant extracts showed some degree of activity against microorganims (as a clear zone of paper disc). The dataobtained from disc diffusion method indicated that ethylacetate extract was the most sensitive againstmicroorganism tested with the strongest inhibition zone (10.5 – 20.1 mm) followed by methanol and n-hexaneextracts with inhibition zones < 12 mm except n-hexane extracts was most active to S. thypii (22,9 mm) but notactive to E. coli.

CONCLUSION

The results showed that ethylacetate extracts displayed the higest antioxidant and antimicrobial activity whilemethanol and n-hexane extracts showed lower antioxidant and antimicrobial activity. The n-hexane extractshowed no antimicrobial activity against E. coli.

ACKNOWLEDGMENTS

Thanks to the Rektor of University of Sumatera Utara which has funded this research through DIPA USU 2014(Hibah Bersaing Research Grant)

REFERENCES

1. Bondet, V., Williams W.B., and Berset, C., 1997, Kinetic and mechanism of antioxidant activity using DPPH free radicalmethod. Lebensmittel-Wissenschaft Un Technologie, 30, 609-615.

2. Dalimarta, S., 2008, Atlas Tumbuhan Indonesia, Jilid ke-5, Niaga Swadaya, Jakarta.3. Grosvenor, P.W., Supriono, A. and Gray, D.O., 1995, Medicinal Plants from Riau Province, Sumatra, Indonesia, Part 2 :

0

5

10

15

20

25

Diam

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of z

ones

of i

nhib

ition

(mm

)

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effects of flavonoids present or the other compounds such as phenolics which may potentiate the antioxidantactivity of flavonoids. These secondary metabolites antioxidant activity have been reported in this plant7.

Antimicrobial activity. The growth inhibition zone diameter for the agar disc diffusion method of the sampleshave been given in Figure 3.

FIGURE 3. Grafic antimicrobial activity of the various extracts from leaves C.atropurpureus

The plant extracts showed some degree of activity against microorganims (as a clear zone of paper disc). The dataobtained from disc diffusion method indicated that ethylacetate extract was the most sensitive againstmicroorganism tested with the strongest inhibition zone (10.5 – 20.1 mm) followed by methanol and n-hexaneextracts with inhibition zones < 12 mm except n-hexane extracts was most active to S. thypii (22,9 mm) but notactive to E. coli.

CONCLUSION

The results showed that ethylacetate extracts displayed the higest antioxidant and antimicrobial activity whilemethanol and n-hexane extracts showed lower antioxidant and antimicrobial activity. The n-hexane extractshowed no antimicrobial activity against E. coli.

ACKNOWLEDGMENTS

Thanks to the Rektor of University of Sumatera Utara which has funded this research through DIPA USU 2014(Hibah Bersaing Research Grant)

REFERENCES

1. Bondet, V., Williams W.B., and Berset, C., 1997, Kinetic and mechanism of antioxidant activity using DPPH free radicalmethod. Lebensmittel-Wissenschaft Un Technologie, 30, 609-615.

2. Dalimarta, S., 2008, Atlas Tumbuhan Indonesia, Jilid ke-5, Niaga Swadaya, Jakarta.3. Grosvenor, P.W., Supriono, A. and Gray, D.O., 1995, Medicinal Plants from Riau Province, Sumatra, Indonesia, Part 2 :

Microbial Test

Methanol Extract

n-hexane Extract

Ethylacetate Extract

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effects of flavonoids present or the other compounds such as phenolics which may potentiate the antioxidantactivity of flavonoids. These secondary metabolites antioxidant activity have been reported in this plant7.

Antimicrobial activity. The growth inhibition zone diameter for the agar disc diffusion method of the sampleshave been given in Figure 3.

FIGURE 3. Grafic antimicrobial activity of the various extracts from leaves C.atropurpureus

The plant extracts showed some degree of activity against microorganims (as a clear zone of paper disc). The dataobtained from disc diffusion method indicated that ethylacetate extract was the most sensitive againstmicroorganism tested with the strongest inhibition zone (10.5 – 20.1 mm) followed by methanol and n-hexaneextracts with inhibition zones < 12 mm except n-hexane extracts was most active to S. thypii (22,9 mm) but notactive to E. coli.

