tilization Of Ammonium Hydroxide Compound As Carbosorb For Measurement Of Carbon-14 In Determination Age Of Coral Reef Sample has been performed. The objective of this research is to Determine the age of Coral Sample of Spermonde Islands through Activity Measurements of carbon-14 with LSC (Liquid Scintillation Counting) method. Coral sample were taken from around Langkai Island. The steps of this research are: Sample preparation, CO2 absorption with solution of MEA, DEA and TEA and measurement of carbon-14 activity using Liquid Scintillation Counter (LSC) Hidex 300 SL. Absorption CO2 using ammonium hydroxide. The specific activity of coral sample using carbosorb ammonium hydroxide was 14.43 ± 1,2 DPM/g C. The age of coral sample calculated from the specific activity using carbosorb ammonium hydroxide was 484.63 ± 54 years.Keywords : LSC (Liquid Scintilation Counter), Carbon-14, CO2 Absorption, Ammonium hydroxide, Langkai Islan

Maming, Maming

Tenrisa’na, Andi

Zakir, Muhammad

English

Marina Chimica Acta

 55  Marina Chimica Acta, April 2015 Jurusan Kimia, FMIPA UNHAS Vol. 16  No.1 ISSN 1441-2132 UTILIZATION OF AMMONIUM HYDROXIDE COMPOUND AS CARBOSORB  FOR MEASUREMENT OF CARBON-14 IN DETERMINATION AGE OF CORAL REEF SAMPLE FROM SPERMONDE ISLANDS  Andi Tenrisa’na*, Muhammad Zakir and Maming  Radiation Chemistry Laboratory, Hasanuddin University Kampus UNHAS Tamalanrea, Makassar, 90245 *contact : t.sanna89@gmail.com   ABSTRACT  Utilization Of Ammonium Hydroxide Compound As Carbosorb For Measurement Of Carbon-14 In Determination Age Of Coral Reef Sample has been performed. The objective of this research is to Determine the age of Coral Sample of Spermonde Islands through Activity Measurements of carbon-14 with LSC (Liquid Scintillation Counting) method. Coral sample were taken from around Langkai Island. The steps of this research are: Sample preparation, CO2 absorption with solution of MEA, DEA and TEA and measurement of carbon-14 activity using Liquid Scintillation Counter (LSC) Hidex 300 SL. Absorption CO2 using ammonium hydroxide. The specific activity of coral  sample using carbosorb ammonium hydroxide was 14.43 ± 1,2 DPM/g C. The age of coral  sample calculated from the specific activity using carbosorb ammonium hydroxide was 484.63 ± 54  years. Keywords : LSC (Liquid Scintilation Counter), Carbon-14, CO2 Absorption, Ammonium hydroxide, Langkai Island  INTRODUCTION  Spermonde Islands is one of the most important area in South Sulawesi. Spermonde Islands identified     ± 400,000 ha. Coral reefs are found in the waters of Indonesia are more than 60,000 km2 and most of them found from eastern to western Indonesia. There are 350 species of coral found  in Indonesia, 250 species of which found  in Spermonde Islands the reef area of 150 km2. Spermonde Islands coral diversity levels are quite high because there are 78 genera and sub-genera, with 262 species of a total coral judging from the level of deployment, approximately 80% -87% of the region, the outer reef (Coremap, 2003). Determination of age of the coral reefs die in a sea also has enormous benefits in studying the geography of the sea coral origin such as samples to trace and study the establishment of a sector in coastal rock formations. Besides the determination of age, coral reefs can also be used to determine the apparent radiocarbon age of the sea (Yuliati and Akhadi, 2005). Arman et all (2013) determined age of the coral reefs and growth rate of reef to determine the characteristics of the water such as an increase in sea surface temperatures, one of which caused by the El-Nino in the Thousand Islands. Characteristics of the waters can be identified through a decrease in the rate of linear growth of coral reefs, especially in times of El-nino on a large scale as in 1997-1998 and 1982-1983. The decline in the rate of linear growth is also due to factors occurring water conditions on a small scale (local) as a result of increased levels of pollutants, nutrients and sedimentation. Determination age of the coral reefs can be known through radiocarbon dating method. This method is based on the calculation of the 14C activity was  56  Utilization of Ammonium… Vol. 16  No.1 contained in a carbon sample. The value of this activity is then converted into the age when compared with the reference standard modern. 14C (radiocarbon) is produced in the atmosphere produced with the reaction between cosmic radiation and nitrogen, forming 14C. When a subsystem (trees, sea shells and others) isolated from the global system (eg trees are cut, or dead and buried in the ground) and then no more radiocarbon is added to it, then the activities of the radiocarbon (14C in a number of subsystems or footage) start reduced in accordance with the law of radioactive decay (Faisal, 2009). The last few years, scientists have developed a liquid scintillation counting method for the measurement of total α and β in environmental samples, because existing methods (electrodeposition method) is quite complicated. Liquid scintillation counting method is now not only used for the counting of low-energy β radiation, but can be used also for counting of α and β total. This method is known as LSC (Liquid scintillation Counting). Advantages compared with the previous method is a liquid preparation facilitate sample dissolved homogeneously, so there is no effect of self-absorption. This method can detect 3H and 14C, and can determine α and β the total at once, thereby saving time (Tjahaja and Mutiah, 2000). Method of age determination using 14C during chopping is done by liquid scintillation counter with C6H6, chopping C in the form of graphite with AMS (Accelerator Mass Spectrometry) and chopping CH4 with Mini Gas Proportional Spectrometry. These methods are rarely used in the determination