Acetonitrile at a PH of 7 (neutral) is added to each of the test tube samples. Mix the samples on a vertex shaker for 3 minutes and transfer to a 20 ml centrifuge tube and place in a TurboVap under 5-psi nitrogen at room temperature and allow it to completely dry. The dry resides are now put in 1ml of acetonitrile for testing (analysis). 4. Chromatographic Condition 10ml of the extract is now taken to be analyzed using a mass spectrometer and a liquid chromatograph.
Ethylene glycol has been widely used in the polyol process for the synthesis of metal (pure and alloyed) nanoparticles due to its strong reducing power and relatively high boiling point (~1970C). In this method ethylene glycol (fisher scientific 99.5%) is used as solvent and strong base sodium hydroxide (NaOH) (Qualigens 98%) is used as reducing agent along with NaBH4. Iron chloride tetra hydrate (FeCl2.4H2O) (Moly Chem 98%), Cobaltous acetate (Co(CH3COO)2.4H2O) (sd-fine chem. Limited 99%) are the metal precursors used in this Co and FeCo synthesis, PVP (C6H9NO)n (sigma Aldrich 99.9%) acts as surfactant. 2.1 Synthesis of Co Nanoparticles 2.1.1 Experimental
Referring to Table 1, the reactants for each run were transferred to an Erlenmeyer Flask (250 mL) via a buret. Using a precision pipette, the volume of I3- required for each run was carefully extracted and poured into the flask containing all of the reactants. Immediately after the Iodine solution was placed in the flask, the LabQuest began collection data. Meanwhile, a small portion of the solution, was used to rinse the cuvette, then using a disposable pipette a small amount of the solution was transferred to the cuvette (approx. ¾).
The solvents DMF and methanol were distilled for purification. Other chemicals were used as obtained. 2.2 Preparation of polystyrene (PS) Polystyrene prepared by free radical polymerization of styrene monomer. Styrene (1 mole) was taken in a round bottom flask (RBF) fitted with a reflux condenser. DMF was used as a solvent and AIBN (0.5% w/w of total monomer) as free radical initiator .The reaction was carried out at 70±2° C for 6 hour with constant stirring.
The mixture was finally made upto 5 mL with distilled water and placed in hot water bath at 95ºC for 1 h. After cooling, 1 mL of distilled water and 5 mL of the mixture of n-butanol and pyridine (15:1, v/v) was added. The mixture was vortexed and after centrifugation at 4000 rpm for 10 minutes, the absorbance of the organic layer (upper layer) was measured in UV-Vis spectrophotometer (Shimatzu) at 532 nm against blank using distilled water. TBA when allowed to react with MDA aerobically formed a colored complex [MDA-(TBA) 2 complex] which was measured with spectrophotometer. MDA concentration (measured as TBARS) was calculated as
The solution homogeneity expelled, by centrifugation for 10 min. The sample was centrifuged and separated into two layers, and took the top of the sample is injected for HPLC (11,12). Measured concentration in total lipid: The total fats balanced concentration of the pesticide getting by dividing the measured pesticide residue concentration in the overalll tissue sample by the decimal fraction of the sample that consisted of ether-extractable lipid. The total lipid content of each specimen was estimated from its total cholesterol & triglycerides levels by using a summation method. Analytical results for organochlorine pesticides were reported on a lipid-adjusted basis (nanograms per gram or parts per billion) (14).
CER Labs 2-3 Figure 1. Friedel-Crafts Acylation. Claim: An acetyl group was efficiently introduced to ferrocene by Friedel-Crafts Acylation (Figure 1). We isolated our crude yield while comparing 2 purification techniques: column chromatography and recrystallization. TLC, NMR, and IR spectroscopy were used throughout the process to identify ferrocene and acetylferrocene in addition to evaluating the levels of purity.
In the round-bottom flask (100 mL), we placed p-aminobenzoic acid (1.2 g) and ethanol (12 mL). We swirled the mixture until the solid dissolved completely. We used Pasteur pipet to add concentrated sulfuric acid (1.0 mL) to the flask. We added boiling stone and assembled the reflux. Then, we did reflux for 75 minutes.
The solvent system used for analysis was 10 mM NaOAc/ 150 mM NaOH and the kestoses were eluted at a flow rate of 1 mL /min. 3.2.2. Investigation of reaction parameters There are certain reaction conditions that may favour the production of one kestose isomer over the other. Therefore, several parameters (pH, temperature and time) were chosen and investigated to develop the optimum reaction conditions for each of the kestoses. The experiments for each parameter was carried out in triplicate.
1.1. UV-SPECTROPHOTOMETRY Spectroscopy is the measurement and interpretation of electromagnetic radiation absorbed or emitted when the molecules or atoms or ions of a sample move from one energy state to another energy state. Spectroscopy is a general methodology that can be adapted in many ways to extract the information you need (energies of electronic, vibrational, rotational states, structure and symmetry of molecules, dynamic information). Ultraviolet-Visible Spectrophotometry is one of the most frequently employed techniques in Pharmaceutical analysis. It involves the measurement of the amount of Ultraviolet (190-380nm) radiation by a substance in a solution.