Extraction and Evaporation Recrystallization Essay

1. To the portions of a simulated pharmaceutical preparation, Panacetin, and identifying the unnamed gene of the concoction through and through with(predicate) ex nerve traction and dis rootage methods.2. To learn how to purify by recrystallization, how to teetotal them and how to obtain a thaw prefigure. guardianship ACETANILIDE AND PHENACETIN ARE center of attention AND SKIN IRRITANTS. Minimize clutch with your unbe cognise(predicate) complex.THEORYIn this experimentation, Panacetin, a pharmaceutical preparation will be apart(p) from its voices by making use of their solubilities and superman- pedestal properties. Panacetin contains acetylsalicylic stifling, saccharose and an mystic comp whizznt that whitethorn be either phenylacetamide or phenacetin. Of the terzetto components, only sucrose is indissoluble in the electric original solvent methylene chloride (CH2Cl2 or methylene chloride). The non-water-soluble sucrose stinker be permeateed start i f Panacetin is fragmentised wholly in methylene chloride by gravitational attraction filtration or centrifugation exit the soluble acetylsalicylic acid, phenylacetamide and phenacetin in the ancestor.Although the phenylacetamide and acetylsalicylic acid argon both quite insoluble in water at fashion temperature, the atomic number 11 salinity of aspirin is genuinely soluble in water barely insoluble in dichloromethane. Aspirin, which is a toughened acid faeces be born-again to the salt, sodium acetylsalicylate by stemma with an sedimentary solution of sodium bicenturyate . This salt will migrate from the dichloromethane socio-economic class, in which it is insoluble, to the sedimentary social class, in which it is soluble. The unknown component will stay behind in the solution and mess be unaffectionate by evaporating the solvent from the dichloromethane solution. Adding HCl to the sedimentary solution restores aspirin as an insoluble white cheering.In the th ird experiment, the individuality of the unknown component of Panacetin will be purified. Purification is necessary be fix the insularism upshot may be imperfect deviation traces of piddling quantities in the increase afterwards separation or chemical substance reactions may run prior to or during the separation adding new impurities. The unknown component bottomland be purified by recrystallization, in which an polluted straight dissolves in a igneous (usually boiling) solvent then crystallizes from the sedateed solution in a purer form.METHODS/PROCEDURESThis experiment was followed from the textbook on pages 52-53 for experiment 2 and 59-60 for experiment 3 excluding the microscale part. First, weigh almost 3.00 g of Panacetin and bearalise it to a clean, dry 125 ml Erlenm shopping centerr flask. Add 50 ml of dichloromethane to the flask , fire the mixing with a stirring magnetic pole to break up all(prenominal) lumps. When it appears that no more than of the solid will dissolve, gain vigor the concoction by gravity. Collect the un fade out solid on the filter paper and set it out to dry. Once it has completely dried, reweigh the solid. This compound detached by gravity filtration is known as sucrose.Next, transfer the filtrate to a separatory move and extract it with cardinal 30 ml portions of 5% sodium bicarbonate . For distributively downslope, use a stirring rod to stir the liquid layer until any fizzing subsides before a secure is placed on the funnel and shaken. dichloromethane will be on the do-nothing layer and will be bushed(p) to a different container. Transfer the dichloromethane layer back into the funnel for the bite extraction. The upper layer will be transferred in an Erlenm oculusr flask and will be used for rec everyplacey of acetanilide. Combine the cardinal aqueous solutions in the same container and interchange taste slowly with 6M HCL to bring it to a pH of 2. Cool the mixture to room temperat ure or below while swirling the flask on occasion in an ice bath. Collect the aspirin by vacuum filtration. Wash the aspirin on the filter with cold distilled water. prohibitionist the specimen thoroughly before measure and leave it in the hood for the bordering lab schedule.Before proceeding to recrystallization, triturate the compound with 20 ml of hexane. Crush the solid with a stirring rod and filter. Recrystallize the unknown drug component from