RINGKASAN PENGEMBANGAN ELEKTRODA SELEKTIF ION TIMBAL(II) TIPE KAWAT TERLAPIS YANG SEDERHANA DAN MURAH SEBAGAI SENSOR POTENSIOMETRI LINGKUNGAN LOGAM BERAT TIMBAL(II) Peneiitian ini dilakukan untuk mengembangkan suatu prototipe elektroda selektif ion timbal(II) sebagai anion PbCXt2" tipe kawat terlapis yang dapat digunakan sebagai sensor potensiometri lingkungan dari iogam berat timba}(II) di lingkungan yang akurat, cepat, sederhana, dan murah. Pemantauan pencemaran Pb dalam iingkungan sangat penting daiam mewujudkan keamanan iingkungan di Indonesia karena iogam Pb merupakan eiemen stabil (non biodegradable) yang sangat toksik bagi manusia dan hewan karena menimbulkan efek negatif pada susunan syaraf pusat, sistem reproduksi, pencernaan, sistem pembuiuh darah jantung serta ginjal. Konsentrasi Pb dalam darah > 10/dL dapat menimbuikan penurunan kecerdasan dan penurunan perkembangan syaraf anak-anak. Tujuan dari penelitian ini adalah mengembangkan pembuatan elektroda tipe kawat terlapis yang selektif terhadap ion timbal(II) sebagai anion PbCI42" serta dapat digunakan sebagai metoda altematif untuk mendeteksi kadar logam berat timba!(II) di lapangan yang akurat, sederhana, cepat dan murah. Penelitian ini diseleseikan dalam waktu 2 tahun. Pada tahap pertama diselesaikan beberapa tahap pekerjaan penelitian yang meliputi: (1) membuat konstruksi elektroda selektif ion (ESI) timba!(II) tipe kawat teriapis yang terdiri dari: badan elektroda, membran dan kabel koaksial RG-58 sebagai penghubung ESI ke alat potensiometer, (2) mengkarakterisasi sifat dasar ESI timbal(II) sebeium diaplikaakan untuk pengukuran Pb(II) di lapangan guna mengetahui kualitas parameter operasionalnya^B) mengaplikasikan ESI Pb(II) pada analisis Pb(II) sebagai anion PbCI42- daiam air iimbah buatan secara potensiometri yang hasilnya dibandingkan dengan metoda baku spektrofotometri serapan atom (MS), Parameter yang dibandingkan adalah sensitivitas metoda, kesalahan yang diberikan serta kemudahan dalam peiaksanaan analisis. Hasil penelitian menunjukkan bahwa ESI Pb(II) bermembran dengan komposisi (% berat) 4% metilfrioktilamoniumtetrakloFOplurnba^II^SO^/o PVQ65,5% DBP, 0,5% D2EHPA dalam pelarut THF (1:3 % b/v) yang dilapiskan pada kawat platina berdiameter 0,5 mmm dan dihubungkan langsung ke alat potensiometer oleh kabei koaksial RG-58 menunjukkan ukuran keeii, konstruksinya sederhana, mempunyai reprodusibilitas pembuatan yang baik, memiiiki karakter optimal untuk pengukuran anaiis timbal(II) sebagai anion PbCI42" secara potensiometri pada penentuan timbal(II) daiam air fimbah buatan pada konsentrasi 0,1-103 ppm dengan kesalahan 0,04-3,8% dapt menggantikan metoda spektrofotometri serapan atom (SSA) yang memberikan kesalahan 0,1-1,62%. Penelitian tahap kedua bertujuan untuk menguji sensor (ESI) Pb(II) tipekawat teriapis hasil pembuatan tahap pertama pada penentuan timbal(II) daiam sampe! air sumur, air limbah industri dan air sungai sepanjang DAS Brantas huiu serta sampei udara di kota Malang yang hasilnya dibandingkan dengan metoda baku SSA pada kondisi optimal Sampei air sumur diambil dari daerah Kiayatan (K) dan Sumbersari (S), sampei air limbah industri electroplatingdiambil dari daerah Landungsari (L) dan Blimbing ("0 dengan teknik pengambilan pada saat survey. Sampei air sungai diambil dari 10 titik aliran DAS Brantas berdasarkan lebar dan kedalaman sungai Brantas yakni: (1) Sumber Brantas ,(2) Dam Coban Ta!un, (3) Jembatan Brantas Batu, (4) Jembatan Pendem, (5) Jembatan Dinoyo, (6) Jembatan Bumiayu, (7) Jembatan Kedung Pedaringan, (8) Up Stream Dam Sengguruh, (9) Jembatan Sengguruh dan (10) Waduk Karangkates, ilakukan pada aliran sungai samping kiri, tengah dan
