In this experiment, a mixture of three substances (benzoic acid, 2-naphthol, and 1-4 dimethoxybenzene) will be separated based off acidity strength using the liquid-liquid extraction technique through a separatory funnel. Benzoic acid and 2-napthol will be converted into ionic salts when reacting with their appropriate bases (sodium bicarbonate and sodium hydroxide). Both ionic salts will then form solids through the addition of acidic HCl. Neutral 1,4 – dimethoxybenzene forms a solid through the evaporation of ether. Each compound will then be purified through recrystallization, using the processes of dissolving the solid in either water or methanol, and isolating the solid through vacuum filtration. After a week of evaporation, the compounds will then be examined for both …show more content…
Based on the observed melting point range, the sample of Benzoic Acid was pure. The melting point range of the product read 122.5°C -123.2°C. The melting point fell within the melting point range of pure Benzoic Acid (121°C – 125°C), indicating both products are similar to one another. The melting point range of the sample was also very narrow (<1°C), indicating the sample was not comprised of any major impurities. Based on the observed melting point range, the sample of 2-naphthol was relatively pure. The sample’s melting point range (121.3°C – 122.6°C) was slightly below the range of pure 2-naphthol (123°C – 124°C), indicating the possibility of impurities. Yet, the melting point range of the sample was very narrow (≅1°C), indicating the sample was not comprised of any major impurities. Based on the observed melting point range, the sample of 1,4 – dimethoxybenzene was very impure. The sample’s melting point range (116.5°C – 120.9°C) was much higher than pure 1-4 dimethoxybenzene (58°C – 60°C), indicating major impurities within the sample. The wide observed melting point range also indicates a depressed melting point, leading to the conclusion that the compound is
The primary goal of this laboratory project was to identify an unknown compound and determine its chemical and physical properties. First the appearance, odor, solubility, and conductivity of the compound were observed and measured so that they could be compared to those of known compounds. Then the cation present in the compound was identified using the flame test. The identity of the anion present in the compound was deduced through a series of chemical tests (Cooper, 2009).
The technique used to narrow down the identity of unknown white compound were solubility test, pH test, flame test, and ion test. The first technique used to narrowed the properties of unknown white compound was using solubility test. To conduct solubility test, 0.25 gram of unknown white compound was dissolved in 100 mL of water. After carefully observing the change while string unknown white compound in water, the unknown white compound was soluble because it dissolved in water completely. Using bursen burner, matches and deionized water, flame test was conducted for unknown compound and it burned lilac color. Then compared the color of unknown white compound to other compound that were narrowed. The results of flame test for compounds that were narrowed down is shown in the following table. The pH test was conducted using litmus paper. 0.50 gram of unknown white compound was measured and dissolved in 10 mL of water in beaker. After dissolving, placed the litmus paper in solution and recorded the pH value of unknown compound which was neutral. Then compared the pH value of unknown white compound to compound that were narrow down. The pH result of the KCL, KNO3, NaCl, and K2SO4 is presented in the following table. The ion test was also conducted in order to make sure that the identity of unknown white compound was matched with the compound that were narrow down. After conducting the test, the result of unknown white compound which formed precipitate compared to KCl, KNO3,NaCl, and K2SO4. The results shown in the following
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The theoretical weight was 599.6 mg. This yields a percent yield of 3.7%. Table 1 also illustrates the experimental melting point of 99.3-102.1◦C. A melting point that has a range larger than 3◦C is indicative of impurities in the sample. A few possibilities of impurities could have been unreacted norbornene, and water. Evidence that supports that there was unreacted norbornene in the final sample was the fact that the product was a jelly-like structure. Norbornene by itself has a jelly-like structure. However, once norbornene reacted with the acid-catalyst (H2O2), then it should have changed the chemical structure of the molecule and once the solution was brought back down to room temperature, crystals should have formed. Since a jelly-like, or oil-like product was present at the end of the reaction, then this is indicative that there was unreacted norbornene in the sample. The second impurity that may have been present in the final product was water. Instead of adding 3 mL of sodium bicarbonate and then 3 mL of brine, 3 mL of brine was added first and then 3 mL of sodium bicarbonate was added. This experimental error caused excess aqueous solution to be added to the diethyl ether. Since excess water was added to the final product, about 4x the amount of anhydrous sodium sulfate was needed in order to remove the water from the product. This was another indication that there was too much water in
The boiling point of the product was conducted with the silicone oil. Lastly, for each chemical test, three test tubes were prepared with 2-methylcyclohexanol, the product, and 1-decene in each test tube, and a drop of the reagent were added to test tubes. The percent yield was calculated to be 74.8% with 12.6g of the product obtained. This result showed that most of 2-methylcyclohexanol was successfully dehydrated and produced the product. The loss of the product could be due to the incomplete reaction or distillation and through washing and extraction of the product. The boiling point range resulted as 112oC to 118oC. This boiling point range revealed that it is acceptable because the literature boiling point range included possible products, which are 1-methylcyclohexene, 3-methylcyclohexene, and methylenecyclohexane, are 110 to 111oC, 104oC, and 102 to 103 oC. For the results of IR spectroscopy, 2-methylcyclocahnol showed peaks at 3300 cm-1 and 2930 cm-1, which indicated the presence of alcohol and alkane functional group. Then, the peak from the product showed the same peak at 2930 cm-1 but the absence of the other peak, which indicated the absence of the alcohol
The experiment was conducted in three parts: Part A of the experiment consisted of extracting caffeine from an aqueous solution; Part B consisted of using three different compounds: benzoic acid, succinic acid, and sodium benzoate; and the last part of the experiment consisted of using a solid neutral compound with an acid or base impurity.