CONCLUSION

The results showed that ethylacetate extracts displayed the higest antioxidant and antimicrobial activity whilemethanol and n-hexane extracts showed lower antioxidant and antimicrobial activity. The n-hexane extractshowed no antimicrobial activity against E. coli.

ACKNOWLEDGMENTS

Thanks to the Rektor of University of Sumatera Utara which has funded this research through DIPA USU 2014(Hibah Bersaing Research Grant)

REFERENCES

1. Bondet, V., Williams W.B., and Berset, C., 1997, Kinetic and mechanism of antioxidant activity using DPPH free radicalmethod. Lebensmittel-Wissenschaft Un Technologie, 30, 609-615.

2. Dalimarta, S., 2008, Atlas Tumbuhan Indonesia, Jilid ke-5, Niaga Swadaya, Jakarta.3. Grosvenor, P.W., Supriono, A. and Gray, D.O., 1995, Medicinal Plants from Riau Province, Sumatra, Indonesia, Part 2 :

Methanol Extract

n-hexane Extract

Ethylacetate Extract

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Antibacterial and Antifungal Activity, J.of Ethnopharmacology (45), 97-111.4. Katalinic, V., Molis, M., and Jukic, M., 2006, Screening of 70 medicinal plant extracts for antioxidant capacity and total

phenol, Food Chemistry 94(4), 550-5575. Kitamura, S, 2006, Transport of Flavonoids: From Cytosolic Synthesis to Vacuolar Accumulation, In Grotewold, E., At

The Science of Flavonoids, The Ohio State University Columbus, Ohio, USA.6. Kumala,S., dan Desi, 2009, Aktivitas antibakteri ekstrak daun iler (Coleus atropurpureus Benth) terhadap beberapa

bakteri gram (+) dan gram(-), Jurnal Bahan Alam Indonesia, Vol 1, 12-147. Lenny, S., Barus, T., Marpaung, L. dan Nasution, P., 2012, Identifikasi senyawa flavonoid dari daun tumbuhan Iler

(Coleus atropurpureus Benth), Prosiding Seminar dan Rapat Tahunan (semirata) BKS-PTN Barat Bidang MIPATahun 2012.

8. Lin, J.K. and Weng, M.S., 2006, Flavonoids as Nutraceuticals, In Grotewold, E., At The Science of Flavonoids, TheOhio State University Columbus, Ohio, USA.

9. Marica, M.S., Ivona J., Ana M. and Zeljan M., 2008 In Monika W.H., Joseph S. and Teresa K., At Thin LayerChromatography in Phytochemistry, CRC Press.

10. Pietta, Pier-Giorgio, 2000, Flavonoids as Antioxidants, J. Natural Product (63), 1035-1042.11. Swantara, I.M.D., 2010, Isolasi dan Identifikasi Fraksi Toksik Ekstrak Tumbuhan Iler (Coleus scutellarioides [L.] Benth)

Indonesian Journal of Cancer Vol. 4, No. 1, 9-13.12. Thomas, A.N.S, 1995, Tanaman Obat Tradisional, Volume 2, Cetakan ke-15, Kanisius, Yogyakarta.13. Wang, C.C., Lee, C.J., Chen, L.G., Chang, T.L., Ke, W.M. and Lo, Y.F., 2011, The Correlation Between Skin-Care

Effects and Phytochemical Contents in Lamiaceae Plants, Food Chemistry (124), 833-841

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The Level of High School Student’s Awareness Toward Environment

A.Halim1, Melvina1, and Ibnu Khaldun2

1Department of Physics Education, 2Department of Chemics EducationTeacher Training and Education Faculty, Syiah Kuala University

Email: [email protected]

Abstract: This study aims to determine the level of environmental awareness among high school students in Indonesia andMalaysia. Environmental awareness is one of indicators in science and technology culture and measured by usingInstrument of Science and Technology Culture. The research method is survey, conducted towards high school students inIndonesia (Java and Sumatra) and Malaysia (semenanjung). The data were analyzed by using descriptive statistics. Thisresearch results that Malaysian high school students have higher awareness level of human behavior that causeenvironmental problems (68 %), compared to Indonesian high school students (39 %). The similar result was also foundthat Indonesian high school students have low expectations toward the future of the environment (12%) while Malaysianhigh school students is more optimistic about environment future (38 %). It means that teachers and other stakeholders ineducation are strongly encouraged to give deep and holistic explanation on environmental problems to high schoolstudents.

