PRECONCENTRATION AND TRACE ANALYSIS OF Cd(II) BASED ON FLOW INJECTION ANALYSIS USING ION IMPRINTED POLYMERS (IIPs)
Industrialization produced not only useful products but also hazardous waste for the environment. Cadmium is one of heavy metal used fairly widespread in industry and technology, on the other hand it has pollution effect on environment due to its toxicity. Cadmium generally found in a very...
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id-itb.:340782019-02-04T08:40:50ZPRECONCENTRATION AND TRACE ANALYSIS OF Cd(II) BASED ON FLOW INJECTION ANALYSIS USING ION IMPRINTED POLYMERS (IIPs) Asti Rahayu, Martina Kimia Indonesia Theses ion imprinted polymers, cadmium, preconcentration, FIA INSTITUT TEKNOLOGI BANDUNG https://digilib.itb.ac.id/gdl/view/34078 Industrialization produced not only useful products but also hazardous waste for the environment. Cadmium is one of heavy metal used fairly widespread in industry and technology, on the other hand it has pollution effect on environment due to its toxicity. Cadmium generally found in a very low concentration, typically at ?g/L range, therefore preconcentration stage is required for analysis. Ion imprinted polymers (IIPs) is a functional material that has adequate capacity and selective retention for preconcentration purposes. Through polymerization of salicylic acid and formaldehyde in the presence of binary complex Cd(II)-4-(2- pyridylazo) resorcinol, a selective functional material for Cd(II) has successfully synthesized. Salicylic acid and formaldehyde were prepared in a ratio of 1: 8, this higher formaldehyde to salysilic acid ratio is able to increase the ability of polymer retention. Characterization of NIPs, IIPs, and Cd-IPs using FT-IR indicated that NIPs and IIPs polymer have formed as shown as the presence of - CH2-bridge vibration band which is not found in IR spectrum of salicylic acid as monomer. Absorption band shift of C=O and N=N which is found in the Cd-IPs spectrum show that Cd(II) ions has been released from IIPs with addition of EDTA. Characterization of Cd-IPs retention properties synthesized by batch method, the retention capacity was found to be 22.65 mg/g Cd-IPs at pH 5 in 10 minutes contact time. Afterwards, the synthesized Cd-IPs polymer is used in the development of preconcentration tecnique based on flow injection analysis. Cd- IPs that is used as packed column has good thermal stability and reusability; this was confirmed by Thermal Gravimetric Analysis (TGA) and the ability of the polymer to be used repeatedly up to fifty times. Measurements were performed in 2 mL/minute flow rate using water which is acidified using HNO3 until pH 5 as carrier. This method was based on Cd(II) ion retention in Cd-IPs. The retained Cd(II) in Cd-IPs which further eluted quantitatively using EDTA 0.05 M directly to the nebulizer system of atomic absorption spectrometer. This developed method of analysis has been used for determination of cadmium in water samples from the Cidurian River, West Java, Indonesia. The obtained analytical performance is quite good, as shown by the precision values expressed in relative standard deviation of 1.82 (n= 11), detection limit of 16.41 µg/L (S/N= 3), and sensitivity was to be 13.7 ?g/L. Interference test for the presence of other metal ions such as Cu(II), Pb(II), and Zn(II) did not show a significant effect. Enrichment Factor (EF); concentration efficiency (CE) and consumptive index (CI) were found respectively: 15; 5.32 minute-1 and 0.43 mL. The proposed method of this analysis is able to provide fast analysis times, good sensitivity, simplicity of manifold and minimum amount of waste generated in analysis process as its own method of analysis that is reliable and efficient. text |
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Kimia Asti Rahayu, Martina PRECONCENTRATION AND TRACE ANALYSIS OF Cd(II) BASED ON FLOW INJECTION ANALYSIS USING ION IMPRINTED POLYMERS (IIPs) |
