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Separation of the Components of A Ternary Mixture

9/14/2011

Introduction
This lab was the separation of the components of a ternary mixture. The three objectives in this lab were: 1. Learn the different separation techniques which include; sublimation, extraction, decantation, filtration and evaporation. 2. Separate three components in a mixture using the separation techniques learned. 3. Determine the mass percentages of each of the three components present in a mixture. In order to separate the components of a ternary mixture, one must understand what a mixture is and the different separation techniques that can be used. Mixtures are defined as a physical combination of two or more pure substances. Separation techniques are used to separate components that are not chemically combined. Because only physically combined mixtures are being used in this experiment, the separation techniques described in this experiment are based on physical changes, rather than chemical changes.

5 separation techniques
1. Sublimation- Involves the heating of a solid that passes directly into a gaseous phase without transitioning into a liquid phase. The reverse process where a gas goes into the solid phase is called deposition or condensation. 2. Evaporation- Involves the heating of a mixture in order to separate a volatile liquid in the form of a vapor, while the residual components remain dry. 3. Extraction- Involves using of a solvent that selectively dissolves only a single component while the other components remain insoluble. 4. Filtration- Involves separating a liquid from a solid using a porous material such as filter paper. The porous material allows the liquid to pass through it but not the solid. 5. Decantation- Involves the separation of a liquid from insoluble solid sediment by carefully pouring the liquid without disturbing the solid.

Mixtures can be classified by composition as either a: 1. Homogenous Mixture: a mixture classified by having a uniform composition and appearance throughout. This mixture can have all of its components in one phase. 2. Heterogeneous Mixture: a mixture classified by having a composition that varies from one region to another. These mixtures can have components in different phases.

In this experiment a mixture containing Naphthalene (C H ), common table salt (NaCl), and sea sand (Si0 ) will be separated according to a separation scheme shown in Figure A. The separation of this mixture consists of 3 main steps: 1. Sublimation of naphthalene. 2. Extraction of NaCl using water as a solvent. 3. Recovering of NaCl and sea sand by evaporating water.

FIGURE A

Mixture Separation Scheme


Mixture: Naphthalene, NaCl, Sea Sand Heat in Fume Hood

Residue: NaCl, Sea Sand

Naphthalene Sublimes

Extract with H O

Filter

Solution: NaCl (aq)

Residue: Wet Sea Sand

Evaporate HO

Evaporate HO

NaCl(s)

Sea Sand

Procedure
A. Preliminary Steps
1. Obtain a sample of the mixture, record the unknown code number on the data sheet. 2. Obtain a wide mouth 250 ml Erlenmeyer flask (Figure 1) and carefully weigh it to the nearest 0.01 g on the top loading scale (Figure 2) and record its mass on the data sheet. 3. Place about 2 g of the mixture into the Erlenmeyer flask and carefully weigh it to the nearest 0.01 g with the top loading scale and record its mass on the data sheet. 4. Determine the mass of the mixture y subtracting the mass of the empty Erlenmeyer flask from the mass of the Erlenmeyer flask containing the mixture and record the calculated mass onto the data sheet.

B. Sublimation of Naphthalene
*NOTE: The sublimation of naphthalene must be carried out in a fume hood. 1. Set up a hotplate (Figure 3) in the fume hood (Figure 4) and turn the hotplate on. 2. Place an evaporating dish (Figure 5) containing ice on top of the Erlenmeyer flask containing the mixture (Figure B-1). *Make sure that no water gets on the underside of the evaporating dish or inside the flask. 3. Place the sublimation assembly on the hotplate that is in the fume hood. Soon you will notice a solid will start collecting on the underside of the evaporating dish. Continue heating for 15 minutes. 4. Carefully remove the assembly from the hotplate. 5. Carefully remove the evaporating dish from the Erlenmeyer flask and collect the solid by carefully scraping it off with a spatula (Figure 6) into a separate container. (this will be disposed of later) 6. Stir the contents of the Erlenmeyer flask with a glass rod (Figure 7). (REPEAT STEPS 3-5) 7. Combine all of the scrapped naphthalene from the underside of the evaporating dish and dispose of it into the correct labeled waste container. 8. Allow the Erlenmeyer flask to cool down. Once it is cool weigh the Erlenmeyer flask with the remaining solid in it and record the mass onto the data sheet. 9. Calculate the mass of the sublimed naphthalene by subtracting the mass of the Erlenmeyer flask with the remaining solid from the mass of the Erlenmeyer flask with the original mixture. After calculations record the calculated mass onto the data sheet.