Keywords: High School Students, awareness, environment, science characteristics, basic science.

INTRODUCTION

Group researcher of TIMSS (Trends in International Mathematics and Science Study) has developed frameworks tomeasure understanding of science and technology among high school students around the world. Understandingof science and technology is a central knowledge and plays important role in modern society [6]. In addition,understanding of science and technology gives significant contribution to individual, community, professionalism,and cultural life of every person. Therefore, the study of science and technology education now is not only focusedon pedagogy of science education and technology, but also has evolved in many multidisciplinary fields such asenvironmental science education research [1], culture of science education research and technology [3,4], sciencetechnology and society education and scientific literacy education.

The level of measurement of existence or manifestation of science and technology culture among high schoolstudents includes 9 indicators, namely (1) attitude towards Science and Technology, (2) environmental awareness,(3) nature of scientific knowledge, (4) ethics of science and technology, (5) attitudes towards use of trial test, (6)understand the limitations of human mind, (7) my view related to the following indicators, (8) the habit ofscientific-minded students, (9) Science student activities outside of school, and (10) basic knowledge of science[3,7,8].

Environmental Awareness in this study is high school students' awareness towards environment around theirschools or neighborhoods. In context of science and technology culture study, environmental awareness is one ofthe most relevant indicators that have high contribution to science and technology culture among high schoolstudents. This fact is showed by the results of validity of science and technology culture instrument that is 0.81 foralpha Crombak and 0.99 for Reliability of indicator of students’ awareness toward the environment [8].

As an effort to enrich the knowledge, especially related to science and technology education. Through thisresearch will be assessed the level of environmental awareness to high school students in Indonesia and Malaysia.This research purpose specifically on students’ views and perception of: (1) role of science and technology insolving environmental problems, (2) future of environment, (3) The equal right of lives towards human and

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animals, (4) society’s awareness on environment, (5) society’s responsibility towards environment, and (6) humanactivity as one of causes that triggers environmental problems .

METHODOLOGY AND DISCUSSION

This study used survey technique towards 467 high school students in Indonesia (Java and Sumatra) and 690 highschool students in Malaysia (peninsula), the respondents are aged 15-17 years old. Data was collected by usinginstrument of Science and Technology Culture, where one of indicators is students’ awareness towardenvironment. Based on indicator of environmental awareness is developed eight items, namely; (1) Environmentalproblem can be solved by science and technology, (2) I believe the future of our environment, (3) Animals have thesame right to life as humans, (4) We need to get a solution to our environmental problems, (5) Society need to beaware or sensitive to the problem environment, (6) Society need to be responsible for protecting the environment,(7) Human activity is a cause of environment problem, and (8) We need to provide a meaningful contribution toprotecting the environment.

The pattern of students’ response use questionnaire and Likert scale by 5 points, namely 1 = Strongly Agree (SS), 2= Agree (S), 3 = No Knowledge (TP), 4 = Disagree (TS), 5 = Strongly Disagree (STS). The instrument (only forindicators of awareness of environment) are shown in Table 1, below

TABLE 1. Indicators and environmental awareness ItemNo Section B: Awarness toward environment SS S TP TS STSB1 Environmental problem can be solved by science and technology 1 2 3 4 5B2 I am optimistic about the future of our environment 1 2 3 4 5B3 Animal should have the same right to life as people 1 2 3 4 5B4 We should find solution to our environmental problem 1 2 3 4 5B5 Society should be aware about environmental problem 1 2 3 4 5B6 Society should care more about protection of the environment 1 2 3 4 5B7 Human activity is a cause of environment problem 1 2 3 4 5B8 Each one of us should make a significant contribution to environmental

protection 1 2 3 4 5

(Source: Halim.et.al. 2009)

Based on 5 point Likert scale above is developed students' levels of awareness toward environment, as shown inTable 2 below.

