Abstract & References Vol 25 No 6 (2021)

Malaysian Journal of Analytical Sciences Vol 25 No 6 (2021): 895 - 910

DETERMINATION OF SODIUM HYDROXIDE CONCENTRATION UNDER HETEROGENEOUS CONDITIONS FOR THE PREPARATION OF N-CARBOXYMETHYL CHITOSAN

(Penentuan Kepekatan Natrium Hidroksida dalam Keadaan Heterogen bagi Penghasilan N-Karboksimetil Kitosan)

Nurul Adilah Rodzali and Nadhratun Naiim Mobarak*

Department of Chemical Sciences, Faculty of Science and Technology

Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor, Malaysia

*Corresponding author: nadhratunnaiim@ukm.edu.my

Received: 3 September 2021; Accepted: 27 October 2021; Published: 27 December 2021

Abstract

N-carboxymethyl chitosan (N-CMC) is one of the promising chitosan derivatives which has been used to improve the limitation of chitosan and can be synthesized via direct alkylation in the presence of base. In this work, the effect of sodium hydroxide concentration under heterogeneous conditions has been investigated to obtained N-CMC. The concentration of sodium hydroxide (NaOH) was varied from 1.5 M to 7.5 M. This research showed that the substitution site of chitosan is affected by the concentration of NaOH. The results revealed that N-CMC was successfully synthesized at higher NaOH concentration, 6.0 M, and 7.5 M under heterogeneous conditions. The presence of peak at 1321 cm^-1 and 3.2 ppm from Fourier transform infrared (FTIR) and ¹H nuclear magnetic resonance (NMR) spectroscopy, respectively, proving the carboxymethyl group substitution occurred at amino (NH₂) site. X-ray diffraction (XRD) analysis showed insignificant differences in degree of crystallinity of N-CMC at both NaOH concentrations. However, Thermogravimetry analysis (TGA) and differential scanning calorimetry (DSC) revealed that obtained N-CMC possessed distinct thermal properties as the glass transition temperature of 6.0 M was lower than 7.5 M NaOH. Therefore, the selection of NaOH concentration in N-CMC production must be determined according to the intended functional application.

Keywords: N-carboxymethyl chitosan, N-substitution, heterogeneous conditions, NaOH concentration

Abstrak

N-karboksimetil kitosan (N-CMC) merupakan salah satu terbitan kitosan yang telah digunakan bagi menambahbaik kekurangan kitosan dan boleh disintesis melalui pengakilan secara terus dengan kehadiran bes. Dalam kajian ini, kesan kepekatan natrium hidroksida (NaOH) dalam keadaan heterogen telah dikaji untuk menghasilkan N-CMC. Kepekatan natrium hidroksida (NaOH) dibezakan daripada 1.5 M hingga 7.5 M. Kajian ini menunjukkan tapak penggantian pada kitosan dipengaruhi oleh kepekatan NaOH. Hasil kajian menunjukkan N-CMC telah berjaya disintesis pada kepekatan yang lebih tinggi, 6.0 M and 7.5 M dalam keadaan heterogen. Kehadiran puncak pada 1321 cm^-1 dan 3.2 ppm masing-masing pada spektroskopi inframerah transformasi Fourier (FTIR) dan resonans magnet nukleus ¹H (NMR), membuktikan penukargantian kumpulan karboksimetil berlaku pada tapak amina (NH₂). Analisis pembelauan sinar-X (XRD) menunjukkan perubahan yang tidak ketara bagi darjah kehabluran N-CMC pada kedua-dua kepekatan NaOH. Walau bagaimanapun, analisis termogravimetri (TGA) dan kalorimetri pengimbasan pembezaan (DSC) menunjukkan N-CMC yang dihasilkan mempunyai sifat terma yang berbeza dimana suhu peralihan kaca bagi 6.0 M lebih rendah berbanding 7.5 M NaOH. Oleh itu, pemilihan kepekatan NaOH dalam penghasilan N-CMC ditentukan berdasarkan aplikasi yang akan digunakan.

Kata kunci: N-karboksimetil kitosan, penggantian-N, keadaan heterogen, kepekatan NaOH

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