kanan pada tiap-tiap daerah sampling pada saat survey. Hasil penentuan timbal(II) pada kedua metoda SSA maupun potensiometer menggunakan sensor Pb(II) dilkukan uji presisi dan akurasi.Dari hasil penelitian ini diperoSeh bahwa ESI PbCL,2" tipe kawat teriapis dapat digunakan sebagai sensor ion Pb(II) dalam sampe! air iimbah industri, air sumur dan air sungai DAS Brantas hulu serta sampei udara di daerah kota/kabupaten Malang pada rentang konsentrasi 0,0364 - 2,32 ppm memberikan ketepatan sebesar 96,3% dan keteliban sebesar 99,0%.Hasil peneiitian menyatakan bahwa sensor ion Pb(II) yang dibuat dapat digunakan sebagai metoda aiternatif disamping metoda spektrofotometri serapan atom di lapangan untuk penentuan air (iimbah industri,sumur, sungai DAS Brantas) serta udara dengan memberikan kesalahan sebesar 3,7% serta memiliki kelebihan cepat, mudah dan murah dsbandingkan metioda spektrofotometri serapan atom (SSA)
SUMMARY DEVELOPMENT OF A SIMPLE AND CHEAP COATED WIRE LEAD ION SELECTIVE ELECTRODE AS A POTENTIOMETRIC SENSOR ENVIRONMENTAL OF HEAVY METAL LEAD(II) The research has been done in order to develop a prototype coated wire lead(H) as PbC!42' anion selective electrode wich is can be used as an environmental potentiometric sensor of lead(II) wich is has relatively fast response, simplicity, speed, and low cost Monitoring lead(II) in environment is urgent need in order to make safety environment in Indonesia , bacause lead is an extremely stable element categorized as a heavy metals. It is very toxic to human and animals, because lead can adversely affect the developing nervous system in children at > 10 jxg/dL in blood, including learning disabilities and reduced fertility in women The aim of the research is to deveiope preparation of coated wire electrodes (CWE) wich are selective to lead(II) ion as PbCU2" anion and can be used as alternative methods to determine the lead level in the field analysis. T his research was conducted on 2 years. The objective of the first phase study were: (1) making coated wire lead(II) ion selective electrode (lead(II) CWE) construction consit of electrode's body, membrane and coaxial cable to join iead(II) CWE to a potentiometer, (2) to characterize the basic properties of lead(II) ion selective electrode (ISE) before their application to measuring lead(II) ion in field analysis in order to be able to know their operational parameters quality, (3) application these iead(II) ion CWE in artificial wastewater potentiometric analysis and their result compare to the atomic absorption spectrophotometric standard method. The parameter to be compare are: sensitivity, accuracy and ease of preparation and procedures. The result showed that these iead(II) ton CWE base on membranes composition found was 30,0 wt.