of age because of the cost of equipment and materials to repair the sample is very expensive. Sample preparation is quite complicated, long and requires consideration of adequate technical skills so as to study hydrology especially uneconomical and inefficient, because only one sample can be analyzed daily. The last two decades have started to develop CO2 absorption method is better than previous methods (Satrio and Abidin, 2007). Yarianto et all (2001) used liquid scintillation counter to determine the optimum conditions for the determination of the radioactivity of 32P labeled insect pests. Panggabean (2002) reported the adaptation of the method of analysis of 14C in sea water using NaOH absorber by means of LSC. In 2010 Suyarso reported past changes in sea level by the age of the fossil shells with CO2 absorption method using a liquid scintillation counter. Satria et al (2012) determined the age of the Lapindo mud water and mountain stalactites kidul with CO2 absorption method using a liquid scintillation counter. Therefore, in this study will be conducted to determine the age of the coral reefs in the maritime Spermonde through measurements of 14C activity by LSC method using NH4OH carbosorb.   MATERIAL AND METHODS Materials The materials of this study was 30% H2O2, HClO4 1 N, 1 N NaOH, ethanolamine, N2 gas HP (High Purity), 10% HCl, AgNO3, silica gel, marble, scintillator aqualight LLT, filter paper, distilled water and coral reefs .  Apparatus Preparation tool in the form of round-bottom flask, impinger, funnel, absorption column, glass cup, mortar, gloves, oven, hammer and tools glasses commonly used in laboratories as well as β radiation count tool of carbon-14 sample is LSC Hidex 300 SL.   Sampling Coral sample taken at seawater near one of the islands in the Spermonde Archipelago, which is in Langkai Island at a depth about 4-5 m. Langkai Island  57  Utilization of Ammonium… Vol. 16  No.1 located on coordinate S: 05o 01’ 47,055” E: 119o 05’ 50,272”.   Phisical and Chemical Cleaning Cleaning methods are designed to remove contaminating carbon sources that accumulate both while the specimen is on the sea floor and while it is stored on land after collection. Water rinses and scrubbing with a brush remove sediment from inside the coral and between the septa. Samples are then immersed in a 1:1 mixture of 30% H2O2  and 1N NaOH and ultrasonicated for 15 minutes. However, this process often leaves a brownish/orange organic stain on the CaCO3. Quick dips (30 seconds to 2 minutes) in a 1:1 mixture of 30% H2O2  and 1N HClO4 effectively remove this stain. After the dilute perchloric step, samples are rinsed thoroughly with clean distilled water. For the second acid wash, pre-weighed samples are dipped into 6N HCl for 15–60 seconds followed by rinses in two separate beakers of distilled H2O. After drying for several minutes in a 60 °C oven, the samples are cooled and reweighed to determine the percent of sample removed. Samples are then crushed in an agate mortar and pestle to facilitate dissolution in the reaction flasks.1  Carbon Dioxide Absorption Dried coral were transferred to flask that connected to a separation funnel as hydrochloric acid reservoir. Prior to carbon dioxide absorption, the nitrogen gas was streamed along the system. Solution of 10 % HCl was added by drops to the sample until bubles formed (Fig.1).Gas is channeled into an impinger contains 40 mL ammonium hydroxide as carbosorb after passed acid trap and water trap. The process was stopped when the gas not formed by adding the hydrochloric acid. Concentration of CO2 absorbed was quantified from the difference of weight before and after absorption process   Figure 1. Design of absorption system of carbon dioxide from coral sample   The same method is used to absorb CO2 from Marble for use in the measurement of the Background  Determination of Total Carbon  (NH4)2CO3 dissolved pipetted in Erlenmeyer 10 mL to titration with 5 M HCl solution after the addition of a few drops of indicator MO until the color changes from brown to pink. Furthermore, pipette 10 ml of (NH4)2CO3 into a beaker for added  BaCl2 10% solution until be precipitation (saturated). Subsequently, the precipitate and the filtrate was separated used filtered, then the filtrate was pipetted into Erlenmeyer 10 mL for titrated with 5 M HCl solution with the addition of a few drops of indicator PP until the color changes from purple to clear.  Carbon-14 Counting Approximately 8 mL of sample or background mixture with 12 mL scintillator in 20 mL vial. The mixture was homogenated by shaking and saved from light exposure, and then lied on 20 mL vial plate tray. Counting the sample as protocol LSC Hidex 300 SL and it was counted at 5-240 minutes in range.   RESULT AND DISCUSSION Phisical and Chemical Cleaning Coral sampel that have been physically and chemically cleaned looked clean and white. The chemical cleaning removed impurities and carbon source on the surface up to 8,63 %. The result of these experiments are not much different from the result of deep-sea coral sample  58  Utilization of Ammonium… Vol. 16  No.1 cleanup was done by Adkins et al. 1 and Maming et al.6 The missing part of the sample is a natural contaminant that accumulates over the coral reef waters and dissolved matrix surface.  Counting Carbon-14 The results of measurements of 14C activity measured on the instrument is expressed in units of Count Per Minute (CPM) which shows the number of β particles produced from 14C in coral sample in every minute, and the activity of coral sample is expressed in units Disintegration Per Minute (DPM) which shows the actual number of atoms in the 14C decays coral samples in every minute. The relationship between the value of DPM and the value CPM is expressed as a form of efficiency in units of counting which stated Triple Double Coincidence Ratio (TDCR).  