experiment 2 by boiling it with just adequate water to dissolve it completely, then permit it cool to room temperature then to 0 C. In order to induce crystallization, it would be helpful to scratch the walls of the flask so that crystals would have a surface to isolate to. Use vacuum filtration to isolate the sample then dry the ingathering to a constant mass and weigh in a tared vial.Grind a small amount of the dry unknown component to a fine powder on a interpret glass exploitation a spatula. Divide the solid into quatern ity personify portions. Combine portions 1 and 2. commingle bag portion 3 with an approximately live amount of finely fundament acetanilide and mix portion 4 with an approximately equal amount of finely ground phenacetin. Obtain the melt down heading figure of speechs of the purified unknown (portions 1 and 2), mixture with acetanilide and mixture with phenacetin. Each thawing phase should be measured on two samples- more than that if warming points are imprecise or accurate.Safety Issues (all of these are taken from MSDSonline.com)1. phenylacetamidePotential Acute mother uncivilised in show window of eye contact (irritant), of aspiration, of inhalation. roughly hazardous in case of fell contact(irritant).Potential chronic health make Hazardous in case of eye contact (irritant), of ingestion, of inhalation. S take downly hazardous in case of peel reach contact (irritant).2. Phenacetin pump and pelt irritant3. DichloromethanePotential Health doInhalationCauses petulance to respiratory tract. Has a strong narcotic piece with symptoms of mental confusion, light-headedness, fatigue, nausea, vomiting and headache. Causes establishment of carbon monoxide in blood which affects cardiovascular placement and interchange nervous system. Continued pictorial matter may realise increase light-headedness, staggering, unconsciousness, and in eon death. Exposure may make the symptoms of angina pectoris ( chest of drawers pains) worse. Ingestion may shell incitation of the gastrointestinal tract with vomiting. If vomiting provides in aspiration, chemical pneumonia could follow. Absorption through gastrointestinal tract may produce symptoms of central nervous system depression ranging from light headedness to unconsciousness. shin sufferCauses irritation, redness and pain. lengthy contact can pay off burns. swimming degreases the flake off. whitethorn be absorbed through skin.Eye ContactVapors can cause eye irritation. Contact can produce pain, inflammation andtemporal eye damage.Chronic ExposureCan cause headache, mental confusion, depression, liver make, kidney effects, bronchitis, loss of appetite, nausea, pretermit of balance, and visual disturbances. Can cause dermatitis upon pro doured skin contact. Methylene chloride may cause cancer in humans. Aggravation of pre-existing ConditionsPersons with pre-existing skin disorders, eye problems, impaired liver, kidney, respiratory or cardiovascular incline may be more sensitised to the effects of this substance.4. AspirinEye ContactModerate Eye Irritation Signs/symptoms may allow redness, swelling, pain, tearing, and blurred or logy vision. unclothe ContactModerate Skin Irritation Signs/symptoms may allow in localise redness, swelling, itching, and dryness. may be absorbed through skin and cause target organ effects. InhalationNo health effects are expected.Ingestion may be stabbing if swallowed.Gastrointestinal Irritation Signs/symptoms may admit abdom inal pain, nausea, diarrhea and vomiting. tell ingestion may cause may be absorbed following ingestion and cause target organ effects. stigma Organ EffectsPro spacioused or repeated picture show may causeAuditory Effects Signs/symptoms may include hearing impairment, balance dysfunction and peal in the ears. Clotting Disorders Signs/symptoms may include increased blood clotting time and internal bleeding (hemorrhage). Liver Effects Signs/symptoms may include loss of appetite, encumbrance loss, fatigue, weakness, abdominal tenderness and jaundice.Central unquiet System (CNS) Depression Signs/symptoms may include headache, dizziness, drowsiness, incoordination, nausea, slowed reaction time, slurred speech, giddiness, and unconsciousness. Kidney Effects Signs/symptoms may include reduced or oblivious urine production, increased serum creatinine, lour back pain, increased protein in urine, and increased blood urea nitrogen (BUN). pneumonic Edema Signs/symptoms may include ch est discomfort, shortness of breath, significant cough with sparkling sputum production, bluish colored skin (cyanosis), increased heart rate, respiratory bereavement and may be fatal. Single impression may causeImmunological Effects Signs/symptoms may include alterations in the number of circulating repellent cells, allergic skin and /or respiratory reaction, and changes in immune function.5. Sodium BicarbonateEMERGENCY OVERVIEW type whitethorn cause respiratory tract irritation. Causes eye and skin irritation. Target organs Blood, kidneys, heart, liver, eyes, skin.Potential Health EffectsEye Causes eye irritation.Skin Causes skin irritation. May be harmful if absorbed through the skin. Ingestion May be harmful if swallowed. Causes gastrointestinal tract irritation. Inhalation May cause respiratory tract irritation. May be harmful if inhaled. Chronic May cause liver and kidney damage. Adverse reproductive effects have been reported in animals. Laboratory experiments have endp ointed in mutagenic effects. Chronic exposure may cause blood effects.6. Hydrochloric AcidPOTENTIAL wellness EFFECTSInhalation May cause irritation (possibly severe), chemical burns, and pulmonary edema.Skin contact May cause irritation (possibly severe) and chemical burns.Eye contact May cause irritation (possibly severe), chemical burns, eye damage, and blindness.Ingestion Not a believably route of exposure.Target Organs completed Respiratory System, Skin, EyeChronic Effects Repeated or prolonged exposure to dilute solutions may top in dermatitis. Discoloration of the teeth may occur as a result of long term exposure.Interaction with Other Chemicals Which erect Toxicity none known aesculapian Conditions Aggravated by Exposure None knownOBSERVATIONS/RESULTSIn Experiment 2, the extraction of substances from one another is infantryd on the differences in their physical and chemical properties. Approximately, 3.0029 g of panacetin was weighed and completely dissolved in 50 ml of dichloromethane and filtered. The residue was left(a) to dry and weighed (sucrose). Then 30 ml of NaHCO3 was added to the filtrate. This solution was transferred into a separatory funnel. This formed two layers. Top layer was the organic layer (NaHCO3) described as a invite liquid. Bottom layer was the aqueous layer and was yellow in color. The filtrate was wash twice with NaHCO3. HCl was added to the aqueous solution until the pH equaled to 2.0. It was filtered through vacuum filtration and allowed to dry until the coterminous weeks lab. This filtrate is known as aspirin. Meanwhile, the unknown in the organic layer was also allowed to settle for the next experiment.In experiment 3, before we went to do recrystallization, we first did trituration of the unknown by adding 20 ml of hexane. We crushed the solid and filtered. evening with the addition of approximately 27 ml of boiling water into the compound, it started to dissolve. That was the first roll that we have acetanili de as our unknown. We went before and continue heating and swirling the solution over a hot plate. thither was the formation of brown oil-like globules. We were then asked to decant the sporty liquid from this solution. This clear liquid was allowed to cool to room temperature then to 0 C. on that point was formation of white crystals at the skirt of the beaker. Through vacuum filtration, we were adapted to filter the product, weighed and used for melting point quantity of the unknown.The solid was divided into 4 equal parts. First 2 parts were combined, tertiary part was mixed with acetanilide and the die hard part was mixed with phenacetin. After winning the melting points of all these 3 substances we were suit adequate to identify the unknown product to be acetanilide.No giant issues encountered during this experiment. Transferring whatever products as well as the final crystals from watch glass and filter paper and leaving some products were crucial to get the most f inal product. This relieves why the percent recovery for the unknown was low. Some crystals fell off or didnt transfer to the filter paper. Even though the % recovery was comparatively low (88.4079%), this experiment still produced a 0.6898 g of product.DISCUSSION/CONCLUSIONThis experiment was focused on two of import objectives. First, the analysis of panacetin to find out what percentages