TABLE 2. Levels of awarness based on the Likert scale 5 points (1 – 5)No. Range of Likert scale Remarks

1 1.00 – 2.44 Have a high awareness2 2.45 – 3.44 Have a medium awareness3 3.45 – 4.44 Have a low awareness4 4.45 – 5.00 There is absolutely no awareness

(Sources: Jack R. Fraenkel. 2011)

Each item is examined, analyzed with descriptive statistics refer to Table 2 above. The results of the data analysisare shown in figure 1 below. The graph in Figure 1 represents the response pattern of 690 high school students inMalaysian Peninsula on 8 items of environmental awareness indicator (B1 to B8). Based on measurement, showsthat item B8 has the largest average that is 2.3.

There is indication that students are less aware of importance of given thoughts and ideas to solve environmentalproblems. This view can be justified, due to education at high schools in Malaysia do not much involves

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environmental problem solving activities scientifically. Therefore, science teachers are strongly encouraged toprovide training or learning project activities associated with forms of project solution for environmental problemsthrough the use of ideas or thoughts.

FIGURE 1. The average response pattern of 690 Malaysian high school students

In contrast, Malaysian high school students have very high awareness related to item B2, namely the believetowards environmental sustainability in the future. If we research and observed, the way of Malaysian governmentaddress environmental issues create high awareness to the students. One of the government actions areregulations on reducing forest fires, prohibiting illegal logging, giving punishment for people who pollute theenvironment, and other forms of legislation. All these laws aim to preserve environment. Whether throughlearning in school or through observation of law implementation in everyday life, unconsciously students buildawareness and assure about future of environment.

FIGURE 2. The average response pattern of 467 Indonesian high school students

The results of data analysis for Indonesian high school students' responses are shown in Figure 2 below. Extremeresponse found on items B2 with average of Likert scale 2.6. Based on data analysis can be inferred that awarenessof Indonesian high school students is at middle level. It means that students are unsure or less optimistic about the

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environmental problem solving activities scientifically. Therefore, science teachers are strongly encouraged toprovide training or learning project activities associated with forms of project solution for environmental problemsthrough the use of ideas or thoughts.

FIGURE 1. The average response pattern of 690 Malaysian high school students

In contrast, Malaysian high school students have very high awareness related to item B2, namely the believetowards environmental sustainability in the future. If we research and observed, the way of Malaysian governmentaddress environmental issues create high awareness to the students. One of the government actions areregulations on reducing forest fires, prohibiting illegal logging, giving punishment for people who pollute theenvironment, and other forms of legislation. All these laws aim to preserve environment. Whether throughlearning in school or through observation of law implementation in everyday life, unconsciously students buildawareness and assure about future of environment.

FIGURE 2. The average response pattern of 467 Indonesian high school students

The results of data analysis for Indonesian high school students' responses are shown in Figure 2 below. Extremeresponse found on items B2 with average of Likert scale 2.6. Based on data analysis can be inferred that awarenessof Indonesian high school students is at middle level. It means that students are unsure or less optimistic about the

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environmental problem solving activities scientifically. Therefore, science teachers are strongly encouraged toprovide training or learning project activities associated with forms of project solution for environmental problemsthrough the use of ideas or thoughts.

FIGURE 1. The average response pattern of 690 Malaysian high school students

In contrast, Malaysian high school students have very high awareness related to item B2, namely the believetowards environmental sustainability in the future. If we research and observed, the way of Malaysian governmentaddress environmental issues create high awareness to the students. One of the government actions areregulations on reducing forest fires, prohibiting illegal logging, giving punishment for people who pollute theenvironment, and other forms of legislation. All these laws aim to preserve environment. Whether throughlearning in school or through observation of law implementation in everyday life, unconsciously students buildawareness and assure about future of environment.

FIGURE 2. The average response pattern of 467 Indonesian high school students

The results of data analysis for Indonesian high school students' responses are shown in Figure 2 below. Extremeresponse found on items B2 with average of Likert scale 2.6. Based on data analysis can be inferred that awarenessof Indonesian high school students is at middle level. It means that students are unsure or less optimistic about the

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future sustainability of the environment in Indonesia. It is caused by lacking of attention or efforts by governmentto protect environment. The fact that government less commitment in implementing regulation of forestprotection and giving punishments to people who violate the laws, where at the end triggers many illegal loggingand deforestation. This phenomena create less assure or optimistic attitude on the students toward future forestenvironment in Indonesia. The highest awareness shown by students in Indonesia is related to the role andresponsibility of community to preserve the environment. It shown by students' responses on item B5 and B6 withaverage of Likert scale is 1.2. Based on the response can be inferred that high schools students in Indonesia putmore trust on community to protect environment rather than government.

