X-ray fluorescent (XRF) X-ray fluorescent (XRF)

XRF Analysis (Genius-IF Xenometric): A sample cup was prepared with propylene thin film. Pulverized sample (~5g) was added to one-third of the cup, sealed properly, and inserted into the sample turret. After powering the X-ray lamp and allowing a 2-minute stabilization, voltage and emission current were adjusted to maintain a dead time between 35–40 kV. The analysis was run to obtain spectral data. Using XRS-FP software, the Master Oxide.tfr file and sample spectrum were processed and saved as a PDF. MP-AES Analysis (Agilent 4100 MP-AES): Samples were digested using 12 mL Aqua Regia (9 mL HNO₃ + 3 mL HCl) for 20 minutes at 100°C. The MP-AES system was powered, connected to gas lines supplying 4.6 bars pressure, and calibrated with standard metal solutions. After calibration and plotting the curve, samples were analyzed sequentially and the results printed out. The system uses high-intensity microwave plasma (~6000°C) and safety features including radiation shielding and status indicators.

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Sample cup was prepared with propylene thin film, ensuring smoothness of the thin film surface.

Pulverized sample was poured into thin film covered cup with sample filled to a third of the sample cup (approx. 5g). The lid of sample cup was covered and it was ensured that there wer no leakages or loose particles on thin film layer and also lids are tightened shut. The sample was then inserted into sample turret of Genius-IF Xenometric XRF sample chamber. The X-ray Lamp was then powered and allowed to stabilize in 2 minutes On the RUN tab, Voltage and Emission current values were set to ensure that observed dead time is between 35-40kv; The analysis was then RUN to obtain spectrum data. XRS-FP Crossroad scientific Software was then open and the Master Oxide.tfr file was uploaded then obtained Spectra file of sample was process then saved and printed to PDF file.

Operation of the Agilent 4100 MP-AES

It involved the use of compressed air, high microwave energy and flammable liquids. The plasma is extremely hot (about 6000°C) and operates using high levels of microwave energy. The plasma emits high intensity light. The microwave excitation assembly is designed to reduce microwave radiation to safe levels while still allowing easy installation of the torch and viewing of the plasma. The various indicator lights are colour coded to represent the status of the instrument. The sample is first digested with 12ml of Aqua Regia (9ml conc nitric acid + 3ml conc hydrochloric acid) for 20 minutes at 100oC.

the MP-AES was then powered and the software was uploaded, while the gas lines connected to the MP-AES was set to supply at a pressure of 4.6 bars. The sampled Prepared for the analysis was then brought forward. The MP-AES was then Calibrated with the standard solution of the metals to be analysed and the calibrated curve was plotted out. Worksheet was then opened and the samples was ran one after the other then the results were printout