ANALYSIS14. Prepare a drying-apparatus that uses the water aspirator on the bench. Transfer the Büchner with your solid(crude or recrystallized) to this setup. Dry the solid for approximately 10 minutes. Break the solid clumpsapart every now and then with a spatula to accelerate the drying process.15. Weigh the dried solid so as to calculate a reaction yield for your report.16. Demonstrate the identity and purity of your acetaminophen product (crude and purified, if you were able torecrystallize it) using:TLC: Dissolve a small amount (~10 mg; the tip of a spatula) in a small volume of ethyl acetate (~1-2 mL)in a test tube before spotting on your plate and eluting.Melting point analysis: Pure acetaminophen melts at 169 °C. Pack a small amount (~ 2 mm of height)of solid in a melting point capillary, and record a melting point using the appropriate apparatus. Heatrapidly at first, but slow down when you get near (~20° below) the target melting point to obtain a moreaccurate measurement.6) A melting "point" analysis is a bit of a misnomer; how so? What do we measure whendoing such an analysis? Why the difference? |

Melting point analysis helps in analyzing the purity of the compound.

Answered: A melting "point analysis is a bit of a…

Principles of Instrumental Analysis

7th Edition

ISBN:9781305577213

Author:Douglas A. Skoog, F. James Holler, Stanley R. Crouch

Publisher:Douglas A. Skoog, F. James Holler, Stanley R. Crouch

Chapter33: Automated Methods Of Analysis

Section: Chapter Questions

Problem 33.8QAP

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In the video (liquid-liquid extraction), why is it necessary to turn the separatory funnel upside down and to open the stopcock?
Why is the final product from recrystallization isolated by vacuum filtration and not by gravity filtration?
Earth, a CHEM 40.1 student, extracted a mixture of pigments from the roots of Rubiatinctorum, commonly known as rose madder. Earth spotted the root extract on twohydrophobic silica gel plates. He then placed each plate in separate developing chambers,one containing solvent system WHITE and the other housing solvent system MIX. Earthallowed the chromatograms to develop for around five minutes. Afterwards, he removedthe plates from the containers and placed them inside an iodine chamber. Thechromatograms resulting from the TLC experiment after visualization are illustrated asfollows. The distances travelled by each spot and by the solvents were measured andrecorded in the displayed table.
Extraction of the aqueous salicylic acid solutions with 10% ethyl acetate/hexane (density ~ 0.7 g/ml) will give two layers in the separatory funnel. Will the aqueous layer be the upper layer or the lower layer? If dichloromethane (density ~ 1.3 g/ml) were substituted for the 10% ethyl acetate/hexane solution, which layer would be the aqueous layer?
CREATE A SCHEMATIC DIAGRAM USING THE PROCEDURE: Weighing of standard reagents 1. Make an improvised weighing dish for solid samples (i.e. aluminum foil). Put the foil inside the analytical balance. 2. Press TARE. 3. Weigh accurately 0.4000 grams of NaCl powder in the foil. The reading of the weight must not exceed + 0.0030 g. Note that unused or excess chemicals should never be returned to the stock bottle. 4. Close the balance glass door. Note the actual weight of the NaCl powder that is reflecting on the analytical balance. 5. Transfer carefully the contents in a 150-ml beaker.
How will you increase the measured yield of recrystallized benzoic acid? The receiving flask from hot filtration should not contain a little amount of solvent. Activated charcoal was not introduced to the solution. During cold filtration, a fluted filter paper was used. After hot filtration the solution was filtered immediately.
A TLC plate showed two spots with Rf values of 0.25 and 0.26. The plate was removed from the developing chamber, the residual solvent was allowed to evaporate from the plate, and then the plate was returned to the developing chamber. What would you expect to see after the second development was complete?
MAKE A METHODOLOGY : MATERIALS/ REAGENTS WITH SCHEMATIC DIAGRAM . THE PICTURE UPLOADED SERVES AS A GUIDE, DO THE SAME THING BASED FROM THE PIC. Procedure: Place 20 drops of each of 0.2M CuSO4 in a centrifuge tube. Then add 5 drops of freshly prepared 6M (NH4)2S to each centrifuge tube. Record your observation. Centrifuge the mixtures for 3 mins. and decant the supernatant liquid. Add 10 drops of DI water and 10 drops of 6M HNO3. Stir and boil the mixture in a hot water bath for 5 mins. centrifuge the mixture for 3 mins. Decant the supernatant solution from procedure 3. Discard the To each of the supernatant liquid, add 6 drops of 6M H2SO4. Allow themixtures to cool and 5 drops of DI water. To the mixtures in procedure 4, add few drops of concentrated NH3 until the solution becomes basic. Confirm using a litmus paper. Record your observation. Add 1 drop of 5M NaOH and 1 drop of 0.1 M SnCl2 to the centrifuge tube containing Bi3+ ion , centrifuge and decant the supernatant liquid. To…
Contrast the physical appearance of the crude material before the recrystallization and that of the material isolated after recrystallization.
When isolating the solid after recrystallization using vacuum filtration what solvent should you use to aid in the rinse from the Erlenmeyer flask to the vacuum filter funnel? (Only pick one answer) Group of answer choices: Cold ethyl acetate Cold ethanol Hot ethyl acetate Hot ethanol Hot water Cold water None of the above, it should not be risned
1.What is the purpose of washing the recrystallized solid with solvent during the vacuum filtration step? Why should the solvent be cold?
Take 100ml of the Foam Bath that contains Sodium Laureth Sulphate Cocamide DEA and add sodium chloride solution in incremental amounts whilst stirring, until more than 5% has been added. Note any physical changes that occur during the addition and stirring process.

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A melting "point analysis is a bit of a misnomer; how so? What do we measure when doing such an analysis? Why the difference? |