10.1. Reducing power by ferric Chloride (FRAP) About 100 mg of Quercetin (Qu), Rutin (Ru), Silibinin (Si), Qu NPs, Ru NPs, Si NPs, Qu-Ru NPs and Qu-Si NPs (Test samples) were dissolved in 100 ml of methanol to obtain a solution of 1000µg/ml. From this stocking solutions, various working conc. were produced to get concentration of 100, 200, 300, 400, 500 µg/ml with distilled water. Different concentration of Quercetin (Qu), Rutin (Ru), Silibinin (Si), Qu NPs, Ru NPs, Si NPs, Qu-Ru NPs and Qu-Si NPs 100 µg/ml, 200 µg/ml, 300 µg/ml, 400 µg/ml, 500 µg/ml were individually mixed along 2.5 milliliter of one percentage C6N6FeK3. and incubating at 500Celcius for 30 minutes. The standard stock solution was prepared by dissolving ascorbic acid (Standard …show more content…
This stock solution was prepared freshly and kept in the dark at ambient temperature when not in used. About 100 mg of Quercetin (Qu), Rutin (Ru), Silibinin (Si), Qu NPs, Ru NPs, Si NPs, Qu-Ru NPs and Qu-Si NPs (Test samples) were dissolved in 100 ml with methanol, to obtain a solution of 1000µg/ml. From this stocking solutions, various working conc. were produced to get concentration of 100, 200, 300, 400, 500 µg/ml with distilled water. The standard stock solution was prepared by dissolving ascorbic acid (Standard Sample) in suitable solvent (methanol) with a final concentration of 1000 µg/ml and different concentration of 100, 200, 300, 400, 500 µg/ml were prepared by distilled water. 0.3 mM solution of free radical standard in CH3OH produced and 1 ml of this solution was admixed to three milliliter of test solution in H2O at different concentration and incubate for 30 minutes, the absorbance was taken at 517nm. Difference between the absorbance value of sample and control of (DPPH) was calculated and expressed as percent scavenging of DPPH radical. 95-104 All experiments were performed in
1.5mL of phosphoric acid including 3-4 boiling chips were also added to the 25mL flask. The short path distillation apparatus was set up as shown in Figure 1. A heating mantle was used to heat up the 25mL flask. The solution was distilled to the receiving flask until a small amount of liquid remained in the initial RBF flask. At this point the presence of thick grey smoke pulling over into the entire apparatus was observed. The apparatus was then left to cool down. Through the use of pasture pipette, the aqueous layer from the distilled solution was drawn out. Sodium carbonate was then added to the remaining organic solution in order to check the pH and to verify the basicity of the solution. The aqueous layer was again drawn out from the solution. Next, 0.5g of sodium sulfate was added to the remaining organic layer and was swirled until the liquid appeared to be dry and clear. The alkenes were transferred into a clean 10mL flaks using another clean pasture pipe. The apparatus from the first distillation was rinsed off with
After 10 minutes the reaction liquid was separated from the solid using a vacuum filtration system and toluene. The product was stored and dried until week 2 of the experiment. The product was weighed to be 0.31 g. Percent yield was calculated to be 38.75%. IR spectra data was conducted for the two starting materials and of the product. Melting point determination was performed on the product and proton NMR spectrum was given. The IR spectrum revealed peaks at 1720 cm-1, which indicated the presence of a lactone group, and 1730 cm-1, representing a functional group of a carboxylic acid (C=O), and 3300cm-1, indicating the presence of an alcohol group (O-H). All three peaks correspond with the desired product. A second TLC using the same mobile and stationary phase as the first was performed and revealed Rf Values of 0.17 and 0.43for the product. The first value was unique to the product indicating that the Diels-Alder reaction was successful. The other Rf value of 0.43 matched that of maleic anhydride indicating some
The purpose of this experiment was to perform a nucleophilic substitution reaction to construct a biologically active compound from two simple parts and then to recrystallize the product collected, which is a purification technique that purifies solids based on differences in solubility. In order to accomplish this, other techniques such as heating at reflux, and suction filtration were used. Heating at reflux is a technique used in lab that allows a solution to be heated for a certain amount of time once it begins boiling. Suction filtration is a separation technique that is combined with a water aspirator and was used to collect the product from this experiment, which was 2-methylphenooxyacetic acid.