% of powdered PVC, 65.5 wt% of plastlcizer DBP and 4wt% of the corresponding ionophore (Aiiquat 336-PbC!4), 0.5 wt% of D2EHPA dissolved in tetrahydrofuran (THF) solven (1:3 w/v) and deposited directly onto a platinum wire approximately 0.5 mm in diameter whose tip had been melted in flame to form a spherical button was soldered to a length of RG-58 coaxial cable to a potentiometer showed have: a small size, simple configuration, It was found to be reproducible, have a optimum characteristic for potentiometric sensor lead(II) ion as PbG42' anion in artificial wastewater in concentration ranging of 0, 135 103 ppm replace to the spectrophotometric method resulting in the error of 0.1-1.62%. The aim of the second phase study is to examine the fead(II) ion sensor (ISE) as coated wire lead(II) selective electrode which constucted in the first phase study on measuring PbCl4 ion in natural water, wastewater and Brantas river water and air sample anlysis at Malang city and their result were compared to the atomic absorption spectrophotometric standard method in optimum condition. The weSJ water samples taken from Kiayatan (K) and Sumbersari (S) area, the electroplating industrial wastewater samples taken from Landungsari (L) and Blimbing (T) covered when taking the survey. River water samples taken from 10 points on the flow of upstream of the Brantas river basin base on width and depth of the river Brantas namely: (1) Source Brantas, (2) Dam Coban Copenhagen, (3) Stone Bridge Brantas, (4) Bridge Pendem, (5) Bridge Dinoyo, (6) Bridge Bumiayu, (7) Bridge Kedung Pedaringan, (8) Up Stream Dam Sengguruh, (9) Bridge Sengguruh and (10) Reservoir Karangkates. The water samples covered from the left side, center and right of the river flow in each sampling area at the time of survey.
The results of determination of lead(II) on both the SSA and the potentiometric method using sensors Pb (II) tested for their accuracy and precision. From the research results obtained tihat coated wire iead(II) as PbC!42~ anion selective electrode can be used as sensors ions Pb (II) in industrial waste water samples, well water and river water upstream of the Brantas river basin and air samples in the town / district of MaSang on the concentration range 0.0364 - 2.32 ppm provides accuracy of 96.3% and accuracy of 99, 0%. The research result states that the ion sensors Pb (II) which can be used as an alternative method in addition to atomic absorption spectrophotometry methods in the field for determination of water (industrial waste, wells, river Brantas river basin) and air to give an error of 3.7% and has the advantage quick, easy and inexpensive compared to the atomic absorption spectrophotometry method (SSA)
DAFTAR PUSTAKA 1.
Agus Pratama Sari, Trmbal, Polutan yang pertama harus dibuang, Jakarta ,Kompas Cyber Media, 21 September 2002 2. Anonlm (2000), Pengkajian Surnber-Sumber Pencemar Logam Berat cfi Wiiayah Kail Surabaya., BAPEDALDA Tsngkat I Uawa Timur dan Lembaga Persgabtfian MasyarakatlnstitutTeKncAogi SepuUih Nopember Surabaya 3. Ardakany/M,AA.Ensafi,/ H.NaeimL, A, Dastanpoa, A.Shamili (2003), Coated WireBased, New Scniff Base PotentJornetric Sensor for Lead(II) Ion, Russian Journal ofElectrochemistry, 39,269-275 4. Buck R.P., E. Lindner (2001), Tracing tiie history of SelecHve ion sensor, Anal.ChemJF&sruarf, 88A-97A 5. Biihlmann, P., M, Hayakawa., Tf Ohshiro., S, Amemiya dan Y, Umezawa (2001), Influence of natural, electrically neutral