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Nandre, S. J., Gayakwad, A. A., & Pawar, H. S. (2026). Comparatively Study of Physical and Structural Properties ofTransition Metal Oxalate Crystal. International Journal of Research, 13(13), 721–730. https://doi.org/10.26643/rb.v118i5.7998

S. J. Nandre¹, A. A. Gayakwad², H. S. Pawar^3
1Department of Physics, Uttamrao Patil Arts and Science College, Dahiwel, (Dhule) M.S. ²R.C. Patel Anu. Higher Secondary Ashramschool, Shirpur,(Dhule) M.S.
³V.J.N.T. Late Dalpatbhau Rathod Junior College, Mordadtanda, (Dhule) M.S.

Abstract                                                                                                                                

At room temperature, a single crystal of manganese oxalate and cadmium was produced using the agar-agar gel method. The effects of various parameters on the formation of cadmium manganese crystals have been studied and recorded. Compares and assesses the growth and properties of the two crystals under study.Using X-ray diffraction analysis, the structure of the developed crystal was determined. FTIR has performed the chemical study to determine the crystal's growing functional group. Images from a scanning electron microscope show that layer deposition was used to build the crystals.

Keywords: Single diffusion, Crystal growth, XRD, FTIR, SEM.

1.1. Introduction

Transition metal oxalate crystals have been the subject of extensive research due to their diverse properties and potential applications. Comparatively analysing the structural features, physical properties, and chemical behaviour of several transition metal oxalate crystals is the aim of this work [1-2]. Coordination geometries cantered on the metal ion are typically found in transition metal oxalate crystals. Typical forms include tetrahedral, square planar, and octahedral geometries [3]. The steric requirements of the oxalate ligands and the electronic structure of the metal ion influence the choice of shape. Interest in this class of inorganic materials has grown due to the unique properties and potential applications of transition metal oxalate crystals.Among these, the crystals of manganese oxalate and cadmium are particularly interesting due to their peculiar properties and uses [4]. The purpose of this study is to contrast the crystals of manganese and cadmium oxalate. Therefore, in the present work, we have investigated the mechanism of production of manganese oxalate and cadmium crystals. Both kinds of crystals were created utilizing single diffusion processes in the gel method. evaluates and contrasts the growth and properties of the two crystals under study.

 

2. Materials and Methods

The cadmium and manganese oxalate crystals were grown at room temperature in the current work using the single diffusion agar-agar gel technique. Cadmium chloride (CdCl₂), manganese chloride (MnCl₂), oxalic acid (H₂C₂O₄) and agar- agar powder were used as chemical compound. All the chemical compounds were AR grade. To prepare all the experimental solutions, distilled water was used. The crystalizing vessel was a 250 mL glass beaker and a single glass tube that was 15 cm long and 2.5 cm in diameter. The test tube was filled with the initial reactance of the required volume and molarity in single diffusion. The gel was made by combining 0.5 to 2.5 grams of agar powder with 100 ml of boiling water. The resulting hot agar-agar gel was then transferred into a test tube and allowed to set. The second reactant, an oxalic acid solution of the appropriate volume and molarity, was put on top of the gel after it had set and aged. Cotton plugs were used to seal open end of the test tubes which was maintained at room temperature. After a few days, there was some nucleation on the interface of test tubes. The different shaped crystals that had developed there were then removed from the gel. As the crystals grew, they were gathered and examined. The reaction which command to the growth of cadmium and manganese oxalate crystal were expressed as,

3.Results & Discussion

3.1 Crystal Growth

Cadmium oxalate and manganese oxalate crystals were produced applying the gel method and a single diffusion procedure [5]. In the current study, developed better-quality cadmium oxalate crystals in the gel after a few days. These crystals were formed like diamonds, pentagonal, elliptical, cubic, aquamarine, emerald, kite, and alum like shape. They were also whitish in colour and had an average dimension of 7 x 3 x 2 mm³. Different shape of grown cadmium oxalate crystal as shown in fig 1.1. In the course of an eight-week nucleation process, three crystals of manganese oxalate were created. An excellent quality exhibiting various morphologies of manganese oxalate crystals, such as granular, spheroidal, crumb, oval-shaped, sago seed, hailstone, rock of salt, spherical, and white milk in coloured [6], with an average size of 2 x 2 x 1 mm³as shown in fig.1.2. Making use of the single diffusion gel technique was advantageous as it allowed us to obtain just well-formed and high-quality crystals. Table 1.1 reports the ideal growth conditions for gel-grown crystals, which were determined by adjusting several factors such as the gel setting time, gel percentage, reactant concentration, supernatant concentrations, and aging times, etc.