The standard curve was plotted for FeSO4 with concentration range of 0.2-1mM, and there was a strong correlation between FeSO4 concentration and antioxidant capacity (R²= 0.992) and the equation was Y=0.1958X-0.2452. The standard curve displayed a linear trend between 0.2 to 1mM FeSO4. There was strong correlation between pectin concentration and antioxidant activity for all the pectin samples tested (R2=0.9778, 0.9885, 0.9742 and 0.9954), for the native, 100W, 200W and 400W degraded pectin respectively. Sonicated pectin had increased antioxidant activity with 400W treated pectin having 43% relative FRAP activity at 4mg/mL, the same concentration of native pectin had a lower relative FRAP activity 16.4% compared to FeSO4. There was generally increased antioxidant activity with increasing sonication power applied. The results are consistent with the previous observation by Pokora et al., [66], who reported that enzymatic hydrolysis of egg yolk protein and white protein improved their radical scavenging (DPPH) capacity, ferric reducing power, and chelating of iron activity. Native pectin is a complex molecule with complex side group structure, and during sonolysis the large molecule is depolymerized yielding low degree of polymerization pectin , thus exposing prior hidden functional groups and creating functional groups at the scission sites, e.g. carbonyl groups. The reducing agents mostly act as hydrogen/electron atom donors thus
When forming the Grignard reagent, the solution became brown in color and as it proceeded the solution became lighter. After a week, the solution was pink/red with clear/white crystals. In the addition of HCl, the solution began to become yellow and two layers began to form. The top layer was yellow and the lower layer was clear/white. The final alcohol product yield was calculated to be 88.317 percent by dividing the weight of the product (6.789 g) by the theoretical yield of 7.69 g. When placed in the infrared spectroscopy machine, alcohol (υO-H) was found at wavenumber of 3366.75 cm-1
Abstract: One mixture of two unknown liquid compounds and one mixture of two unknown solid compounds were separated, isolated, purified, and characterized by boiling point. Two liquid unknowns were separated, isolated, and purified via simple distillation. Then, the process of an acid-base extraction and washing were used to separate two unknown compounds into two crude compounds: an organic acid and a neutral organic compound. Each crude compound was purified by recrystallization, resulting in a carboxylic acid (RCO2H) and a pure organic compound (RZ). The resulting mass of the pure carboxylic acid was 1.688g with a percent recovery of 31.80%, the boiling range was 244-245 °C, and its density was 2.0879g/mL. The resulting mass of the pure organic solid was 2.4902g with a percent recovery of 46.91%, the boiling range was 52.0-53.4°C, and its density was 1.5956 g/mL.
Boiling chips were added to the 100 mL round-bottom flask. 50 mL of 1-propanol-water mixture (50% v/v) was added in the flask and heated until a drop rate of 15 to 20 drops per minute was achieved. Distilled into a 10 mL graduated cylinder, temperature and volume were recorded at 1 mL intervals. Distillation was stopped when the temperature increased to 90 degrees.
Objective: In steam distillation lab (lab 3), we must obtain pure Eugenol from cloves through the process of steam distillation. In the crystallization lab (lab 4) part 1, we must acquire the best possible pure crystallization of acetylsalicylic acid from aspirin and in part 2 we must obtain a similar pure crystallization of benzil from an impure mixture of benzil.
The original solution once the 1-butanol, hydrobromic acid, and sulfuric acid were added was yellow-orange in color. After distilling the distillate was clear then became partially cloudy. The calculated yield of the product was approximately 5.41%. The calculated yield was low due to a fluctuating temperature during the reaction and possible impurities formed.
3.4 Large scale reactions with purification and analysis of pigments Large scale experiments involving the oxidation of DOP in the presence of various POLs or other compounds were set up. DOP (about 30mg) was dissolved in 10mL water and about 100mg test compound or POL was added as a powder to dissolve in the mixture inside the wells of a cell-culture dish. The polysaccharides use in this experiments were FUCO, chitosan (CHITO), CARRA, XYL, CMC, GUM, CS A, HA, PEC, DEX, DEX_S and CS C. Other substances tested in this experiment were sodium acetate (NaOAc), sodium glucuronate (NaGlcA) and L-ascorbic acid (L-ASC). No cations were added to these mixtures.
The conversion of succinate to fumarate took place in the citric acid cycle, where the reaction reduced FAD to FADH₂ that produced free electrons that enter the Electron Transport Chain. By using DCPIP, an alternate electron acceptor, the reaction of the dye was monitored through its color change. DCPIP is blue in its oxidized form and colorless in its reduce state form. To determine the
The solution takes the gel form after vigorous stirring and overnight heating at 60C. The samples were then pelletized and sintered at 1100C and 1400C for 3 hours in a muffle furnace under air atmosphere (heating rate 10C/min.).
4-nitro-o-phenylenediamine (5 mmol, 0.77 g) in 25 ml ethanol was slowly added to ethanolic solution (25 ml) containing isatin (5 mmol, 0.74 g), followed by the slow addition of 5- bromosalicylaldehyde (5 mmol, 1.00 g) dissolved in 25 ml ethanol. A colored precipitate was obtained on refluxing the solution for 3 h, (cf. Scheme 1) [24]. The precipitate was filtered by suction and washed thoroughly with ethanol. The pure compound was dried in desiccator over anhydrous calcium chloride.
Based on the results of the tests and computations, the experiment did not go completely as what the experimenters want. The crude aspirin obtained was 67% while the percent recovery of the recrystallized aspirin was 50%. It can be concluded that by recrystallizing the crude aspirin, the percent yield decreases. The percent yield was below average and the recrystallized sample was not pure based on the tests that showed positive results of the product being contaminated with salicylic acid. When the product was reacted with ferric chloride, it gave dirty pink complex with undissolved precipitate and in Baeyer’s test, it showed disappearance of the purple complex and formation of brown precipitate after heating, both of which indicates that
Subsequently, 10mL of 3.5% H2O2 were added dropwise to the reaction mixture and was stirred for 20 minutes before heating to boiling at 80°C for 5 minutes. The reaction mixture was then taken off heat and allowed to cool undisturbed in an ice-bath for 30 minutes. Suction filtration was performed after to collect the crystals from the chilled solution The product was then washed with chilled 95% ethanol (2 x 15mL) and followed by diethyl ether (2 x 10mL). The crude product was then left to dry before recording the yield. 20mg of the crude product is then accurately weighed out and dissolved in deionized water in a 25mL volumetric flask. Deionized water was added to the volumetric flask to the mark and the UV-vis absorption spectrum of the crude product was recorded.