C. Separation of the water insoluble solid


1. Add 25 ml of distilled water to the solid in the Erlenmeyer flask. Heat and stir for 5 minutes. The NaCl should dissolve fully in the water, while the sea sand remains insoluble. 2. Weigh a clean 150-ml beaker (Figure 8) with 2-3 boiling chips (Figure 9) to the nearest 0.01 g and record its mass onto the data sheet. 3. Fold a piece of filter paper (Figure 10) according to the steps shown in figure C-1 4. Place the folded filter paper inside a funnel (figure 11). The paper will need to be wetted with water, once wet adjust the filter paper so that it lies flat on the walls of the funnel. 5. Assemble the apparatus for gravity filtration (Figure 12) as it is shown in Figure C-2, placing a clean beaker (beaker 1) under the funnel. 6. Pour the mixture contained in the Erlenmeyer flask into the gravity filtration apparatus and collect the filtrate into beaker 1 as shown in Figure C-3 *DO NOT DISCARD THE FILTER PAPER: the filter paper containing the wet sand needs to be set aside for part D. 7. Rinse the Erlenmeyer flask with 5 ml of water, pour over the residue in the funnel. And add the liquid to the filtrate in beaker 1. * REPEAT THIS STEP ONCE MORE. 8. Place beaker 1 on the hotplate and heat. As the amount of liquid reduces, the NaCl dissolved will start to precipitate as a white solid. When the liquid is fully evaporated, allow the beaker to cool down to room temperature. 9. Weigh beaker 1 with the dry NaCl, and record the mass on the data sheet. 10. Determine the mass of the recovered NaCl by subtracting the mass of the empty beaker 1. Once calculations are done record the mass of the recovered NaCl on the data sheet. Figures of Steps B & C

Figure B-1

Figure C-2

Figure C-1

D. Drying the Sea Sand Sample for Recovery Calculations


1. Weigh a second clean 150-ml beaker (beaker 2) to the nearest 0.01 g and record its mass on the data sheet. 2. Transfer the wet sand from the filter paper to beaker 2. 3. Place beaker 2 with the wet sea sand on the hotplate and heat the sand to dryness. When the sand is completely dry, the sand should be free flowing. 4. Allow the sand to cool to reoom temperature. Weigh the beaker containing the fry sand to the nearest 0.01 g and record this mass onto the data sheet. 5. Determine the mass of the recovered sea sand by subtracting the mass of the empty beaker 2 from the mass of the beaker containing the dry sand. Record the mass of the recovered sand on the data sheet.

E. Calculations and Equations


1. Calculate the percent yield using the following formula:  % yield= (1.73g/1.76g)x100= 98.3%     

2. Calculate the percentage of each component in the mixture using the following
formula:

% Naphthalene= (0.13g/1.76g)x100= 7.39% %NaCl= (1.23g/1.76g)x100= 69.9% %Sea sand= (0.37g/1.76g)x100= 21.0% = 98.3% (% Yield)

Equipment
Here are some pictures of the equipment used in this experiment:
Figure 2 Figure 3

Figure 1

Figure 4

Figure 7 Figure 5 Figure 6

Figure 8 Figure 9 Figure 11

Figure 10

Figure 12

Unknown Code #:

Data and Calculations

588

Data Sheet Separation of the components of a Ternary Mixture 1. Mass of Erlenmeyer flask 126.74 g 2. Mass of Erlenmeyer flask + Mixture 3. Mass of Mixture (2)-(1) 4. Mass of Erlenmeyer flask and solid after sublimation 5. Mass of naphthalene (2)-(4) 6. Mass of beaker 1 7. Mass of beaker 1 and NaCl 8. Mass of NaCl (7)-(6) 9. Mass of Beaker 2 10. Mass of beaker 2 and Sea sand 11. Mass of sand (10)-(9) Calculations 12. Mass of recovered solids (5)+(8)+(11) 13. Percent Yield %=[(12)/(3)] x 100 14. Percentage of naphthalene %=[(5)/(3)] x 100 15. Percentage of NaCl 1.73 g 98.3% 7.39% 69.9% 128.5 g 1.76 g 128.63 g 0.13 g 67.09 g 68.32 g 1.23 g 66.36 g 66.73 g 0.37 g

