Obtain two capillary tubes that are sealed at one end. The search on this page works by searching the content. Experimental synthesis of aspirin and melting point purity. Load one tube with your synthesized sample as follows. However, it produces allergylike and toxic effects in many individuals. Also, your melting point range may be greater than 2 degrees. Reduce the sample to a fine powder by using mortar and pestle. Certificate of analysis coa specification sheet pdf. Aqueous solubility of inorganic compounds at various temperatures the solubility of over 300 common inorganic compounds in water is tabulated here as a function of temperature. The data in the table have been derived from many sources, including both the primary literature and evaluated compilations. Salicylamide is used in combination with both aspirin and caffeine in the overthecounter pain remedies. The advanced preparation will vary depending on the nature of the experiment, but some general rules will be applicable to all experiments.
The identification of unknown compounds is an important task of the organic chemist. In this experiment, you will measure the melting point of your synthesized asa product, salicylic acid, a crushed aspirin tablet, and pure asa from a manufacturer. Range of the melting point indicate the purity of the compound. Aspirin melting point essay medicine and health articles. Calculate the average melting temperature, and compare this temperature to the melting point for salicylic acid found in the crc handbook of chemistry and physics. A melting point capillary tube with 12cm depth of fine crystals was loaded. The usefulness of functional groups will be illustrated as well as the use of nmr, ir, and melting point in characterizing a product. Dont heat too fast aspirin product had a melting point range of 110. Aspirin is also used longterm to help prevent further heart attacks, ischaemic. Aspirin is a salicylate drug, often used as an analgesic to relieve minor aches and pains, as an antiinflammatory compound that inhibits cox1. The number of the compound is listed below, so you can easily look it up in the beginning of section three. The aspirin crystals were observed under the microscope and were drawn on the result sheet. The crc handbook of chemistry and physics hbcp contains over 700 tables in over 450 documents which may be divided into several pages, all categorised into 17 major subject areas. The merck index online offers the same highly authoritative information as the print edition in a convenient and easily searchable full text database.
Synthesis of aspirin and melting point determination namehood. Results at the end of the experiment, the result gotten should be a result of 40 60 % yield and a melting point that is around the theoretical melting point of aspirin, which is 5ac 6ac. When available, the triple point pressure is listed. Salicylamide is a nonprescription drug with analgesic and antipyretic properties. Aspirin or acetylsalicylic acid acetosal is a drug in the family of salicylates, often used as an analgesic against minor pains and aches, antipyretic against fever, and antiinflammatory. The values of melting point of acetaminophen are in the range of 168172 0 c. The melting point of a substance depends on pressure and is usually specified at a standard pressure such as 1 atmosphere or 100 kpa when considered as the temperature of. In this twoweek experiment the important area of organic chemistry will be illustrated by the preparation and characterization of two compounds. Due to its wide range, and lower value than that of the theoretical melting point of 6c, it was assessed that the prepared aspirin was impure. Recently, aspirin has been found to be associated with a decreased risk of heart disease and other newly found health benefits. The melting point is the temperature in which aspirin will go from a solid to a liquid. Experiment 22 synthesis of aspirin and oil of wintergreen. The preparation of aspirin, the recrystallisation of aspirin and the melting point determination of aspirin. Chemical properties aspirin should it be the ideal.
The melting point of a substance depends on pressure and is usually specified at a standard pressure such as 1 atmosphere or 100 kpa. This agent exhibits analgesic, antipyretic, and anticoagulant properties. The problem with getting a value for the melting point of an organic substance is the purity of the material. Appendixes include a chronology of the drug that starts in 400 b. Specific inflammatory conditions which aspirin is used to treat include kawasaki disease, pericarditis, and rheumatic fever.
Pdf design synthesis and crystallization of acetaminophen. Acetylsalicylic acid binds to and acetylates serine residues in cyclooxygenases, resulting in decreased synthesis of prostaglandin, platelet aggregation, and inflammation. They also include cautions for giving aspirin to children, older people, and animals, and finally consider aspirin s various brands and forms as well as its alternatives. For more information, see handbook of environmental fate and exposure data. Solubility is defined as the concentration of the compound in a solution that is in equilibrium with a solid phase at the specified temperature. The melting point range of pure aspirin is 8140 c and the melting point range of the salicylic acid starting material is 158161 c. At the melting point the solid and liquid phase exist in equilibrium. Use a boiling water bath to calibrate the thermometer in your melting point apparatus as demonstrated by your instructor. Guide to the crc handbook of chemistry and physics physical. C a list of products containing aspirin, acetaminophen, or ibuprofen. Mar 01, 2007 the problem with getting a value for the melting point of an organic substance is the purity of the material. Dont heat too fast aspirin is only found in individuals who have consumed this drug. Aspirin has different chemical features than any other molecules. A purine alkaloid that occurs naturally in tea and coffee.