Comparison of level of high school students' environmental awareness in Indonesia and Malaysia were analyzedusing t-test with different amount of respondent. The results of data analysis provided average response 1,907 forMalaysian and 1,667 for Indonesian. While the results of value-t calculation obtained 9.7. Based on the degree offreedom from total of respondent of high school students in Malaysia and Indonesia provided T table 2.58. Both tand T values as statistic show significant difference with significant level 0f 0.05 and probability P = 0.00. As theresult, it shows that in overall high school students in Indonesia have higher levels of environmental awarenessthan the students in Malaysia. But, the Malaysian students have higher level of environmental awarenesscompared to the Indonesian students at certain items.

CONCLUSION

In overall, high school students in Indonesia have level of environmental awareness better than the Malaysianstudents. But, Malaysian high school students have higher level of environmental awareness on certain itemscompared to Indonesian high school students. For example is item B2, level of Malaysian high school students (1.6)is higher consciousness than the Indonesian high school students (2.5). Based on data analysis, can be inferred thatthe level of environmental awareness of Indonesian high schools students is at middle category. It indicates thatIndonesian students are not sure or less optimist towards environmental sustainability in Indonesia. Students’ lowawareness and belief due to less commitment by government in protecting our environment.

ACKNOWLEDGMENTS

Our thanks to all parties who had contributed thoughts, ideas and financial in conducting this research. EspeciallyDirectorate General of Higher Education, who had supported funding through research grants and internationalpublications. We thank you all very much. Hopefully your help will be granted reward from Allah SWT. Amen.

REFERENCES

1. Ramo´n S. Barthelemy, Charles Henderson, and Megan L. Grunert (2013) Physics Education Research 9.020107 (2013).2. Jack R. Fraenkel (2011) How to Design and Evaluate Research in Education, Mc Graw Hill. N.Y3. Rusilawati Othman. 2007. Budaya sains dan teknologi dikalangan murid sekolah dan hubungannya dengan pertambahan

tempoh pembelajaran sains. Tesis Ph.D, Fakulti Pendidikan, Universiti Kebangsaan Malaysia.4. Godin B., and Gingras Y., 2000. What is scientific and technological culture and how is it measured? A multidimensional

model. Public Understand. Sci. 9 (2000) 43–58.5. Collins S, Reiss M, and Simon S., 2006. A literature review of research conducted on young people’s attitudes to science

education and biomedical science. A report published by the Wellcome Trust, IOE Lodon, August 2006.6. TIMSS and PISA (2009) Assessment Framework: Key competencies in reading, mathematics and science. OECD,

Canada7. Halim, A. (2008) Pilot tes pengembangan instrument budaya sains dan teknologi. Laporan Penelitian Hibab Publikasi

Internasional. Unsyiah.8. Lilia Halim., (2007). Pembangunan dan validitas instrument budaya sains dan teknologi. Laporan Penelitian hibah OPF.

Universiti Kebangsanaan Malaysia.

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Increased of Purity Silicon from Natural Sand with Variation of Heating Timethrough Magnesiotermal

Andriayania*, Nofrijon Sofyanb, Herlince Sihotangc, Saur Lumban Rajad

a,c,d Department of Chemistry, Faculty of Mathematics and Natural SciencesUniversity of Sumatera Utara; bDepartement of Metallurgical and Materials Engineering, University of Indonesia

*[email protected]

Abstract. Extraction of silicon from natural sand obtained from Asahan in North Sumatera has been done. The reaction wascarried out using magnesium and followed by a purification using inorganic acids. Silicone products were characterized usingXRD and quantitatively analyzed using Relative Intensity Ratio (RIR) methode. The level purity of product silicon on heating for 3hours was obtained (90.5%), 4 hours was obtained (92.1%) and 5 hours was obtained (100%). Silicone products are reacted withchlorine gas produces a semi-crystalline silica and is hygroscopic.