%=[(8)/(3) ]x 100 16. Percentage of Sea sand %=[(11)/(3)] x 100

21.0%

Results and Discussion


In this lab certain separation techniques were used and learned. Sublimation of naphthalene was done in part B. First an empty Erlenmeyer flask was obtained and weighed. 2g of an unknown mixture was placed into the flask and weighed again. The mass of the mixture was obtained by subtracting the weight of the empty Erlenmeyer flask from the Erlenmeyer flask containing the mixture. The mass of the mixture was 1.76g according to calculations. Next an evaporating dish containing ice was put on top of an Erlenmeyer flask containing the unknown mixture. This assembly was placed on the hot plate in the fume hood. It was noticed that a white solid started collecting on the underside of the evaporating dish. After heating for another 15 minutes the assembly was removed from the hotplate. Using a spatula the solid under the evaporating dish was scraped off and put into a beaker. After the solid was scraped off, the remaining solid in the Erlenmeyer flask was stirred with a glass rod. The assembly was heated again for 15 minutes and the solid under the dish was added to the beaker containing the previous solid that was scraped off. The contents of the beaker were disposed of in the labeled waste container. After heating the Erlenmeyer flask for a second time it was set aside to cool down. Once it was completely cool, the Erlenmeyer flask with the remaining solid was weighed. The mass of the sublimed naphthalene was calculated by subtracting the mass of the Erlenmeyer flask with the remaining solid from the mass of the Erlenmeyer flask with the original mixture. After calculations the mass of the naphthalene came out to be 0.13 g. Part C extraction was observed in separation of the water insoluble solid. The Erlenmeyer flask from part B was used. 25 ml of distilled water was added to the solid in the Erlenmeyer flask, it was then heated while stirred occasionally for 5 minutes. The NaCl was said to dissolve leaving only the insoluble sea sand in the flask with the water. Three boiling chips were added to a clean 150 ml beaker and were weighed to the nearest 0.01 g. Filtration was also observed in this experiment, first filter paper was folded and wetted then placed flat into a funnel. The funnel was placed into the apparatus for the gravity filtration. The beaker containing the boiling chips was placed under the funnel. The remaining mixture found in the Erlenmeyer flask was then poured into the gravity filtration apparatus and the filtrate was collected into the beaker with the boiling chips. After that the funnel was removed and an additional 5 ml of distilled water was put into the flask and poured over the residue found in the funnel. The 5 ml of water

was poured twice over the funnel. After all of the residue and filtrate was filtered the beaker was placed on a hotplate, the water boiled for a few minutes and the amount of liquid reduced quickly. The NaCl that was dissolved started to precipitate into a white solid. Once all of the liquid was gone the beaker was taken off the hotplate to be cooled to room temperature. Once it was fully cooled the weight of the beaker containing now dry NaCl was taken. The mass of the recovered NaCl was determined by subtracting the mass of the empty beaker and the mass of the beaker containing the dry NaCl. According to calculations the mass of the recovered NaCl was measured at 1.23 g. In part D, the sea sand had to be dried for the recovery calculations on the data sheet. To dry sea sand first the sand was placed into a clean 150 ml beaker and was weighed. The wet sand was then transferred from the filter paper into the clean beaker. The beaker containing the sand was then placed onto the hot plate, until the sand had dried completely. The sand was then cooled to room temperature and weighed to the nearest 0.01 g. The mass of the recovered sea sand was determined by subtracting the mass of the empty beaker from the mass of the beaker containing dry sea sand. The mass of the recovered sea sand was calculated at 0.37 g. For the Calculations part of the experiment percent yield and percentages of all substances was found. The percent yield was found by dividing the mass of the recovered solids by the mass of the mixture, then multiplying the answer by 100. (1.73/1.76)x100= 98.3%. The percentage yield for this experiment came out to be 98.3%. The makeup of that 98.3% is divided up between naphthalene at 7.39%, NaCl at 69.9% and sea sand at 21.0%. Some errors that could have been made in this experiment include: 1. Not measuring the 2 grams of unknown mixture in the beginning of the experiment. 2. Rushing through the experiment by not letting the sand fully dry, not letting the naphthalene sublimate for 30 minutes, or not letting the NaCl dissolve in the water. 3. In the lab book it was stated not to let the water boil during the heating of the filtered water. In the lab though the water was allowed to be boiled, which may have disturbed the experiment. 4. Reasons why percentage yield may have differed from 100% could also be human error in calculations and the mass of the recovered solids was less than the mixture %. 5. If water got on the underside of the evaporating dish or inside the flask during naphthalene sublimation, it would affect the naphthalene from sublimating into a gas.

Post Lab Questions


1. What was your percent yield? The percent yield for this experiment was 98.3%. This was found by dividing the mass of the recovered solids by the mass of the beginning mixture and multiplying by 100. (1.73g/1.76g)x100= 98.3% 2. Give two reasons why the percentage yield can differ from 100%. Do not include in your answer explanations like Human error or instrumental error . Two reasons why the percentage yield could differ from 100% include rushing and not letting all of the NaCl dissolve or not letting the naphthalene sublimate completely, and if the mass of the recovered solids was less than the mixture %. 3. If a student was unable to completely dissolve all the NaCl in the water, what effect would this have on the calculation of the percentage yield? Would the percentage yield be higher, lower or unaffected? The percentage yield would be lower because the mass of the NaCl would not have been fully calculated in the mass of recovered solids. When the NaCl precipitates into a white solid it would be a smaller amount thus affecting the percentage yield. 4. The sand was not completely free of water when the mass was reported on the data sheet. How does this affect the calculated percentage composition of the sand in the mixture? Would the calculated percentage composition of the sand be higher, lower, or unaffected? The percent composition would be higher because the mass would be calculated higher in the sand. The water would weigh the sand down and you would not be taking the mass of the sand you would be taking the mass of the sand plus the water in it.

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