Measurement of background was done by the CO2 absorption using marble as a source of CO2  background. Marble is a carbon source with old age that is considered to contain carbon-14 with very low activity. Determination of the optimum time of counting was performed to determine the best time and the resulting DPM value and TDCR value stable as a sign that the sample counting process running optimally. In 90-240 minutes, activity values of 14C ranging achieve stability. The optimum time of counting sample and background are determined based on the figure 2. The optimum time of counting is 120 minutes for sample and optimum time of counting is 60 minutes for background.    Figure 2. Determination of Counting  Time Optimum Sample and Background Of Coral Reef  Determination of specific activity of the sample of coral reefs can known based counting from sample and background  at the optimum time respectively 120 and 60 minutes. The counting is done as much as 7 times repetition, in order to obtain the average activity of the sample and the background can be seen in Table 2. The average activity data is then used to determine the value of the specific activity of samples of coral reefs.   Table 2. Activity of 14C Sample and Background Sample Background DPM TDCR DPM TDCR 108,030 107,630 107,310 106,990 106,770 106,500 106,030 0,604 0,588 0,603 0,603 0,600 0,606 0,604 104,690 104,320 103,370 103,320 102,800 102,660 101,920 0,602 0,604 0,605 0,596 0,607 0,609 0,610   59  Utilization of Ammonium… Vol. 16  No.1  The specific activity of samples of coral reefs can be determined from the difference between the results of Disintegration Per Minute (DPM) of sample and the results of Disintegration Per Minute (DPM) background divided by the total content of carbon in 8 mL of sample were mixed with 12 ml of scintillator. Determination of total carbon contained in the coral reef sample titration method and gravimetric method. Both methods are very supportive in this study. Total carbon mass obtained on samples of coral reefs are shown in Table 3. The value of the specific activity is indicated by DPM units per unit mass. Specific activity data samples of coral reefs are shown in Table 3. The value of the specific activity (As) shows the number of atoms of 14C that decays every minute in one gram of carbon element.   Table 3.  The Specific Activity (As) of Coral Reef Sample from Langkai Island  DPMs DPMb DPM C-total (g) As (DPM/gC) As C-14 life 107.037 103.297 3,740 0,2592 14,43 ± 1,2 15,30 ± 0,1  Age determination of coral sample is determined based on the specific activities that have been obtained previously. The age of coral  sample calculated from the specific activity using ammonium hydroxide as carbosorb was 484.63 ± 54 years.   CONCLUSION The specific activity of coral  sample using ammonium hydroxide as carbosorb was 14.43 ± 1,2 DPM/g C. The age of coral  sample calculated from the specific activity using ammonium hydroxide as carbosorb was    484.63 ± 54  years.  BIBLIOGRAPHY  Adkins, J.F., Griffin, S., Kashgaria, M., Cheng, H., Druffel, E.R.M., Boyle, E.A., Edwards, R.L., Shen, C.C. (2002)  Radiocarbon Dating of Deep-Sea Corals. Radiocarbon. 44 (2) : 567-580. Antoni, 1995, Studi Distribusi Radioisotop Sulfur -35 Dalam Organ Tubuh Karrper (Cyprinus Carpio) Dengan Metode Pencacahan Sintilasi Cair, Jurnal Tidak Diterbitkan, Jurusan Kimia Fakultas Matemmatika dan Ilmu Pengetahuan Alam Universitas Hasanuddin, Makassar. Arman, A. dkk., 2013, Studi Penentuan Umur dan Laju Pertumbuhan Terumbu Karang terkait dengan Perubahan Iklim Ekstrim Menggunakan Sinar-X, Jurnal Ilmiah Aplikasi Isotop dan Radiasi, 9 (1): 1-10. Kasnir, M., 2011, Analisis Aspek Ekologi Penatakelolaan Minawisata Bahari di Kepulauan Spermonde Kabupaten Pangkep, Sulawesi Selatan, Ilmu Kelautan, 16 (2): 61-69. Lenterak, 2013, Terumbu Karang Perekam Gempa Bumi Alami, (Online), (http://lenterakecil.com///terumbu- karang- perekam- gempa - bumi -alami, diakses 2 Januari 2014). Libby, W.F.(1960) Radiocarbon Dating. Nobel Lecture. Elsevier Publishing Company: Amsterdam. Panggabean, S. M., 2002, Adaptasi Metode Analisis C-14 dalam Air Laut, Hasil Penelitian Pusat Pengembangan Pengelolaan Limbah Radioaktif. Satrio dan Abidin, Z., 2007, Perbandingan Metode Sintesis Benzena dan Absorpsi CO2 Untuk Penanggalan Radioisotop 14C, Jurnal Ilmiah  60  Utilization of Ammonium… Vol. 16  No.1 Aplikasi Isotop dan Radiasi, Jakarta, 3 (1): 1-26. Satrio, Sidauruk, P., dan Pratikno, B., 2012, Studi Iklim dan Vegetasi Menggunakan Pengukuran Isotop Alam Stalaktit Goa Seropan, Gunung Kidul-Yogyakarta, Jurnal Ilmiah Aplikasi Isotop dan Radiasi, Jakarta, 8 (1): 43-52. Satrio, Pratikno, B. dan Sidauruk, P., 2012, Studi Asal-Usul Air Lumpur Lapindo Periode 2007-2012 Menggunakan Isotop Alam, Jurnal Ilmiah Aplikasi Isotop dan Radiasi, Jakarta, 8 (2): 89-100. Sidauruk, P. dan Satrio, 2010, 2-Metoksietilamin sebagai Alternatif Absorber CO2 Untuk Analisis 14C dalam Tanah dan Air Tanah, Jurnal Ilmiah Aplikasi Isotop dan Rasiasi, Jakarta, 6 (2): 117-124. Tjahaja, I.P., dan Mutiah, 2000, Metode Pencacahan Sintilasi Cair : Salah Satu Alternatif untuk Pengukuran α dan β Total dalam Sampel Lingkungan, Indonesian Journal of Nuclear Science and Technology, 1 (1): 31-46. Yarianto, S., Susilo, B., Sutrisno, S., 2001, Kondisi Optimal untuk Penentuan Radioaktivitas Serangga Hama Bertanda P-32 dengan Menggunakan Pencacah Sintilasi Cair, Risalah Pertemuan Ilmiah Penelitian dan Pengembangan Aplikasi Isotop dan Radiasi, Fakultas Teknik, Universitas Gajah Mada, Yogyakarta.  Yuliati, H., Akhadi, M., 2005, Radionuklida Kosmogenik Untuk Penaggalan, Puslitbang Keselamatan Radiasi dan Biomedika Nuklir, Pusat radiasi Batam.    