Keywords: natural sand, silicone, magnesiothermal, XRD, RIR

INTRODUCTION

Quartz sand is a mineral composed of crystals of silica (SiO2) as the main component and other minerals in theform of metal oxides in small amounts. Quartz sand has a translucent white or other colors depend on thecompound impurities. Quartz sand are found along the coast at Tanjung Tiram Asahan North Sumatera has achemical composition of SiO2 (72.92%), Fe2O3 (0.31%), Na2O (1.59%), K2O (6.17%), CaO (2.81%), Al2O3 (14.73%) andMgO (0.65%) (Distam-prpsu-2, 2004). Thus silica is very abundant source of silicon. Silicon (Si) as the secondelement in the earth's crust after oxygen [2], is not found in a free state that is usually obtained from theextraction of silica and other materials. There are several ways of extraction of silicon from silica such as quartzsand reduction with carbon at high temperatures using an electric furnace [3,4,5], extraction of silica from riversZauma, Zamfara state [6], reduction fume silica by magnesium powder, reduction silica using aluminum and sulpur[7], reduction of amorphous silica using calcium [8], reduction of porous SiO2 pellets electrochemically using fusedCaCl2 and/or CaCl2-NaCl salt mixture [9].

Silicon exists in the form crystalin shiny metal and silicon powder as brownish-black. Because it has properties ofmetals and non-metals (metalloids) are widely used as materials in various fields. The level of purity silicondetermine its usefulness. Chemical analysis of the level of purity silicon for the semiconductor industry weredivided into four groups [10]: (1) metallurgical-grade silicon (99 ppm), (2) solar-grade silicon (99.999 9 ppm), (3)polycrystalline solar-grade silicon (99.999 99 ppm) and electronic-grade silicon (999 999 999 99 999 ppm). Siliconpowder can be oxidized to the ceramic material (Si3N4) [11], in the form of crystalline silicon used for solar cells[3,10]. To improve the purity silicon, in this paper we perform the extraction of silicon from natural sand usingmagnesium. Reaction conditions by varying the heating time in the furnace. Analysis of the structure of siliconproducts were characterized by XRD and composition quantitatively analyzed using the Reference Intensity Ratio(RIR) base computer. The RIR method to analyze quantitatively the microstructure and mineralogy. Furthermore,silicon product obtained is reacted with chlorine gas to obtain a compound of silicon tetrachloride (SiCl4). Theproducts obtained were analyzed using FT-IR.

EXPERIMENTAL

Instruments. The instrument used are: glass tools, droping funnel, metal bowls, stone mortar and pestle, anelectric sieve, hotplate and stirrer, scales, centrifuges, furnaces, ovens. Characterization of the crystal structureand composition using XRD performed at Yogyakarta State University Yogyakarta, FT-IR characterization conductedin Indonesian Research Institute (LIPI), Jakarta.

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Materials. Materials used: natural sand were obtained from Tanjung Tiram Asahan in North Sumatera,concentrated sulfuric acid and hydrochloric acid, hydrofluoric acid, magnesium powder, acetic acid, manganesedioxide, sodium hydroxide, aerosil, distilled water and aqua bides. Experiments conducted in the ResearchLaboratory (LP), Basic Science Laboratory (LIDA), Inorganic Chemistry Laboratory University of Sumatera Utara.

Purification of Silica (SiO2) from Natural Sand. Silica (SiO2 ) is purified from natural sand obtained from theTanjung Tiram Asahan in North Sumatra, performed as ever dilkukan in [13]. White silica solids were characterizedby XRD and analyzed quantitatively using the RIR method.

Extraction of Silicon (Si) from silica (SiO2). Silica (SiO2) natural sand mixed with magnesium powder with a ratio(1:1.75), is inserted into a vessel of metal, stirring until blended and sealed properly. Inserted into the furnace andheated at a temperature 800C for 4 hours. The reaction mixture was cooled and purification with three step. Inthe first stage solids added 150 mL of 2M HCl, stirred while heated at 800C for 3 hours. Then filtered, the solidswashed with aquabides and dried. After drying the second stage purification process is done by adding a mixtureof 2M HCl and CH3COOH 25% with a ratio(1: 2). The mixture were stirred and heated at 80C for 3 hours. The solidwas separated and washed with aquabides and dried. Further purification third step is done by adding hydrofluoricacid 4.8% and acetic acid (CH3COOH) 25% with a ratio (1: 2), stirred and heated at 80C for 3 hours. The mixture iscooled and the solids are separated then washed with aqabides and dried. The solids were characterized by X-raydiffraction (XRD). Silicon extraction process of natural sand is done by varying the heating time for 4 hours and 5hours.

