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grafting of chitin by irradiation technique
grafting of chitin by irradiation technique
grafting of chitin by irradiation technique
grafting of chitin by irradiation technique
grafting of chitin by irradiation technique
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grafting of chitin by irradiation technique

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Studies on radiation grafting of hydrophilic monomer onto chitin for ion exchange application were examined . Over the past several years , chitin has been receiving increased attention for its …

Studies on radiation grafting of hydrophilic monomer onto chitin for ion exchange application were examined . Over the past several years , chitin has been receiving increased attention for its application such as ion exchange . They are utilized scarcely because of problems associated with poor solubility, hidrophilicity and low reactivity. Graft copolymerization induced by irradiation is one of the methods for chitin modification in order to improve its properties such as hydrophilicity and reactivity. The aim of this research is to increasing the ability of chitin as ion exchange for heavy metal adsorbent.

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  • 1. IRRADIATION GRAFTING OF HYDROPHYLIC MONOMER ONTO CHITIN FOR ION EXCHANGE APPLICATION Gatot Trimulyadi Rekso Center for Research and Development of Isotopes and Radiation Technology Jl . Lebakbulus raya No 49, Jakarta 12240, INDONESIA Fax 62 21 7691607, E-Mail : Gatot2811@yahoo.comAbstract: Studies on radiation grafting of hydrophilic monomer onto chitin for ion exchange application wereexamined . Over the past several years , chitin has been receiving increased attention for its application such asion exchange . They are utilized scarcely because of problems associated with poor solubility, hidrophilicity andlow reactivity. Graft copolymerization induced by irradiation is one of the methods for chitin modification inorder to improve its properties such as hydrophilicity and reactivity. The aim of this research is to increasing theability of chitin as ion exchange for heavy metal adsorbent. The hydrophilic monomers used were acrylic acidand acryl amide. In the present experiment , the pre-radiation per oxidized method was employed . Theirradiation of sample was carried out in Co-60 gamma irradiation source at room temperature . The monomerssolutions acrylic acid or acryl amide than introduce into irradiated chitin and the graft polymerization wascarried out in nitrogen atmosphere. The presentation of grafting has been determined as a variation of monomerconcentration and temperature as a function of time of reaction. The grafted chitin obtained was washed anddried in vacuum and the percentage of grafting was measured by gravimetric method . Measuring the capasity ofadsorption of grafted chitin to Cr, Cu and Hg metal ion was determined by using AAS and CV AAS. The resultshows that using acryl amide give percentage of grafting higher compare with acrylic acid. The presence ofmonomer grafted onto chitin is demonstrated by FTIR spectrum with the appearing of carbonyl functional group.Chitin grafted with acrylic acid give a higher rate of adsorption of metal ion Cr, Cu and Hg compare grafted withacryl amide. The high rate of adsorption is for metal ion Hg it was found 294.3 mg/g for chit-g-Aac and 257.3mg/g for Chit-g-Aam.Keywords : Chitin, irradiation, grafting, ion exchangeINTRODUCTION. The adsorption behavior of chitin and its concerns In order to solve the environmental problem due with various degree of deacetylization. This highto industrial development, many factor have been adsorption capacity was ascribable primarily to itsstudied . Generally, both solid and liquid industrial remarkable hydrophilicity in cooperation with thewaste can make seriously environmental problems. relatively high amino group content. It is indicate that the importance of hydrophlicity and suggestThe liquid waste with the heavy metal content in the that , in order to develop adsorbents of high capacity ,large scale of production can be hazardous to it is make indicate the importance of hydrophilicityenvironmental conditions. Separation method of essential to make chitin derivatives highlyheavy metal using ion exchange adsorbent to adsorb hydrophylic and yet insoluble in water. Chitosan ismetal ion should be cheap, simple and industrial natural polysaccharide and has the same skeletonuseful in waste treatment. The natural chelating structure as cellulose, by a radiation modificationmarine polymer