Physicochemical, Thermal and Spectroscopic Characterization of Sodium Selenate Using XRD, PSD, DSC, TGA/DTG, UV-vis, and FT-IR 1. INTRODUCTION

Year 2017, Volume: 21 Issue: 2, 311 - 318, 01.04.2017

Mahendra Kumar Trivedi Kalyan Kumar Sethi Panda Panda Snehasis Jana

https://doi.org/10.12991/marupj.300796

Abstract

Sodium selenate is an important inorganic compound, but

lacks reliable and accurate physico-chemical and spectral

characterization information. This article described the

in-depth physicochemical, thermal, and spectroscopic

characterization of sodium selenate using various analytical

techniques. The powder X-ray diffractogram showed welldefined,

narrow and sharp peaks indicating that sodium

selenate is crystalline in nature. The crystallite size was found

to be in the range of 28.75 to 49.97 nm. The average particle size

was found to be of 3.93 (d10), 14.44 (d50), and 40.65 (d90) μm with

an average surface area of 0.676 m2/g. The differential scanning

calorimetry showed the endothermic inflation at 588.81 °C

with the latent heat of fusion 103 J/g. The thermogravimetric

analysis revealed two steps of the thermal degradation process.

Similarly, the differential thermogravimetric analysis exhibited

the major peaks in the thermogram and disclosed Tmax at

852.65 °C. This indicated sodium selenate thermally more

stable in nature. The UV-visible spectrum showed maximum

absorbance at 205.1 nm (λmax). The Fourier transform infrared

spectrum showed a peak at 888 cm-1 due to the Se-O stretching.

These information would be very much useful in the field of

nutraceuticals/ pharmaceuticals and other industries using

sodium selenate as an ingredient.

Keywords

Sodium selenate, Crystallite size, Particle size, Thermal analysis

Sodyum selenat’ın XRD, PSD, DSC, TGA/DTG, UV-VIS ve FT-IR yöntemleri ile fizikokimyasal, termal ve spektroskopik karakterizasyonu

Abstract

Önemli bir inorganik bileşik olan sodium selanat’ın

fizikokimyasal ve spektral yöntemlerle karakterizasyonuna

dair kesin ve güvenilir veri bulunmamaktadır. Bu makale,

sodium selenat’ın çeşitli analitik yöntemler kullanılarak yapılan

fizikokimyasal, termal ve spektroskopik karakterizasyonu

ile ilgili geniş kapsamlı veri içermektedir. Toz X-ışını

difraktogramı, sodyum selenatın kristal yapıda olduğunu

gösteren iyi tanımlanmış, dar ve keskin zirveler göstermiştir.

Kristalit boyutu 28.75 - 49.97 nm aralığında bulunmuştur.

Ortalama partikül boyutu 3.93 (d10), 14.44 (d50), ve 40.65

(d90) μm, ortalama yüzey alanı 0.676 m2/g’dır. Diferansiyel

taramalı kalorimetre kullanılarak yapılan çalışmalarda 588.81

°C’de endotermik şişkinlik gösteren sodium selenat’ın gizil

füzyon ısısı 103 J/g olarak tespit edilmiştir. Termogravimetrik

çalışmalar, sodium selenat’ın termal bozunma sürecinin iki

basamaklı olduğunu göstermiştir. Benzer şekilde, diferansiyel

termogravimetrik analizlerde de termogramda iki ana pik ve

852.65 °C’de Tmax tespit edilmiştir. Bu sodyum selenatın doğada

termal olarak daha kararlı olduğunu gösterdi. UV-görünür

spektrum, 205.1 nm’de (λmax) maksimum absorbans gösterdi.

FT-IR spektrumunda, 888 cm-1’de Se-O gerilme titreşimlerine

atfedilen bir band görülmüştür. Bu bilgiler, nutrasötikler / ilaçlar

ve bir bileşen olarak sodyum selenat kullanan diğer endüstriler

için çok yararlı olacaktır.

