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Aim of the experiment: The purpose of this experiment is to separate the individual components of Panacetin to find the percentages

of each component in this drug. Chemical structures: Chemical

MF

Structure Structures from http://pubchem.ncbi.nlm.nih.gov/

Water

H2O

Dichloromethane (methylene chloride)

CH2Cl2

Sodium Bicarbonate

NaHCO3

Hydrochloric Acid

HCl

Sucrose

C12H22O11

Aspirin

C9H4O4

Table of physical properties: Chemical MW Moles used MP BP Density (g/mL) 1 1.33 Solubility Potential Hazards Irritant

Water Dichloromethane (methylene chloride) Sodium Bicarbonate Hydrochloric Acid Sucrose

18.02 g/mol 84.92 g/mol 84.01 g/mol 36.46 g/mol 342.3 g/mol 180.15 g/mol

-97C

100C 40C

Slightly soluble Water Water

109C -74C

53C

2.159 1.09

Irritant Corrosive, Poison -

186C

1.587

Water, methanol Water (slightly)

Aspirin (acetylsalicylic acid)

139C

1.35

Irritant

Calculations: 30mL 5% Sodium Bicarbonate = 0.126 g Moles Sodium Bicarbonate = 0.0014998 moles 7.0 mL 6 M HCl = 1.531 g Moles HCl = 0.0419912 moles

Requirements: Glassware: Glass rods Small flasks Glass vials Glass containers or beakers Erlenmeyer flasks Separatory funnel Filter flasks Narrow stemmed funnel Graduated cylinder Evaporation container Filter traps Chemicals: Panacetin Dichloromethane 5% sodium bicarbonate 6 M hydrochloric acid Distilled water Equipment: Fluted filter paper Scale pH paper Rubber tubing Aspirator Scale/balance Rubber stoppers Vacuum source Ring stand Chlorinated solvent recovery container Ice bath or cold water bath Steam bath or hot water bath

Procedure: (from Multiscale Operational Organic Chemistry, p 48-55) Separation of Sucrose: 1. Measure 3.00g of Panacetin. Transfer this sample to a clean and dry 125mL Erlenmeyer flask. 2. Add 50mL of dichloromethane to the flask from step 1. 3. Use glass stirring rod to help dissolve the solid. Rod may be used to break up any solid pieces in the solution. 4. Weigh fluted filter paper. Record weight.

5. Filter mixture by gravity using fluted filter paper, into small flask. Save filtrate for next step. 6. Sucrose is on top of filter paper. Allow filter paper with sucrose to completely dry. Weigh filter paper with sucrose. Record weight. 7. Submit sucrose to instructor if requested. Be sure to weigh and label vial. Separation of Aspirin 1. Transfer filtrate from previous procedure into separatory funnel. 2. Extract the filtrate with a 30mL portion of 5% sodium bicarbonate. Stir with a glass rod until fizzing stops before putting in a stopper and shaking the separatory funnel. 3. Transfer each layer to a different container and return dichloromethane layer to separatory funnel. (Dichloromethane will be in bottom layer.) 4. Repeat step 2. 5. Combine both aqueous extracts in the same container. Save dichloromethane layer for the next procedure. 6. Slowly add 7.0mL of 6 M hydrochloric acid to the aqueous extracts from step 5 while stirring with a glass rod. 7. Test pH of solution. Add more acid if necessary to bring pH down to 2 or lower. 8. Cool mixture in an ice bath for at least 10 minutes. 9. Collect aspirin by vacuum filtration. 10. Wash aspirin on the filter with cold water. 11. Allow aspirin to dry on the filter for a few minutes with the aspirator running. 12. Dry aspirin to constant mass. 13. Weigh aspirin and record. 14. Submit aspirin to instructor in labeled vial. 15. Filtrate can be washed down the drain. Isolation of the Unknown Component 1. Evaporate solvent from dichloromethane solution. Use filter flask attached to trap and aspirator for evaporation. 2. Heat and swirl solution over a steam bath or hot water bath to increase evaporation rate. 3. Cool trap in a beaker of ice water. This will recover dichloromethane. 4. Discontinue evaporation when only a solid residue remains in the flask or no more solvent evaporates. 5. Transfer unknown component to tared vial and allow it to dry to constant mass. 6. Weigh mass. 7. Calculate percent recovery. Divide sum of masses of all components by mass of Panacetin that was used from start. 8. Calculate percentage composition of Panacetin based on total mass of components. Percentages should add up to 100%.

9. Recovered dichloromethane should be disposed in designated chlorinated solvent recovery container.

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