Ensure gloves are worn at all times when handling strong acids and bases within the experiment of the preparation of benzocaine. 4-aminobenzoic acid (3.0g, 0.022 moles) was suspended into a dry round-bottomed flask (100cm3) followed by methylated sprits (20 cm3). Taking extra care the concentrated sulphuric acid of (3.0 cm3, 0.031 moles) was added. Immediately after the condenser was fitted on, and the components in the flask were swirled gently to mix components. It should be ensured that the reactants of the concentrated sulphuric acid and the 4-aminobenzoic acid were not clustered in the ground glass joint between the condenser itself and the flask. In order to heat the mixture to a boiling point, a heating mantle was used and then further left for gently refluxing for a constituent time of forty minutes. After the duration of the consistent forty minutes the rou...
Solid A was identified to be sodium chloride, solid B was identified to be sucrose, and Solid C was identified to be corn starch. Within the Information Chart – Mystery White Solid Lab there are results that distinguishes itself from the other 4 experimental results within each test. Such as: the high conductivity and high melting point of sodium chloride, and the iodine reaction of corn starch. Solid A is an ionic compound due to its high melting point and high electrical conductivity (7), within the Information Chart – Mystery White Solid Lab there is only one ionic compound which is sodium chloride, with the test results of Solid A, it can be concluded that is a sodium chloride. Solid B was identified as sucrose due to its low electrical
The theoretical yield of the m-nitrobenzoate was de-termined to be 4.59 grams. The actual amount of crude product was determined to be 3.11 grams. The percent yield of the crude product was determined to be 67.75 %. The actual amount of pure product formed was found to be 4.38 grams. The percent yield of the pure product was determined to be 95.42%. Regarding the thin layer chromatography, the line from the solvent front was 8 centimeters.
The purpose of this experiment was to learn and preform an acid-base extraction technique to separate organic compounds successfully and obtaining amounts of each component in the mixture. In this experiment, the separation will be done by separatory funnel preforming on two liquids that are immiscible from two layers when added together. The individual components of Phensuprin (Acetylsalicylic acid, Acetanilide, and Sucrose as a filler) was separated based upon their solubility and reactivity, and the amount of each component in the mixture was obtained. Also, the purity of each component will be determined by the melting point of the component.
In order to separate the mixture of fluorene, o-toluic acid, and 1, 4-dibromobenzene, the previously learned techniques of extraction and crystallization are needed to perform the experiment. First, 10.0 mL of diethyl ether would be added to the mixture in a centrifuge tube (1) and shaken until the mixture completely dissolved (2). Diethyl ether is the best solvent for dissolving the mixture, because though it is a polar molecule, its ethyl groups make it a nonpolar solvent. The compounds, fluorene and 1, 4-dibromobenzene, are also nonpolar; therefore, it would be easier for it to be dissolved in this organic solvent.
The conical vial was placed in a small beaker and allowed to cool to room temperature. The mixture was Cooled thoroughly in an ice bath for 15-20 minutes and crystals collected by vacuum filtration on a Hirsch funnel. The vial was rinsed with about 5 mL of ice water and transferred into to the Hirsch funnel and again washed with two additional 5mL portions of ice water. Crystals were dried for 5-10 minutes by allowing air to be drawn through them while they remained on the Hirsch funnel. The product was transferred to a watch glass plate and allow the crystals to dry in air. Crude acetaminophen product was weighed and set aside a small sample for a melting point determination and a color comparison after the next step. Calculation of the percentage yield of crude acetaminophen (MW = 151.2). was done and recorded in the lab notebook.
Benzyl bromide, an unknown nucleophile and sodium hydroxide was synthesized to form a benzyl ether product. This product was purified and analyzed to find the unknown in the compound. A condenser and heat reflux was used to prevent reagents from escaping. Then the solid product was vacuum filtered.
Performing this experiment, we used the technique called Acid-Base extraction to isolate Eugenol, which is one of the main ingredients of clove oil. Acid-Base extraction is the most efficient method for isolating organic component; it is efficient because it purifies the acid and base mixture based on their chemical identities. We have seen throughout this experiment that acid and base play an important role, when it comes to solubility in water. Our basic knowledge of acid and base is acid is a proton donor and base is a proton acceptor. This ideology helps us to understand why organic compounds are not soluble in water. When compounds tend to be insoluble, we have to use acid and base reaction, to change its solubility. The changes that occurred
When benzoic acid paired with 1.0 M NaOH, it was observed that both compounds were soluble. Upon the addition of 6.0 M HCl into this solution, benzoic acid became insoluble. Benzoic acid was also insoluble in 1.0 M HCl. Ethyl 4-aminobenzoate was found to be insoluble in 1.0 M NaOH and soluble in 1.0 M HCl. But then, after adding 6.0 M NaOH into the test tube C (mixture of ethyl 4-aminobenzoate and 1.0 M HCl), a white powdery solid (undissolved compound) was formed. These demonstrate that both the acid and base became more soluble when they were ionized and less soluble when they were