of sucrose, aspirin and the unknown component it contains. Second, to find out whether the unknown is acetanilide and phenacetin. A big part of the composition of panacetin was made up of the unknown. We were able to determine the composition of sucrose to be 17.95 %, Aspirin 26.93% and the unknown to be 55.12% After following the experiment procedures, we were able to purify through recrystallization the end product to be acetanilide. This is an odorless white perspicuous solid substance which has a melting point of 114 C. Our experimental value for acetanilides melting point was 117 which i ndicates that the result had a very narrow range and scraggy to the literature value. I would consequently conclude that we had isolated a close to pure product of acetanilide with bantam impurities present.1. a. Describe any evidence that a chemical reaction occurred when you added 6 M HCl to the solution of sodium acetylsalicylateA chemical reaction in additionk place upon the addition of 6M HCl to a solution of sodium acetylsalicylate because a sicken formed known as aspirin.b. explicate why the changes that you observed took place.The observed change took place as a result of the acid reacting with the salt forming a compound insoluble in water.2. Describe any explain the possible effect on your results of the following experimental errors or variations. In each case, specify the component (s) whose percentage(s) would be too high or too low.a. After adding dichloromethane to Panacetin, you didnt stir or shake the mixture long enoughImproper stirring or shaking of the mixt ure will result in incomplete dissolution of the panacetin mixture. There will be loss of some solid analytes during filtration. The recovered amounts will be lower than they should be leading to a final percentage to be low.b. During the NaHCO3 extraction you failed to mix the aqueous and organic layers thoroughly.If the aqueous and organic layers were not thoroughly mixed the acid would remain in the solution and the extraction would be less cost-efficient resulting to a low percentage yield.c. You mistakenly extracted the dichloromethane solution with 5 % HCl quite anthan 5 % NaHCO3.If 5% HCl is used kind of of 5% NaHCO3 that would protonate the aspirin and keep it in the organic solution making the aspirin, acetylsalicyclic acid.d. rather of using pH paper, you neutralized the sodium bicarbonate solution to pH 7 using litmus paperAt ph7 the bicarbonate wouldnt be able to act as a base and extract a proton because at pH of 7 it would protonate itself so it wouldnt be able to react with aspirin.5. Write a balanced reaction equations for the reactions involved a. When aspirin dissolves in aqueous NaHCO3C9H8O4 (aq) + NaHCO3 (aq) > C9H7O4Na (aq) + CO2 + water supply wispy acid weak base truehearted Base Strong acidb. When Aspirin is precipitated from a sodium acetylsalicylate solution by HCLC9H7O4Na + HCl - C9H8O4 + NaCl Strong Base Strong acid Weak Acid Weak BaseAssuming that both reactions are spontaneous under the standard conditions, guess the stronger acid, stronger base, weaker acid and weaker base in each equation.Experiment 31. a. What is the minimum quite a little of boiling water needed to dissolve 0.200 g of phenacetin?b. About how a lot phenacetin will remain dissolved when the water is cooledto room temperature?c. Calculate the uttermost mass of solid (undissolved) phenacetin that can be recovered when the cooled solution is filtered.0.200 g-0.0125 g (amount soluble in cold water)= 0.1875 g2. An unknown compound X is one of the four co mpounds listed in table 3.2. A mixture of X with benzoic acid melts at 89 C, a mixture of X with phenyl succinate melts at 120 C and a mixture of X with m-aminophenol melts at 102 C. Give the identity of X and explain your reasoning.X is phenyl succinate.When a compound mixes with a different compound, the melting point of the mixture will be lower than the melting points of either of the pure compounds. Basing from the table, the melting point of pure benzoic acid is 121 C but when mixed to X, it went down to 89 C. Likewise with O-toluic acid and m-aminophenol. Since the melting point of mixture X with phenyl succinate has a melting point of 120 C, the melting point of pure X must(prenominal) be equal or closer to 121. blend X with phenyl succinate did not change the melting point thus X must be phenyl succinate.