Us epa guidelines for the classification determination are listed in 40 cfr parts 261. The purity of sample was tested by determining its melting point range. Fusion melting point data from nist standard reference database 69. Section disposal considerations chemical waste generators must determine whether a discarded chemical is classified as a hazardous waste. This book contains eight freestanding activities that can be used singly or as a coherent package in a wide range of teaching and learning situations for both academic and vocational courses.
Today you will use salicylic acid as the starting material for acetyl salicylic acid aspirin. Advanced preparation and the notebook before coming to the laboratory you will find that some advanced preparation can save significant time and effort in the laboratory. The melting point temperature ranges were 126oc2oc and 129oc4oc for the crude and recrystallized aspirin samples, respectively. If impurities are present in your crude sample, the melting point range for your product will be lower than the range of pure aspirin. Your instructor will demonstrate the use of this apparatus. The merck index online chemicals, drugs and biologicals. The experimental melting point range of aspirin was determined to be 122 2c. A copy of the crc handbook is available in the laboratory. Place the capillary tube in the melting point apparatus. The search on this page works by searching the content of each page individually, much like any web search. Caffeine is a trimethylxanthine in which the three methyl groups are located at positions 1, 3, and 7.
The melting point or, rarely, liquefaction point of a substance is the temperature at which it changes state from solid to liquid. On the anomalous melting point and the decomposition of acetylsalicylic acid. It has a role as a central nervous system stimulant, a ryanodine receptor modulator, an ec 3. Aspirin, an acetyl derivative of salicylic acid, is a white, crystalline, weakly acidic substance, with a melting point of 6 c 277 f, and a boiling point of 140 c 284 f. A complete listing of abbreviations appears on the introductory portions of the tables.
Melting point depends on pressure, so it should be specified. The merck index online search across all of the entries using text names, classifications and numerical melting point, mol weight, boiling point queries. Make sure to record the crc value before you leave the lab. If you know that your compound has a melting point of 77 degrees, the index will list several compounds that match these criteria. Measure the melting temperature of the product using melting temperature apparatus the procedure will have to be split over more than one lesson because the crystals. Typically, tables of melting points are for standard. Aspirin, also known as acetylsalicylic acid asa, is a medication used to reduce pain, fever, or inflammation. A pure sample of a substance will melt at a sharply defined temperature, an impure sample will show a larger range. Finally, in section 3, melting points of various substances are listed in ascending order. Recrystallise the aspirin in the minimum volume of a mixture of ethanol to water 1. Nist chemistry webbook the national institute of standards and technology nist uses its best efforts to deliver a high quality copy of the database and to verify that the data contained therein have been selected on the basis of sound scientific judgment. Aspirin given shortly after a heart attack decreases the risk of death. You are not within the network of a subscribing institution. Once it is a liquid, the boiling point is the temperature that the vapor pressure of the liquid is large enough that bubbles form inside the body of the liquid.
The melting point of a substance is the temperature at which a solid and liquid phase may coexist in equilibrium and the temperature at which matter changes from solid to liquid form. Pittsburgh pa section on practical pharmacy and dispensing, a. Determining the relative percent yield and attained purities of different synthesis processes is vital to the viability of an affordable commercial product for the aspirin market. Manual thin layer chromatography and melting point. Aspirin is an orally administered nonsteroidal antiinflammatory agent. It contains over 11,500 monographs including historic records not available in the print edition. Determine the melting point of the aspirin sample fill a capillary melting point tube to a depth of 0. The notation tp indicates the temperature where solid, liquid, and gas are in equilibrium at a pressure greater than one atmosphere i. Miscellaneous the melting point of acetylsalicylic acid published by permission of the chairman of the committee of revision, u. Experiment 22 synthesis of aspirin and oil of wintergreen goals. The merck index online will be updated regularly with accurate information curated by experts. Due to the limited number of instruments available, you may. Handbook for organic chemistry lab, sections on writing lab reports chapter 6, melting point chapter 10, and thin layer chromatography chapter 7.
I predict that the melting point high range is due to the fact that multiple compounds. Bulletin of the chemical society of japan 1950, 23 1, 2325. Please try againthere was an issue with your search, no terms could be found. Beneficial and toxic effects of aspirin crc press book. Cookie policy crc handbook of chemistry and physics.
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