Synthesis of silicon tetrachloride (SiCl4). The circuit first instrument was prepared and supplied nitrogen gas. Intoa three-neck flask which was filled with 14 g of MnO2 solids, dropped into concentrated HCl (20 mL) slowly using adropping funnel connected to a tube containing sulfuric acid to absorb water. Then the tube is connected to the Upipe containing aerosil. Furthermore pipe U connected to a container tube silicon which is heated with gas flame.SiCl4 vapor produced flowed into the condenser and container products cooled using ice cubes.

RESULTS AND DISCUSSION

The solid silica (SiO2), which is obtained from natural sand [13], is reacted with magnesium powder and heated to atemperature 800C with silica and magnesium ratio (1:1.75). The heating time variated for 3 hours, 4 hours and 5hours. Product silicon with variation of heating time for 3 hours obtained silicone products blackish brown.Characterization of the structure using X-ray diffraction (XRD) (Figure 1). XRD diffractogram of silicon (Si) shows theangle 2 at 28,487 hkl (111); 47,330 hkl (220); 56,154 hkl (311); 59,34 hkl (222); 69,145 hkl (400); and 76,392hkl (331). XRD data adjusted with the literature [14].

FIGURE 1. Peak Difraktogram XRD Silicon Product at Heating Time for 3 hours

Meas. data:Andriayani1;1,75/Data 1

2-theta (deg)

Inte

nsity

(cps

)

20 40 60 0

10000

20000

30000

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Purity silicon products were analyzed quantitatively using Relative Intensity Ratio (RIR) methode based computerand its composition is shown in Table 1.

TABEL 1. Composition of Silicon Product Using Relative Intensity Ratio (RIR) methode from Heating Time for 3 Hours

Qualitative and Quantitative analysis resultsPhase name Formula Figure of

meritPhase reg. detail DB card number Weigth ratio

Content(%)Silicon, syn Si 0.290 ICDD (PDF-2/Release

2012 RDB)01-070-5680 90.5(8)

Spinel, syn (Mg0.47 Al0.53)(Al1.36 Mg0.53 B0.11) O4

0.959 ICDD (PDF-2/Release2012 RDB)

01-078-6060 9.5(4)

Silicone products from silica reduction by heating time for 4 hours obtained silicone products blackish brown.Characterization of the structure using X-ray diffraction (XRD) shown in Figure 2. Diffractogram peak silicon (Si)shows the angle 2 are at 28,557 hkl (111); 47,411 hkl (220); 56,218 hkl (311); 59,46 hkl (222); 69,210 hkl(400); 76,456 hkl (331) and 88.089 hkl (422). The results of the XRD data adjusted with the literature14.

FIGURE 1. Peak Difraktogram XRD Silicon Product at Heating Time for 4 hours

Purity silicon products were analyzed quantitatively using Relative Intensity Ratio (RIR) methode based computerand its composition is shown in Table 2.

TABEL (2). Composition of Silicon Product Using Relative Intensity Ratio (RIR) methode from Heating Time for 4 Hours

Qualitative and Quantitative analysis resultsPhase name Formula Figure of

meritPhase reg. detail DB card number Weigth ratio

Content(%)Silicon, syn Si 0.417 ICDD (PDF-2/Release 2012 RDB) 01-070-5680 92.1(7)Spinel, Hp, syn,magnesium

MgAl2O4 0.525 ICDD (PDF-2/Release 2012 RDB) 01-072-6946 7.9(3)

Silicone products from reduction of silica by heating time for 5 hours obtained silicon products blackish brown.Characterization structure using X-ray diffraction (XRD) shown in Figure 3. XRD diffractogram peak at an angle 2showed the presence silicon (Si) at 28,520 hkl (111); 47,365 hkl (220); 56,155 hkl (311); 69,192 hkl (400);76,398 hkl (331) and 88.060 hkl (422). The results of the XRD data adjusted with the literature [143].

