Malaysian
Journal of Analytical Sciences Vol 20 No 3 (2016): 531 - 538
DOI:
http://dx.doi.org/10.17576/mjas-2016-2003-10
INFLUENCE
OF CHROMIUM ON THE REDUCTION BEHAVIOR OF FERRIC OXIDE BY USING CARBON MONOXIDE:
TEMPERATURE PROGRAMMED REDUCTION AND KINETIC STUDIES
(Pengaruh
Kromium Terhadap Kelakuan Penurunan Ferik Oksida dengan Menggunakan Karbon
Monoksida: Kajian Penurunan Suhu Berprogram dan
Kinetik)
Tengku Shafazila Tengku Saharuddin1*, Alinda Samsuri1,2,
Fairous Salleh1, Mohammad Bin Kassim1,
Rizafizah Othaman1, Mohamed Wahab Mohamed Hisham1, Mohd
Ambar Yarmo1
1School of Chemical Science and Food Technology,
Faculty of Science and Technology
Universiti
Kebangsaan Malaysia, 43600 UKM Bangi, Selangor, Malaysia
2Centre for Defence Foundation Studies,
Universiti
Pertahanan Nasional Malaysia, Kem Sungai Besi, 57000 Kuala Lumpur, Malaysia
*Corresponding author: tengkushafazila@gmail.com
Received: 24
February 2015; Accepted: 27 October 2015
Abstract
This study was undertaken to investigate
the effect of chromium on the reduction behaviour of ferric oxide with carbon
monoxide (10 %, v/v) in nitrogen as a reductant. Ferric oxide was impregnated
with 3 % chromium to produce chromium-doped ferric oxide (Cr-Fe2O3).
The reduction behaviour and the kinetic studies of Cr-Fe2O3
and Fe2O3 have been studied by temperature programmed
reduction (TPR) and the phases formed of partially and completely reduced
samples were characterized by X-ray diffraction spectroscopy (XRD). Meanwhile,
the activation energy values were calculated from the Arrhenius equation using
Wimmer’s method. TPR results indicate that the reduction of Cr-Fe2O3
proceeded in two reduction steps (Fe2O3 → Fe3O4
→ Fe), while, Fe2O3 proceeded in three reduction steps (Fe2O3
→ Fe3O4 → FeO →
Fe) with doped ferric oxide showed a large shifted towards lower temperature. The
complete reduction of ferric oxide to metallic Fe occur at 700 °C compared to
the undoped ferric oxide (900 °C). The XRD pattern showed that the diffraction
peaks of Cr-Fe2O3 are more intense compare to Fe2O3,
indicating that the improvement on the crystallinity of the characteristic
peaks of Fe2O3 with no additional peak observed meaning that
the chromium particles loaded on the ferric oxide were well dispersed.
Furthermore, additional of 3 % chromium
on ferric oxide gives larger surface area and decrease in the activation
energy up to 12.39 % regarding to transition phases of Fe2O3
→ Fe3O4 during the reduction process may also led to the
increase in the rates of ferric oxide reduction.
Keywords: temperature
programmed reduction, kinetic, reduction, ferric oxide, chromium, carbon monoxide
Abstrak
Kajian ini dijalankan untuk melihat pengaruh kromium
pada kelakuan penurunan ferik oksida di mana karbon monoksida (10%, v/v) di
dalam nitrogen digunakan sebagai agen penurunan. Serbuk ferik oksida yang
didopkan pada kromium (Cr-Fe2O3) disintesis menggunakan
kaedah impregnat. Kelakuan penurunan dan kinetik oleh Cr-Fe2O3
and Fe2O3 dikaji menggunakan
teknik suhu penurunan berprogram (TPR) dan fasa - fasa yang terbentuk bagi
separa dan penurunan penuh dicirikan menggunakan teknik pembelauan sinar X (XRD)
sementara nilai - nilai tenaga pengaktifan dikira daripada persamaan Arrhenius
dan kaedah Wimmer. Profil TPR menunjukkan bahawa penurunan ferik oksida yang didopkan
kromium melalui dua langkah tindak balas penurunan (Fe2O3
→ Fe3O4 → Fe) manakala ferik oksida yang tidak didopkan
melalui tiga langkah tindak balas penurunan (Fe2O3 → Fe3O4
→ FeO → Fe). Suhu proses penurunan tamat beranjak kepada suhu yang lebih rendah
iaitu 700 °C dan proses penurunan tamat pada suhu (900 °C). Difraktogram XRD
terhadap Cr-Fe2O3 menunjukkan peningkatan
pada kehabluran puncak Fe2O3 berbanding ferik
oksida yang tidak didopkan dengan tiada puncak tambahan diperhatikan
dimana ia menjelaskan bahawa zarah kromium yang dimuatkan pada ferik oksida
telah tersebar dengan baik. Di samping itu, tambahan sebanyak 3 % kromium pada
ferik oksida memberikan kawasan permukaan yang lebih besar dan pengurangan tenaga
pengaktifan sehingga 12.39 % bagi peralihan fasa Fe2O3 →
Fe3O4 serta juga membawa kepada peningkatan kepada kadar proses
penurunan ferik oksida tersebut.
Kata kunci: penurunan suhu
berprogram, kinetik, penurunan, ferik oksida, kromium, karbon monoksida
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