chitin, poly(N-acetyl-D- such as graft-co polymerization of hydrophilicglucosamine) and its deacetylated derivative monomer expected to improve its hidrophilicity.andchitosan is useful for removing heavy metal ion performance for application as an ion exchangewaste from discharge water . Chitin , the most adsorbent. In the field of Radiation Process, freeabundant naturally is undoubtedly one of the most radical formation is the key role of the modificationpromising and attracting resources present in technique. Graft modified of chitosan withquantity. Among some interesting properties of hydrophilic functional monomers was suitablechitin , chelating ability arising from its characteristic method to develop its as ion exchange adsorbent.structure is especially noteworthy. Many researchershave explored the feasibility of this approach. In this present study, the purpose of theKurita.K et.,all, conducted experiments with a experiments is to study graft-copolyimerizationnumber of heavy metals. reactions as well as to study the chemical and the 1
  • 2. physical properties of grafted chitin. Hydrophilicmonomers such as acrylic acid, and acryl amide willbe employed for these experiments. The functionalgroup of graft –copolymers is expected to be usefulin the attaching test of metal ions. of graft yield was calculated from the difference in weight ;II. EXPERIMENTAL. Graft yield = ( Wg - Wo ) / Wo x 100 %Material and Experiment: Chitin extracted from Where Wo and Wg are the weight before and afterprawn shell (Penaeus Monodon), it was got from grafting.Muara Karang , North Jakarta. The were initiallywashed by water and then dried at 800 C overnightand conditioned at room temperature for 24 hr. Measuring off adsorption of metal ions by chitinAcrylic acid monomer, and white crystalline powder and its modified : The experiment was done withof acryl amide , obtained from E Merck , and other chitosan with degree of the deacetylization of 78,5 %chemicals of reagent grade were used without and modified chitin were Chitin-g-Aac and Chitin-g-purification. Aam with degree of grafting 32,4 % and 45,6 % and modified chitosan were chitosan-g-Aac and ChitosanRadiation Source : Gamma radiation source of –g-Aam were got from deacetylated modified chitin.Co-60, IRKA batch irradiator , with irradiation dose Measuring the rate of adsorption about 100 mg ofrate about 9,0 kGy/hr was employed in these powder material (chitin,chitosan and it’sexperiments. This radiation source is located at Pasar modifications) equilibrated with 100 ml 0f solutions (Jumat, Center for Research and Development of HgSO4 , CuSO4.5 H2O, K2Cr2O7) 0,1 M, at pH 4,0Isotopes and Radiation Technology, Jakarta, and stirred for 60 min. The metal ion uptakeIndonesia. concentrated after equilibrating were determined byGrafting reaction: In the present experiment, the pre using AAS and for Hg(II) using CV-AAS.irradiation graft co polymerization method wasemployed. In this method a sample of chitin powderof about 500 mg , was put into a glass tube, then III. RESULTS AND DISCUSSIONirradiated in air atmosphere at room temperature. Amonomer acryl amide solution was deairated by Evidence of grafting : The increase in weight of thebubbling with nitrogen gas, then introduced into the extracted grafted sample, as compare with that thepre irradiated sample and the graft polymerization original chitin and their FTIR spectra , was used aswas carried out in a nitrogen atmosphere at certain evidence of grafting. The FTIR spectra of chitin andtempera-ture. The grafted chitin obtained was grafted chitin are shown in Fig 1. It can be seen thatwashed toughly with aquadest and soaked overnight a band around at 1660 cm –1 arises from carbonylin aquadest, then subjected to sox let extraction with absorption of chitin and anew band appear at 3400methanol for 8 hours to extract homopolymer. The cm-1 which correspond to the hydroxyl absorption ofgrafted chitin then was dried in vacuum until they grafted chitin with acrylic acid and at 3500 cm -1 isreached a constant weight at 500 C. The percentage asymmetric stretching of NH2 for grafted chitin with acrylamide. 2