Hplds on the pofcendometric responses of cation-seiective polymeric membrane electrodes, Anal.Qiem, 73, 3199-3205 6. Clifford,D dan X.LJu (1993), Ion exchange for Pb(II) removal, journaf AWWA, Apn\, 135-143 7. Cognis, C, 2006, Aliquat 336, http://www.cognis.com, tanggai akses: 14 April 2006 8. Environmental Protection Agency (EPA), 1996, Environmental Monitoring System Laboratory, Methods for Chemical Analysis of Water and 9. Environmental Protection Agency (EPA), 2002, Short Term Methods for Estimating the Chronic Toxiciiy of Effuent and Receiving Waters to Freshwater Organism, 4 th Edition, Washington DOEPA 10. Evans, K, 1991, PotantfomebY and Ion Selective E/ectwdes, 3ohn Wiley and Sons, New York, 1987, pp 66 - 67 11. Fardiaz, Srikandi, (1992), Polls! Air dan Pofus! Udara, PAUrIPB 12. Fergusson,33Ck E., 1991, The Heavy Elements, Chemistry, EnvironmentalImpact and Health Effect, Qxford:Pergamon Press 13. XUPAC, 2006, General Terms Relevant to Ion-Selective Electrode, IUPAC Compendium of Chemical Technology, http://wvwv.iupac.org/publications/anaiytical compendium/Cha08sec321. pdf,, tanggal akses : 29 Mei 2006 14. KLH, 1995, Saiinan Keputusan Menteri Ungkungan Hidup mengenai Baku Mutu Umbah Industry Departemen Ungkungan Hidup 15. Kompas-cetak,Hurnaniora ,9 Februari,2004 16. Kobayashi,F.f T. Maki., Y,, Nakamura., and SC, Ueda (2005), Determination of Cu,Pb,Fe and Zn in piant Component of a Hyperaccumulating Piant,^®5^?ia/ Scfencef21,l553-1556 17. Logan,T, 2006, Lead Contamination in environmental www EPA/USAOhi Agricultur Research and Development Center
18. Lynde, 5,A, 1997, Environmental Sampling and Monitoring http://cwr.cee.vt.edu/environmenta!/teach/smprimer/ise/ise.html, tanggai akses : 10 Juni 2006 19. Nielsen, HJ., and Hansen, E.H, (1976), New Nitrate Ion-Selective Electrodes Based on Quarternary Ammonium Compounds in Nonporous Poiymer Membranes, Anal. Chim. Ada, 85,1-16 20. Orion Research,Inc 1997, Web Sits Index.http://www.Orionres.com diakses pada tanggai 18 Agustus 2006 21. Perge,E., R.E., Gyurcsanyi, K., Toth and E., Lindner (2001), Picomofar Detection Limits with Current-Pofarized Pb2+ ion Selective Membranes, AnaLChem,73^,42494253 22. Qian,Q., CS.Wilson, K.BJames, H.H.Girault (2001), Micro ITIES detection of Pb(II)e by facilitated ion transfer, Anal.Chem., 73, 497 - 503 23. Rundie, G, 2000, Measuring Procedure, Chapter 9, www.nico2000.net, tanggai akses 9 Maret 2006 24. SuharmiatL, MutiatkumA, (1995), Penentuan Tingkat Pencemaran Logam Berat Tlmba! dalam Air Sungai, Cermin Dun/a Kedokteran, 103,35-38 25. Tatyana,A., 3, Kim., T.H, Harmon (2005), Development and environmental application of Pb(II) selective microsensor based on doped pofypyrole films, Sensors and Actuators R, 106, 512-517 26. Wang,}., (2002), Real-time electrochemical monitoring : toward green analytical chemistry, Ar,<3te/?7,/te£,35,8i 1-816 27. Wikipedtaf20(feXe3dfII)chloride,http://www.wikipeciia.orq/vviki/Lead%28I I%29 chloride, diakses tanggaf 13 3uif 2006 28. Wrobiewskl, W., 2005, Ion Selective Electrodes, http://www.csrq.ch..pw.edu.plf tanggal akses: 14 April 2006 29. Zanjanchi,MAf A.Arvand., M. AkbarL, K. Tabatabaeian., G. Zaraei, 2006, Perchlorate-SelectJve polymeric Membrane Electrode Based on a Cobaloxime as Suitable Carrier, Sensors and Actuators 4113,304-309