UTILIZATION OF AMMONIUM HYDROXIDE COMPOUND AS CARBOSORB

Universitas Hasanuddin: e-Journals

Tilization Of Ammonium Hydroxide Compound As Carbosorb For Measurement Of Carbon-14 In Determination Age Of Coral Reef Sample has been performed. The objective of this research is to Determine the age of Coral Sample of Spermonde Islands through Activity Measurements of carbon-14 with LSC (Liquid Scintillation Counting) method. Coral sample were taken from around Langkai Island. The steps of this research are: Sample preparation, CO2 absorption with solution of MEA, DEA and TEA and measurement of carbon-14 activity using Liquid Scintillation Counter (LSC) Hidex 300 SL. Absorption CO2 using ammonium hydroxide. The specific activity of coral sample using carbosorb ammonium hydroxide was 14.43 ± 1,2 DPM/g C. The age of coral sample calculated from the specific activity using carbosorb ammonium hydroxide was 484.63 ± 54 years

Tenrisa’na, A. (Andi)

Zakir, M. (Muhammad)

Maming, M. (Maming)

Neliti

Utilization of Ammonium Hydroxide Compound as Carbosorb

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UTILIZATION OF AMMONIUM HYDROXIDE COMPOUND AS CARBOSORB

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Marina Chimica Acta

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