Keywords

Sodyum selenat, Kristalit boyutu, Parçacık boyutu, Termal analiz, Yüzey alanı

References

• 1. Martens DA. Selenium. In: Encyclopedia of Water Science.United States Department of Agriculture (USDA), Tucson,Arizona, USA. 2003.
• 2. Stadlober M, Sager M, Irgolic K. Identification andquantification of selenium compounds in sodium selenitesupplemented feeds by HPLC-ICP-MS. Die Bodenkultur2001; 52: 233-41.
• 3. Ganther HE, Baumann CA. Selenium metabolism. II.Modifying effects of sulfate. J Nutr 1962; 77: 408-14.
• 4. Cardoso BR, Ong TP, Jacob-Filho W, Jaluul O, Freitas MI,Cozzolino SM. Nutritional status of selenium in Alzheimer’sdisease patients. Br J Nutr 2010;103: 803-6.
• 5. Chen J, Berry MJ. Selenium and selenoproteins in the brainand brain diseases. J Neurochem 2003; 86: 1-12.
• 6. Ani M, Moshtaghie AA, Aghadavod M. Protective effects ofselenium and zinc on the brain acetylcholinesterase activity inlead intoxified rat. Res Pharm Sci 2007; 2: 80-4.
• 7. Abubakar MG, Taylor A, Ferns GA. The effects of aluminiumand selenium supplementation on brain and liver antioxidantstatus in the rat. Afr J Biotechnol 2004; 3: 88-93.
• 8. Fleet JC. Dietary selenium repletion may reduce cancerincidence in people at high risk who live in areas with low soilselenium. Nutr Rev 1997; 55: 277-9.
• 9. Krieger RI. Handbook of pesticide toxicology, 2nd edition,volume 1. Academic Press. San Diego. 2001, pp. 1908.
• 10. Hanson B, Lindblom SD, Loeffler ML, Pilon-Smits EAH.Selenium protects plants from phloem-feeding aphids due toboth deterrence and toxicity. New Phytol 2004; 162: 655-62.
• 11. Barceloux DG, Barceloux D. Selenium. J Toxicol Clin Toxicol1999; 37: 145-72.
• 12. Thomson CD, Robinson MF. Urinary and fecal excretions andabsorption of a large supplement of selenium: Superiority ofselenate over selenite. Am J Clin Nutr 1986; 44: 659-63.
• 13. Salama RM, Schaalan MF, Elkoussi AA, Khalifa AE. Potentialutility of sodium selenate as an adjunct to metformin intreating type II diabetes mellitus in rats: A perspective onprotein tyrosine phosphatase. Biomed Res Int 2013; 231378.
• 14. Chereson R. Bioavailability, bioequivalence, and drugselection. In: Basic pharmacokinetics, 1st edition. Editors:Makoid CM, Vuchetich PJ, Banakar UV Pharmaceutical Press.London. 2009.
• 15. Langford JI, Wilson AJC. Scherrer after sixty years: A surveyand some new results in the determination of crystallite size. JAppl Cryst 1978; 11: 102-13.
• 16. Buhrke VE, Jenkins R, Smith DK. Preparation of specimensfor X-ray fluorescence and X-ray diffraction analysis. JohnWiley & Sons Inc. New York. 1998, pp. 148.
• 17. Burgess DJ, Duffy E, Etzler F, Hickey AJ. Particle size analysis:AAPS workshop report, cosponsored by the Food and DrugAdministration and the United States Pharmacopeia. AAPS J2004; 6: 23-34.
• 18. Weiner BB. What is a continuous particle size distribution?Brookhaven Instruments, NY, USA. 2011.
• 19. Wolfrom RL The language of particle size. J GXP Compliance2011; 15: 10-20.
• 20. Balzar D, Audebrand, Daymond MR, Fitch A, Hewat A,Langford JI, Le Bail A, Louer D, Masson O, McCowan CN,Popa NC, Stephens PW, Toby HB. Size-strain line-broadeninganalysis of the ceria round-robin sample. J Appl Cryst 2004;37: 911-24.
• 21. Swanson HE, McMurdie HF, Evans MCME, Paretzkin B,DeGroot JH, Carmel SJ.Standard X-Ray Diffraction PowderPatterns. National Bureau of Standards Monograph-25,Section 9, Nat Bur Stand 1971. pp. 55.
• 22. Moore DM, Reynolds Jr RC. X-Ray diffraction and theidentification and analysis of clay mineral, 2nd edition. OxfordUniversity Press. New York. 1997.
• 23. Sardela M. X-ray Analysis Methods. Advanced MaterialsCharacterization Workshop, The Frederick Seitz MaterialsResearch Laboratory-University of Illinois at Urbana-Champaign. 2008.
• 24. Martin AN, Patrick JS. Martin’s physical pharmacyand pharmaceutical sciences: Physical chemical andbiopharmaceutical principles in the pharmaceutical sciences.Phila: Lippincott Williams and Wilkins. 2006.
• 25. Jones AT. Development of the γ-crystal form in randomcopolymers of propylene and their analysis by DSC and X-raymethods. Polymer 1971; 12: 487-508.
• 26. Martin FJ, Albers H, Lambeck PV, Van de Velde GMH,Popma ThJA. Luminescent thin films by the chemical aerosoldeposition technology (CADT). J Aerosol Sci 1991; 22: 435-8.
• 27. Bajaj S, Singla D, Sakhuja N. Stability testing of pharmaceuticalproducts. J Appl Pharm Sci 2012; 2: 129-38.
• 28. Bansal KR. Synthetic Approaches in Organic Chemistry. Jones& Bartlett Publishers International. 1998, pp. 236.
• 29. Miller FA, Wilkins CH. Infrared spectra and characteristicfrequencies of inorganic ions their use in qualitative analysis.Anal Chem 1952; 24: 1281.