PHYSICOCHEMICAL STUDY AND QUANTITATIVE ANALYSIS SWARNA MAKSHIKA BHASMA

Swarnamakshika is grouped under Updhatu of Swarna and is composed of Copper, Iron and Sulphur. In this study Swarnamakshika was subjected to Shodhana by Bharjana with Nimbuka swarasa and Shudha Swarnamakshika was given Bhavana with Nimbuka swarasa and subjected to Varahaputa. With ten Varahaputa Bhasma Siddhi Lakshanas were attained swarnamakshika Marana was done by using Nimbuka swarasa until bhasma siddi lakshanas found and it took 10 puta till it attained reddish brown color. The X-ray diffraction analysis showed that d-identified peaks after 10th puta Swarnamakshika bhasma composition is of Iron oxide with rhombohedral crystal system as main component. EDX analysis of Swarna makshika bhasma shows that it contains Iron and Oxygen, as major element and Copper, Sulphur, Carbon, Aluminium, Calcium etc. as minor elements. FESEM study revealed that the particle size of Ashudha and Shudha Swarnamakshika was in the range of 500 nm-3nm.


INTRODUCTION
Bhasmas are biologically produced nanoparticles, which are prescribed in a lower dose but act even on the smallest body channels (Strotas) and penetrate into the deepest tissues to give desired results. 1 In the present scenario the tradition of making medicines by the practitioners have almost come to an end. Presently many Pharmaceutical industries are preparing classical medicines but have lost their credibility due to increased demand, poor manufacturing practices and not following proper guidelines in order to gain profits. So, preparation of Ayurvedic medicines need immediate and extensive orientation in order to provide quality medicine. Swarnamakshika is a Updhatu of gold and is composed of Copper, Iron

Material and Methods:
This study was carried in the following steps: • Collection and selection of the raw material • Shodhana of Swarnamakshika • Marana of the Swarnamakshika

Collection and selection of the raw material
Ashudha Swarnamakshika was collected from Sri Herbacia Biotech, Amritsar, having all grahaya lakshanas as told in classcics. The raw material was authenticated from Government drug testing laboratory, Patiala.  It was triturated with 340 ml of freshly prepared nimbuka swarasa for 7 hours  Trituration was done until it attains a viscous, semisolid consistency. This is very important step, needs care and skill for proper blending of material and further reduction of particle size takes place in consequent putas, which further shortens the time factor and reduces the fuel quantity by reducing frequency of firing, for proper and uniform mixing of the core and surface of the pellets. b) Preparation of Chakrikas (Pelletization)  After completion of bhavana process, small uniform and approximetly equal size pellets were prepared out of the paste.  Chakrikas were prepared of size 4cm diameter, 0.7cm thickness.  Weight of each chakrika 18-19 grams  Chakrikas were kept for drying.  If chakrikas will not dry properly then it will become hard after subjecting to heat,which are supposed to be soft otherwise  Average weight of chakrika after drying was 625gms.  Quantitative analysis X ray diffraction (XRD) X Ray Diffraction is an efficient analytical technique used to identify and characterize unknown crystalline material. Monochromatic X-rays are used to determine the interplanar spacing of the unknown materials .Sample are analysed as powders with grains in random orientation to ensure that all crystallographic directions are "sampled" by the beam .When the bragg's condition for constructive interference is obtained, "reflection" is produced and the relative peak height is generally proportional to the number of grains in a preferred orientation. Principle Distance between each set of atomic planes (i.e inter atomic space "d") is determined with the help of wavelength of X-Ray beam and angle of diffraction theta by applying bragg's law nλ=2dsin θ No two substances have absolutely identical diffraction patterns the "d" spacing of the ten most intense reflecting planes of atoms are calculated and results are compared with the data of X-Ray powder data file and identification of the sample is done. Method Different methods available for x-ray diffraction are Lane photographic method, Bragg x ray spectrometer method, Rotating crystal method and powder method. In the present study powder method of diffraction has been adopted.

Sample preparation
The sample are ground to a fine homogeneous powder then placed in a sample holder or the specimen may be mixed with a suitable noncrystalline binder and moulded into a suitable

Field emission scanning electron microscopy with energy dispersive x-ray FESEM-EDS 226
Field emission scanning electron microscope is used to observe small structure (as small as one nanometre), A FESEM is a microscope that works with electrons (particles with a negative charge) instead of light, These electrons are liberated by a field emission source the object is scanned by electrons according to a zigzag pattern. The sample region evaluated with FESEM Analysis can also be analyzed to determine the specific elements that comprise the sample region by utilizing Energy Dispersion Spectroscopy (EDS). X-rays are also released from the surface of the sample that carry a unique energy signature that are specific to elements found in the sample. These X-rays are detected with the EDS detector to give elemental information about the sample. EDS provides data about the chemical composition of the sample and provides additional data about the features that are observed in the SEM micrographs. This combined technique is referred to as FESEM-EDS or FESEM-EDX Analysis.

Advantages
• FESEM gives better resolution than SEM. because field emission source is used in FESEM.
• It can tolerate high electrostatic fields.
• FESEM at labs-Services is capable of performing high-resolution imaging with very low accelerating voltages.

Applications
• Ideal microscopic imaging for polymer and thin films.
• Micro-structure studies best suitable for R&D.
• Detail specimen features characterization.
• Material analysis for component layers.

X -Ray Diffraction Study
The 2theta value and intensity of the peak (counts) are represented on X and Y-axis respectively. Higher the value of counts, represents higher the crystallanity of the phase, for identification of each phase minimum 3 strong peak were chosen.    The analysis revealed that Iron and Oxygen as major elements and rest of the elements are found in traces and here Sulphur is in the sulphide form. In Bharjana method of Shodhana, the percentage of Sulphur was decreased which might be due to more quantity of heat. The percentage of Oxygen has shown it as major elements which confirms that the bhasma is in oxide form. FESEM Micrographs of Swarnamakshik bhasma indicates that it belongs to the group of mineral powder. Particles of bhasma are uniformly arranged having extensively reduced grain size due to process effect, while the particles in Ashuddha Swarna makshika and Shuddha Swarrnamakshika were not uniformly arranged.The clustering nature of the bhasma was observed and it was due to the fine nature of these amorphous/ microcrystalline particles.

Conclusion
Swarnamakshika Marana was done until bhasma siddhi lakshanas were attained and it took ten putas. Study of physicochemical parameters revealed increase in percentage of iron and decrease in percentage of copper after Shodhana and subsequent Marana. The X-ray diffraction analysis showed that d-identified peaks after 10th puta Swarnamakshika bhasma composition is of Iron oxide with rhombohedral crystal system as main component. EDX analysis of Swarna makshika bhasma shows that it contains Iron and Oxygen, as major element and Copper, Sulphur, Carbon, Aluminium, Calcium etc. as minor elements. FESEM study revealed that the particle size of Ashudha and Shudha Swarnamakshika was in the range of 500 nm-3 but after subjecting bhasma to subsequent puta s until bhasma siddhi lakshanas were attained, particle size after tenth puta was reduced to 1 which showed excellence of bhasma in regards to particle size.