  • 3. chitin powder and the solubility of the monomer , acryl amide monomer is good soluble in water- methanol solvent . By using acrylic acid or acryl amide concentration above 30 % , high percentage of grafting was obtained. However . the increase in percentage of grafting is followed by increase of homopolymerization, which is difficult to separate. The result shows that the different on percentage of grafting for reaction period of 3 hr and 4 hr is not significant. It can be concluded that the optimum monomer concentration is 30 % with 3 hr reaction period. 100 Acrylic acid 10 % Acrylic acid 20 % ) % g n t f ar g f o e g at n e c e P 80 Fig 1. The FTIR spectra of the original chitin ( Acrylic acid 30 % i 60 Acrylic acid 40 % 40 20 0 0 1 2 3 4 5 6 Reaction time (hr) Fig 3. Effect of acrylic concentration on percentage of grafting 160 10 % Acrylamide 140 Degree of grafting (% ) 20 % Acrylamide 120 30 % Acrylamide 100 40 % AcrylamideFig 2. The FTIR spectra of chitin grafted with acrylic acid 80 monomer 60Effect of monomer concentration and reaction time. 40The effect of acrylic acid and acryl amide monomer 20concentration on the percentage of grafting withreaction period of 1 hr, 2 hr, 3 hr and 4 hr are 0presented on Figure 2 and 3 . It can be seen that the 0 60 120 180 240 300percentage of grafting is independent of the monomerconcentration. Grafting with acryl amide monomer Reaction time (min)give higher yield percentage of grafting compare withacrylic acid monomer. This may results in Fig 4. Effect of acrylamide concentration on percentage ofenhancement of the monomer diffusion into the grafting 3
  • 4. From the figure 5 and 6, it is oblivious that the degree of grafting is largely by the reaction Grafting temperature . The reaction temperature temperature . The higher temperature the higher of play a great role on the grafting process because this degree of grafting obtained. The reason is that the influence on the diffusion of monomer into the increase in temperature improves the monomer matrix polymer of chitin and also on the lifetime of diffusibility as well as the mobility of the monomer. the peroxide radical in the preirradiated chitin. Figure It is recommended that the optimum reaction for this 5 and 6 shows the degree of grafting time curves for grafting system is 70 0 C more than that the increasing the grafting of aqueous of 30 % acrylic acid of degree of grafting is not so much, there is a monomer and 30 % of acrylamide at various nearly constant value. temperature reaction 100 Temp 50 C The ion exchange adsorption of metals ions by grafted chitin and its derivatives. The adsorptionP e rc e n ta g e o f g ra ftin g (% ) 80 Temp 60 C behavior of the resulting grafted chitin with acrylic Temp 70 C acid and acryl amide was examined in comparison 60 with the original chitin and chitosan. The results are Temp 80 C illustrated in Table 1 . 40 Tabel 1. The capacity of adsorption of some 20 metal ions ( mg/gr) by chitin, chitosan and grafted chitin/ chitosan 0 0 1 2 3 4 5 6 The capacity of adsorption Time of reaction (hr) ( mg / g) Fig 5. Effec of time reaction on percentage of grafting of Materials acrylic acid at various temperature reaction Hg(II) Cr(VI) Cu(II) 200 Chitin 92,6 30,6 24,4 React. Temp 50 C Chitosan 174,5 48,4 44,2 Degree of grafting (%) 160 React. Temp 60 C Chitin-g-Aac 294,3 109,5 180,1 React. Temp 70 C 120 React. Temp 80 C Chitin-g-Aam 257.3 94,8 154.6 80 Chitosan-g-Aac 488,9 318,5 362,8 Chitosan-g-AAm 464,2 325,8 398,2 40 0 0 60 120 180 240 300 These results clearly show that chitin modified as Reaction time (min) chitin grafted acryl amide have higher capacity of Fig 6. Effec of time reaction on percentage of grafting of adsorption for ion metal such Hg, Cr, and Cu. The acrylamide at various temperature reaction highest one is for metal ion Hg both grafting with acrylic acid or acryl amide. The chitin modified have an excellent adsorption capacity due to the advantageous location of -OH and –NH2 group in 4
  • 5. the molecule of chitosan to form complex formationand functional group of monomer act as ionexchanger for ions metal.IV. CONCLUSION  Using acryl amide give percentage of grafting higher compare with acrylic acid.  The presence of monomer grafted onto chitin is demonstrated by FTIR spectrum with the appearing of carbonyl functional group.  The optimal condition of monomer acrylic acid or acryl amide concentration was 30 %, temperature 700 C and reaction period of 3 hours.  Chitin grafted with acrylic acid give a higher capacity of adsorption of metal ion Cr, Cu and Hg compare grafted with acryl amide.  The high rate of adsorption is for metal ion Hg it was found 488,9 mg/g for chitosan-g- Aac and 464,2 mg/g for Chitosan-g-Aam.References[1]. Goosen, M.F.A., Application of Chitin andChitosan, Technomic Publishing Company, Inc,Lancaster, Pennsylvania, USA. 1997,.[2] Chapiro, A., Radiation Chemistry of PolymericSystem. Willey Inter-science, New York, 1962.[3] Kurita, K; Koyama,Y ; and Taniguchi, A.Journal of Applied Polymer Science. 1986 , 31, 1169 – 1173 5

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