GENERAL CHEMISTRY 201 LABORATORY FORMAL REPORT

Separation of an Unknown Binary Mixture by Simple and Fractional Distillation

*Reyes, Gail Margarette D.A. Rosario, Mary Ellenohr D.R. Sola, Jennifer S. Group 14 Department of Chemistry, College of Science University of Santo Tomas, Espaa, Manila 1008

Abstract. The experiment focuses on the proper distillation of an unknown binary compound using simple and fractional distillation. The data obtained during this experiment were the % low boiling component which is equal to 12% and the % high boiling component which is equal to 20%. A graph was made in order to compare the results of both the fractional and simple distillation. The graph was also used to determine certain numerical values needed for the computation of both the % high and low boiling component.

INTRODUCTION The process of distillation takes advantage of differences in boiling points. It can separate liquids in a mixture that differ in boiling point just by a few degrees Celsius. The process of distillation is done by converting the substance with the lower boiling point to gas. The gas is then changed back into a liquid and is collected in another container. There are, however, several types of distillation set-ups but this experiment used only two the simple and factional distillation. Simple distillation does not guarantee a pure distillate because the hot vapors are directly channeled to the condenser which cools and condenses the vapor. It involves only a single vaporization-condensation cycle. It is most useful for purifying a liquid that contains either nonvolatile impurities or small amounts of higher or lower-boiling impurities. Fractional distillation allows for several vaporization-condensation cycles in a single operation. It can be used to separate liquids with comparable volatilities and to purify liquids containing relatively large amounts of volatile impurities. The only difference in the apparatus used on both distillation set-ups is the fractionating column which contains a packing material. This is used only on the fractional distillation set-up.

GENERAL CHEMISTRY 201 LABORATORY FORMAL REPORT The objectives of the experiment are to separate the components of an unknown mixture, determine how many components are in the mixture, conduct a distillation curve, calculate the percentage of each component and compare the efficiency of simple and fractional distillation in separating the liquid mixture. EXPERIMENTAL Eight pieces of 13x100 test tubes were calibrated to an amount of 3mL. The glasswares needed to perform the simple/fractional distillation with aluminum foil coiled as packing material were laid out. The apparatus for simple and fractional distillation were assembled as shown in the setup below. Figure 1.1 Simple Distillation Set-Up Figure 1.2 Fractional Distillation Set-Up

An amount of 25mL of the unknown assigned binary mixture was placed in a 50mL distilling flask with 2pcs of boiling chips. The wtaer in the condenser was gently turned on. The distilling flask was heated until the first drop of the distillate reached the reciever. The temperature of the first drop was recorded and the heat was adjusted to a rate of 1-2 drops per second. The readings after every 3mL of the distillate collected were taken. The temperature versus volme of the distillate during the entire distillation was recorded . The temprature 1st drop corresponded to zero volume. The distillation was stopped when an amount of 1mL remained in the distilling 2

GENERAL CHEMISTRY 201 LABORATORY FORMAL REPORT flask. The boilung temperature versus the volume of the distillate was graphed and the percentage of the low and high boiling component was calculated. RESULTS AND DISCUSSION An amount of 25mL of the unknown binary mixture was used in the experiment. The same sample was used for both simple and fractional distillation. Volume (mL) Temperature (C) 1st drop 65 C 3 mL 81 C 6 mL 84 C 9 mL 89 C 12 mL 92 C 15 mL 98 C 18 mL 98.5 C 21 mL 116 C 24 mL 130 C Table 1.1. The data obtained from simple distillation. Table 1.1 shows us the relationship of the volume and the temperature of the unknown binary mixture that used the simple distillation. The given data shows that the volume is directly related to the temperature because as the volume increases the temperature also increases. Temperature (C) 57 C 67 C 68 C 61 C 130 C 134 C 132 C 98 C Soln was already 24 mL 1mL in the distilling flask Table 1.2. The data obtained from fractional distillation. Volume (mL) 1st drop 3 mL 6 mL 9 mL 12 mL 15 mL 18 mL 20 mL

GENERAL CHEMISTRY 201 LABORATORY FORMAL REPORT Table 1.2 shows us that there is no definite relationship between the volume and the temperature of the unknown binary mixture that used the fractional distillation set-up. There is a possibility that the data obtained contains errors since the heating of the set-up was disrupted due to instrument malfunction. Figure 2.1. A graphical representation of the data for both simple and fractional distillation.

Figure 2.1 . shows the plotted data of both the simple and fractional distillation. It is a volume versus temperature graph which shows the similarities and differences on the data acquired of both simple and fractional distillation. This shows that the movement of the simple distillation is different from the movement of the fractional distillation. The % low boiling component was computed to be 12% while the % high boiling component was computed to be 20%. The boiling point of a liquid is the temperature at which its vapor pressure equals the external pressure. The boiling point is directly related to the vapor pressure of a liquid. It is also the difference in boiling points where the basis of distillation lies. The most volatile liquid or the one with the lower boiling point is the one that would separate first in the distillation mixture. The

GENERAL CHEMISTRY 201 LABORATORY FORMAL REPORT water inlet is put at the lower portion so that vapors of higher temperature get relatively hot water for cooling and colder vapors get colder water for cooling. Since hot vapor is less dense than cold vapor, it tends to go up of the condenser. By the time the water reaches the upper portion, it has already been warmed by the temperature of the vapors. The contents of the distilling flask must not be heated all the way to dryness because the distillation process would be useless. The liquids will still be with each other because the less volatile liquid is also evaporated and condensed back into the other flask. The boiling chips provide nucleation sites so the liquid boils easily without becoming superheated. Adding the boiling chips once the distillation has started might cause immediate boiling over the solution. The solution must be cooled again before adding boiling chips to avoid any product loss. The fractionating column is used for the separation of liquids into its component parts, or fractions, based on the differences in their volatilities. Packing materials can be used to improve separation in distillation columns. It offers the advantage of a lower pressure drop across the column. CONCLUSION Not all of the objectives were met during this experiment. There were many errors made during the experiment which made the data inaccurate. Still, most of the objectives were met. The separation of the mixture was done during the experiment but it might not be that accurate. The determination of the components of the mixture was not made since the separation was not a complete success. The distillation curve was constructed and the percentage of the low and high boiling capacity was computed. The efficiency of the fractional and simple distillation was not that emphasized since the data contained many errors. The factors that affected the data obtained were the lack of instruments, time pressure and human error. The experiment could still be accepted but there are inaccuracies included in the data. 5

GENERAL CHEMISTRY 201 LABORATORY FORMAL REPORT

REFERENCES 1. H.E. LeMay Jr., H. Beall, K.M. Robblee, D.C. Brower. Chemistry Connections to Our Changing World. 1st Edition. Prentice Hall Upper Saddle River, N.J. (1996) 78. 2. A. Sherman, S. Sherman, L. Russikoff. Basic concepts of chemistry. 4th Edition. Houghton Mifflin Boston (1988) 313-315. 3. J.W. Lehman. Multiscale Operational Organic Chemistry: A Problem Solving Approach to the Laboratory. 1st Edition. Prentice Hall Upper Saddle River, N.J (2002) 679-711. 4. K.W. Whitten, R.E. Davis, M.L. Peck. General Chemistry with Qualitative Analysis. 5th Edition. Saunders College Publishing USA (1996) 452-454.