Fractional Distillation

PA Sta t e Sta n d a r d s : 3.7.10.B Apply appr o pri a t e instru m e n t s and app a r a t u s to exa m i n e a variety of object s and proc e s s e s . 3.7.12.A Apply adv a n c e d tools, mat e ri als and tech ni q u e s to answ e r com pl e x que s tion s. 3.4.10.A Explain conc e p t s abo ut the struct ur e and prop e r ti e s of ma tt e r. 2.4.11.E Demo n s t r a t e ma t h e m a t i c a l solution s to proble m s . 1.2.11.A Read and und e r s t a n d the centr al cont e n t of inform a tio n al texts and docu m e n t s in all aca d e m i c are a s .

Introduction: Fractional distillation is a method to separate mixtures of liquids with boiling points that are close to each other. When a solution is distilled in fractions, it passes through a series of redistillations that increase the purity of the final products. The column (condenser) is packed with a nonreacti e material in order to increase the surface area. This column is referred to as a fractionating column. !s the liquid is heated, apor will begin to rise. The apors condense as they come in contact with the cooler surfaces in the fractionating column. "ontinued heating of the liquid causes more apors to rise. The condensed apors in the column re# apori$e and mo e up the column. !s this process is repeated many times, the component which apori$es the easiest (lowest boiling point) reaches the top of the column first and is collected in the collection ial. The other components will be collected in order of ascending boiling points. This process is also useful in separating mixtures with many different liquids. "rude oil, for example, is separated in towers that are %&' feet high. (ne hundred different components are separated from )'',''' barrels of crude oil per day. Guiding Question:
*lease answer the following question before beginning the lab.

*redict the order in which the following chemicals would condense after distillation.

%#propanol methanol +* ,-.) ." +* &/.& ."

acetone +* /0.- ."

Fraction al Distillation

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Equipment / Materials 1 glass ials %''#m2 beaker +oiling chips "rystalli$ing 3ish 3igital thermometer 4ot plate Opt. Equipment/Materials %#propanol !cetone 8as "hromatograph 9imwips

5ce 6icroscale kit 6ixture of organic liquids 7and 7teel wool

2aptop 6ethanol *rinter 7yringe

Safety: Wear safety glasses at all times in the lab. 3o O! use open flames. (pen flames may ignite the fumes of the distillation. 3o not spray water into the sand bath # hot sand will spray and ha e the potential to burn someone, especially in the eyes. When using a hot plate with a sand bath, do not heat the hot plate on a high setting. "lamp both the beaker and condenser securely but not tight enough to break the glassware. "rocedure: %. 5f using the 8" to analy$e the fractions, run a sample of the mixture before you begin the distillation. ). *our about 1 # 0 m2 of the unknown mixture into the short necked round#bottom flask. !dd a boiling chip. 1. 7et up your apparatus as Figure % indicates. !s you set up, be sure to check that the rubber connectors are not torn. 5f needed, puncture a hole in a rubber septum to fit the digital thermometer. 0. *lace ice and water in the beaker surrounding the ser e as an ice bath. Figure 1. collection ial to

Fraction al Distillation

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&. 4eat slowly with a hot plate until the liquid gently boils. :ote the condensation of the apor as it rises in steps through the steel wool. (;emember to not set the hot plate on a high setting.) /. The temperature will increase rapidly at first as the apor condenses on the end of the thermometer. !t this point, the temperature will remain fairly constant, around &- <". This is the boiling point of the first liquid. 2iquid will start to drip into the ial. The temperature will decrease slightly before beginning to increase further. !s the temperature decreases, carefully remo e the ial, label it =!,= and place a new ial in the cold water. The second component should begin to condense and drip into the ial around /& <", as this is the boiling point of the second liquid. !s the temperature decreases, carefully remo e the ial, label it =+=, and place it in a new ial. The third component should begin to condense around ,- <", as this is the boiling point of the third liquid. "ollect some of the third fraction, but do O! allow the flask to boil dry. 2abel this ial ="=. "arefully remo e the thermometer, and let the apparatus cool completely.

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%'. "arefully disassemble the distillation apparatus, and place the pieces in the appropriate spaces in the microscale kit. Data !a#le: Fraction $ % & +oiling point 5dentity

Questions: %. 4ow would using a longer column affect the purity of the components collected? ). 4ow would using a longer column affect the time required to completely separate the mixture? 1. 4ow would using more packing material in the column affect the purity of the components collected? 0. 4ow would using more packing material in the column affect the time required to completely separate the mixture?

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Optional E'tension: Identification and "urity using Gas &(romatograp(y %. Turn on the laptop and log on. 2. 3. Turn on the GC plug it into the lapto p. Start the Peak Sam pl e softw ar e . A dat a acquisition syst e m popu p should app e a r with phra s e s like initializing, waking up, signing on, settin g mod e s , and calibratin g. "lick on edit menu, then select channels. @nder "hannel %, pick Temperature. "lick on the numbers to highlight them, then click "hange. "hange the numbers as followsA Start 150 C Hold 10 minut e s Ram p 0 degr e e / min Until the te m p e r a t u r e is 150 C Be sure the time scale start s at zero and ends at 10 min. Use the arrows to adjust. Clean the syring e by rinsing it 10 -- 15 time s with one of the stan d a r d s . With the plung e r fully depr e s s e d , plac e the nee dl e into the sa m pl e. Slowly draw up the plung e r to obt ain a sa m pl e in the syring e. Remov e the syring e from the sa m pl e . Disch ar g e this sa m pl e into the sink or onto a Kimwipe. Depre s s the plung e r, and put the syring e ne e dl e back into the sa m pl e. Draw up a seco n d sa m pl e and disch a r g e it. Repe a t . Do not pu s h on th e plu n g e r wh e n th e n e e d l e is insi d e a sa m p l e . Place the syring e ne e dl e back into the sa m pl e and withdr a w over 1 microliter. Remov e the ne e dl e from the sa m pl e bottle, the n depr e s s the plung e r to the 1 microliter line. Wipe the nee dl e with a Kimwipe. Click on the Z or butt o n on the run scre e n to zero the curre n t . Insert the ne e dl e carefully into the injection port of the GC until the entire ne e dl e is inside the instru m e n t .

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10. Inject the sa m pl e and start the dat a collection simult a n e o u s ly by depr e s si n g the syring e plung e r and pres sin g the spac e bar on the comp u t e r at the sa m e tim e. %%. When the sample peak of a standard returns to baseline, the run may be stopped by pressing the end button on the computer. !fter pressing end, print the graph. +e sure to label the graph.

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12.

Repe a t ste p s 4- 9 for the oth er sta n d a r d s and the collect e d fraction s. Wh e n runni n g an unk n o w n sa m p l e , b e cer t a i n to let th e dat a coll e c t lon g en o u g h to g e t all po s s i b l e p e a k s .

Data and &alculations: 5dentify the chemicals in the fractions by comparing the retention times in the fractions to those of the standards. @se the area of the peaks to determine the precent compostion of each fraction. "reate an organi$ed method of presenting your data and results.

Fraction al Distillation

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