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Industrialization produced not only useful products but also hazardous waste for the environment. Cadmium is one of heavy metal used fairly widespread in industry and technology, on the other hand it has pollution effect on environment due to its toxicity. Cadmium generally found in a very low concentration, typically at ?g/L range, therefore preconcentration stage is required for analysis. Ion imprinted polymers (IIPs) is a functional material that has adequate capacity and selective retention for preconcentration purposes. Through polymerization of salicylic acid and formaldehyde in the presence of binary complex Cd(II)-4-(2- pyridylazo) resorcinol, a selective functional material for Cd(II) has successfully synthesized. Salicylic acid and formaldehyde were prepared in a ratio of 1: 8, this higher formaldehyde to salysilic acid ratio is able to increase the ability of polymer retention. Characterization of NIPs, IIPs, and Cd-IPs using FT-IR indicated that NIPs and IIPs polymer have formed as shown as the presence of - CH2-bridge vibration band which is not found in IR spectrum of salicylic acid as monomer. Absorption band shift of C=O and N=N which is found in the Cd-IPs spectrum show that Cd(II) ions has been released from IIPs with addition of EDTA. Characterization of Cd-IPs retention properties synthesized by batch method, the retention capacity was found to be 22.65 mg/g Cd-IPs at pH 5 in 10 minutes contact time. Afterwards, the synthesized Cd-IPs polymer is used in the development of preconcentration tecnique based on flow injection analysis. Cd- IPs that is used as packed column has good thermal stability and reusability; this was confirmed by Thermal Gravimetric Analysis (TGA) and the ability of the polymer to be used repeatedly up to fifty times. Measurements were performed in
2 mL/minute flow rate using water which is acidified using HNO3 until pH 5 as carrier. This method was based on Cd(II) ion retention in Cd-IPs. The retained Cd(II) in Cd-IPs which further eluted quantitatively using EDTA 0.05 M directly to the nebulizer system of atomic absorption spectrometer. This developed method of analysis has been used for determination of cadmium in water samples from the Cidurian River, West Java, Indonesia. The obtained analytical performance is quite good, as shown by the precision values expressed in relative standard deviation of 1.82 (n= 11), detection limit of 16.41 µg/L (S/N= 3), and sensitivity was to be 13.7 ?g/L. Interference test for the presence of other metal ions such as Cu(II), Pb(II), and Zn(II) did not show a significant effect. Enrichment Factor (EF); concentration efficiency (CE) and consumptive index (CI) were found
respectively: 15; 5.32 minute-1 and 0.43 mL. The proposed method of this analysis is able to provide fast analysis times, good sensitivity, simplicity of manifold and minimum amount of waste generated in analysis process as its own method of analysis that is reliable and efficient.
|
format |
Theses |
author |
Asti Rahayu, Martina |
author_facet |
Asti Rahayu, Martina |
author_sort |
Asti Rahayu, Martina |
title |
PRECONCENTRATION AND TRACE ANALYSIS OF Cd(II) BASED ON FLOW INJECTION ANALYSIS USING ION IMPRINTED POLYMERS (IIPs) |
title_short |
PRECONCENTRATION AND TRACE ANALYSIS OF Cd(II) BASED ON FLOW INJECTION ANALYSIS USING ION IMPRINTED POLYMERS (IIPs) |
title_full |
PRECONCENTRATION AND TRACE ANALYSIS OF Cd(II) BASED ON FLOW INJECTION ANALYSIS USING ION IMPRINTED POLYMERS (IIPs) |
title_fullStr |
PRECONCENTRATION AND TRACE ANALYSIS OF Cd(II) BASED ON FLOW INJECTION ANALYSIS USING ION IMPRINTED POLYMERS (IIPs) |
title_full_unstemmed |
PRECONCENTRATION AND TRACE ANALYSIS OF Cd(II) BASED ON FLOW INJECTION ANALYSIS USING ION IMPRINTED POLYMERS (IIPs) |
title_sort |
preconcentration and trace analysis of cd(ii) based on flow injection analysis using ion imprinted polymers (iips) |
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