Fig 1.1. Diamond, quadrilateral, pentagonal, aquamarine, emerald, kite, alumlike shape

Fig.1.2. Sago seed, hailstone, rock of salt, spheroidal, crumb and oval shaped observed

 

 

Table 1.1. Optimized growth parameters of the transition metal oxalate crystals

Sr.no	Parameters	Cadmium	Manganese
1.	Concentration and Volume of oxalic acid	1M and 10 ml	1M and 25 ml
2.	Concentration and volume of Supernatant	1M and 5ml	1M and 10 ml
3.	Percentage of gel	1%	1%
4.	Gel setting period	18-24 hours	24 - 36 hours
5.	Crystal maturity period	25 days	56 days
6.	Temperature	Room Temperature	Ambient Temperature
7.	Nature and Colour of the crystal	Translucent and white	Semi translucent and white

 

3.2. X-ray Diffraction (XRD) Analysis

Fig.2. XRD pattern of cadmium oxalate and manganese oxalate crystal

The crystals of cadmium oxalate and manganese oxalate crystals were characterized by using typical Bruker AXS Germany, D8Focus instrument produced Cuka (1.5406 A0) radiation for structural study at Crysta Peak Solution Lab, Pune.  X-ray diffraction spectrum as shown in fig.2 which provides the 2θ, d value, relative intensity, and Millar indices (h k l) of the primary peak. The characteristic peak is visible at 13.88⁰ (2θ) for cadmium oxalate.The XRD pattern reveals that sample is crystalline in the nature having triclinic structure [7-10]. The 2 Peak observed at 11.16⁰, 13.88⁰, 15.42⁰, 16.72⁰, 19.03⁰, 19.79⁰, 22.42⁰, 24.26⁰, 27.92⁰, 31.56⁰, 33.76⁰, 37.65⁰, 55.91⁰, 57.75⁰ which corresponds to (0 0 1), (0 1 0), (1 0 0), (1 0 1), (1 1 1), (0 -1 1), (0 0 2), (1 -1 1), (0 2 0), (0 2 2), (2 0 2), (2 2 1), (1 -3 2), (2 -3 1) plane of reflection respectively. The lattice parameter for was found as a = 6.00 A⁰, b = 6.66 A⁰, c = 8.49 A⁰ i.e. a ≠ b ≠ c, α = 74.66, β = 74.28, γ = 81.00 i.e. α ≠ β ≠ γ and unit cell volume V=314.30 A⁰. The lattice parameter of manganese oxalate crystal from XRD data as a = 12.016, b = 5.632, c = 9.961, α = 90⁰, β = 128.4⁰, γ = 90⁰ and unit cell volume V = 528.29 A⁰. At 18.83⁰ (2θ), the distinctive peak may be seen i.e.  α = γ ≠ β. The XRD pattern suggest that sample is crystalline in the nature having monocline structure [11]. The 2θ Peak seen at 18.37⁰, 18.83⁰, 22.66⁰, 24.45⁰, 29.77⁰, 33.34⁰, 39.27⁰, 44.32⁰, 46.60⁰, 47.36⁰, 49.30⁰, 49.93⁰ which corresponds to (-2 0 1), (2 0 0), (0 0 2), (1 1 1), (-4 0 2), (1 1 -3), (0 0 2), (1 1 3), (-4 2 1), (0 2 3), (-1 3 1), (-4 2 4) plane of reflection respectively.