2-theta (deg)

Inte

nsity

(cps

)

20 40 60 80 0e+000

1e+004

2e+004

3e+004

4e+004

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FIGURE 3. Peak Difraktogram XRD Silicon Product at Heating Time for 5 hours

Purity silicon products were analyzed quantitatively using Relative Intensity Ratio (RIR) methode based computerand its composition is shown in Table 3.

TABEL 3. Composition of Silicon Product Using Relative Intensity Ratio (RIR) methode from Heating Time for 5 Hours

Qualitative and Quantitative analysis resultsPhase name Formula Figure of

meritPhase reg. detail DB card number Weigth ratio

Content(%)Silicon, syn Si 0.355 ICDD (PDF-2/Release 2012 RDB) 01-070-5680 100.0(9)

Silicone product with 92.1% purity level obtained with the heating time for 4 hours then treated with chlorine gasin nitrogen conditions to obtain compounds silicon tetrachloride. After the reaction is carried out silicon tetrachloride compound is obtained in the form of white gas and a pungent odor. Besides, it also produced otherproducts such as white solid (Figure 4) contained in the sample container and condenser. The white solidseparated and characterized using FT-IR to prove the functional group contained in the compound.

FIGURE 4. White Solid from Synthesis Compounds Silicon Tetrachloride

FT-IR spectrum of the white solid product is shown in Figure 4. Absorption peak at the wave number of 3035.71cm-1 indicate the presence of Si-OH stretching vibration of the hydrogen bonding of Si-OH functional group, at1637.19 cm-1 due to the OH bending vibration of adsorbed molecular water, at 1078.96 cm-1 shows the asymmetric

2-theta (deg)

Inte

nsity

(cps

)

20 40 60 80 0e+000

1e+004

2e+004

3e+004

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stretching vibration bands of Si-O-Si of functional groups of Si-O-Si, at 918.26 cm-1 shows the bending vibration ofSi-O (H-H2O) of Si-OH functional group and at 806.32 cm-1 shows the Si-O bending vibrations of the functionalgroups of Si-O-Si. Based on data from FT-IR is a white solid compound of silica (SiO2) which is hygroscopic so it canbe used as a water absorbent material. In this case we test it by letting the open air after a few minutes turnedinto a moist white solid (lumpy) but once dried again in an oven at a temperature of solids 80C becomes dryagain. The ability to adsorb water on silica solids derived due to the Si-OH groups (silanols) on SiO2 surfaces thatcan bind with water molecules through hydrogen bonding.

FIGURE 3.16 FT-IR spectra Semi-crystalline SiO2 Results Reaction Products Silicon (92.1%) with Chlorine Gas (Cl2)

Because the synthesis of SiCl4 produced gaseous products then our next product SiCl4 reacted immediately withdry ethanol produces compounds Si (OC2H) 4 in order to isolate and to characterize the products. These works hasnot been completed and are under characterization.

CONCLUSIONS

1. Extraction of silicon from natural sand obtained from the Tanjung Tiram Asahan in North Sumatera hasbeen done. Extraction was carried out using magnesium and followed by a purification process usinginorganic acids. Silicone products were characterized using XRD and quantitatively analyzed using theRelative Intensity Ratio (RIR). The level of purity silicon products obtained at the time variation of heatingfor 3 hours was (90.5%), 4 hours (92.1%), and 5 hours (100%). Based on these data, the time of heating ina furnace affect the level of product purity silicon.

2. Synthesis of compounds of silicon tetrachloride using silicone product purity (92.1%) resulting whitegaseous SiCl4 and has strong odors. Besides, the resulting white solid material of silica (SiO2) which ishygroscopic so it can be used as an adsorbent to absorb water.

ACKNOWLEDGMENTS

Thanks to the Chancellor of the University of Sumatera Utara which has funded this research through DIPA USU2014 Fundamental Research Grant.

REFERENCES

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2. Lee, J. D,”Concise Inorganic Chemistry”, fourth edition, Chapman & Hall, New York, (1994) pp:3. Masmui and Suhedra, Proseding InSiNas, 2012, pp MT-79-MT-83

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