Table 1.2.Comparison of crystal lattice parameter of grown crystals

Crystal Parameter	Crystal System	a A0	b A0	C A0	Volume A3
Cadmium	Triclinic	6.00	6.66	8.490	314.30
Manganese	Monoclinic	12.016	5.632	9.961	528.29

3.2. Fourier Transforms Infrared Spectroscopy (FTIR)

 

Fig. 3 FTIR spectrum of cadmium oxalate and manganese oxalate crystal

The FTIR spectra of manganese oxalate and cadmium oxalate crystals were obtained using the Shimadzu FTIR-8400S spectrometer at the R. C. Patel Pharmacy Research Institute in Shirpur utilizing the KBr pellet technique in the 4000 cm^-1 to 400 cm^-1 range. The FTIR spectrum of manganese oxalate and cadmium oxalate crystals as shown in fig.3. In grown crystals, the fundamental FTIR frequencies were measured [12]. Cadmium oxalate and manganese oxalate crystals are found to have functional groups including O-H strong starching of water molecules, C-C starching, C-O stretching vibration bond, C-H bending bond, and metal oxygen bond [13-19]. Table 1.3 provides a summary of the functional group data obtained in crystals.

 

Table 1.3Comparison of FTIR data of transition metal oxalate crystals.

Sr. No	Wave Number cm-1		Assignments
	Cadmium	Manganese
1.	3427.78, 2272.20, 2246.97	3377.69,3334.44	O-H stretching and water molecule
2.	1599.71	1618.37	C-C
3.	1369.89, 1312.40	1313.91	C-O
4.	790.36	813.12	C-H
5.	665.35	720.36	Metal oxygen bond

 

3.3. Scanning Electron Microscope (SEM)

Fig.4.1 Different SEM photograph of cadmium oxalate crystal

The morphology of the powdered samples of cadmium oxalate and manganese oxalate crystals was examined using scanning electron microscopy. The Nova Nano SEM 450 was used for the SEM analysis at the Crysta Peak Solution Lab in Pune. The SEM images of cadmium oxalate and manganese oxalate crystals as shown in fig. 4.1 and 4.2 respectively.The chemical exhibits a range of morphologies with regular phases and a mostly crystalline structure, according to SEM photographs. Cadmium oxalate crystals are depicted in SEM photos with several morphologies, including columnar, triangular, polygonal, garnet and capsulated, cocci, ruby, cashew shape, rod, spherical,  elliptical, cylindrical, walnuts, and bitter gourd ,opal, oval, and spade and for manganese oxalate ice cube pieces, flat, square, rectangular, jaggery pieces, pentagonal quadrilateral, planks of woods, cocci, flat, square, rectangular, pentagonal, rod, capsulated, elliptical, spherical, round etc. shapes are investigated in SEM photograph [20-22].

 

Fig.4.2. Different SEM images of cadmium oxalate crystal

 

 

4.Conclusions

·         The single diffusion technique in agar-agar gel was used to effectively create a single crystal of cadmium and manganese oxalate crystals.

·         White colour with average size of 7 x 3 x 2 mm³ single crystal of cadmium oxalate crystals obtained during a period of 3 weeks and white colour with average size of 2 x 2 x 1 mm³single crystal of manganese oxalate crystals were obtained during a period near about 2 months.

·         X-ray diffractometer measure that grown crystals are in crystalline in nature and having monoclinic structure for manganese oxalate and triclinic structure for cadmium oxalate crystal.

·         Fourier Transforms Infrared Spectroscopy (FTIR) identified that grown oxalate crystals reveals the presence of oxalate ligands (C–C, C–O,) and crystallization water molecule (C–H).

·         SEM image suggest that grown crystals have different morphology like columnar, ice cube pieces,jaggery pieces, triangular, polygonal, garnet, cashew shape, rod, spherical, capsulated, cocci, ruby, elliptical, cylindrical, walnuts, bitter gourd and oval.

Acknowledgments

The principal, Dr. R. R. Ahire, S.G.P. Arts, Commerce and Science College, Sakri is acknowledged by the authors for providing laboratory facilities. We also appreciate the characterization facilities provided by Mr. Satish Bagal, Crysta Peak Solution Lab Pune, R.C. Patel Research and Pharmacy Instituted, Shirpur. For this insightful conversation on chemical reactions and other topics, thank you to Mr. Ganesh Patil and Mr. Deepak Patil of R.C. Patel Pharmacy Instituted, Shirpur.

 

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