Composition Measurement CHEG 2810 Data Acquisition 11/17/09 Ken McFarland & Pacscal M Abstract: In this lab we experimented with quantitative analysis of a mixture of antifreeze and water, starting with pure antifreeze, and washing it out of a four liter container with DI water. In order to find the mass composition of the mixture we used a refractometer. This required creating a calibration curve, plotting the degrees Brix of many mixtures of water and antifreeze against their known mass composition. The theoretical mass fraction of antifreeze in the tank was calculated at each of the times that we took samples, using the flow rate through the tank, and the equation provided in the lab manual. We plotted this theoretical data alongside the experimental values that we calculated using the refractometer and its mass fraction calibration curve. In this graph we found that the overall shape of our data curve matched that of the theoretical data, although our values for the mass fraction of antifreeze were consistently slightly higher from about the halfway point on. Introduction: Knowing the chemical composition of a compound to be used is one of the most fundamental requirements of any chemical process that involves that compound. It can tell you the concentration of any useful components of the composition, their purity, the identity of the impurities, if any, and many other useful pieces of information. Finding the exact chemical composition of a given compound is frequently an expensive, time consuming process. For this reason, shortcuts are often used when they are available. In this lab, we used a refractometer to find the degrees Brix of a solution of antifreeze and water. Degrees Brix is a measurement of grams of sucrose sugar dissolved per 100 grams of solution. A solution of 25 degrees Brix has 25 grams of sugar per 100 grams of solution, or in other words, a 100 gram sample of the solution contains 25 grams of sugar and 75 grams of water. The degrees Brix of a solution is found by a refractometer using the principal of refraction of light. When light passes through two substances with different densities the light bends. If the density of one of two materials is known, and the angle that the light bends, or angle or refraction, is measured then the unknown density of the second material can be found. The handheld refractometer that was used in this lab was calibrated to compare the density of the unknown material, our solution, to that of pure water to find the degrees Brix of the unknown solution. Results and Discussion: The mass fraction of antifreeze and the degrees Brix for the solutions we created with known mass fractions of antifreeze are attached in the appendix in Table 1. These data were used to create the calibration curve for the refractometer that we used to convert from degrees Brix to mass fraction antifreeze. The calibration curve is attached in the appendix as Figure 1. The table of data that we collected from the washout experiment is also attached as Table 2. This contains the degrees Brix for each of our samples, and the time that the sample was taken at. These data were converted from degrees Brix to mass fraction antifreeze, and the mass fraction water was plotted versus time in our graph for the washout portion, which is Figure 2 in the appendix. For the washout portion of the experiment the flow rate through the tank was kept at a steady 315mL/minute for the entire time that we were washing out the antifreeze. We used this figure along with the knowledge that we had 4 liters of antifreeze in our tank to begin with to calculate the theoretical mass fraction of antifreeze in our washout tank at each of the times that we took a sample from it, and also plotted those theoretical points on our graph in Figure 2, to give us some idea of how close to the theoretical correct answer we had gotten for each data point. While both our theoretical and experimental data sets both followed the same curve, the experimental data was over all slightly faster than that of our theoretical data curve, with a noticeable difference starting at about the 0.5 mass fraction point, and increasing as the mass fraction of antifreeze decreased, until the end of the experiment, where there is a difference between the two curves of three to four minutes. This is most likely due to the level of the fluid in the tank not remaining constant, with more water slowly adding to the tank than was being drained by the outflow valve, so that it was not immediately obvious that there was a change in volume, but one that ultimately had a measureable lowering effect of the concentration of antifreeze in our tank. Procedure: We created a calibration curve for the refractometer first, to allow us to convert from the degrees Brix that the refractometer gave us to the mass fraction of antifreeze in our solution. To do this, we found the degrees Brix of a number of samples of a known mass fraction of antifreeze, and plotted them against the degrees Brix of the sample that we got from the refractometer. This allowed us to find the unknown mass fractions of antifreeze in our samples for the washout section of the experiment. In the second part of the experiment, which was the main portion of the lab, we washed out a four liter container of antifreeze using distilled water according to the procedure in our lab manual. To wash out a solution is to add simultaneously add water and remove solution from a container, while holding the overall volume of solution in the container constant, slowly diluting the solution. To do this we had to insure that the inflow of water from the (adjustable) wall spigot was equal to the outflow from the (fixed) drain valve. To do this we first filled the tank with water and then adjusted the flow of the water into the tank until the level of water in the tank remained constant. Once we had equalized the flow rates, we measured the flow rate of solution though the tank, which is used to calculate the theoretical concentration of the solution at any time during the washout. We drained the tank of water, and filled it with four liters of antifreeze. We opened the drainage valve at the same time that we started to add water to the tank. For the first eight minutes we measured the degrees Brix of a sample of the solution draining from the tank every minute. After the first eight minutes, we measured the degrees Brix of the outflow stream every two minutes starting at ten minutes. This was done until a total of thirty minutes had passed, and the degrees Brix of the outflow stream was very close to that of pure water, or 0 degrees Brix. Finally, we converted the degrees Brix of each sample into mass fraction of antifreeze, and plotted the mass fraction versus time. Conclusions: Our graph of mass fraction versus time for the washout portion of the experiment (Figure 2) shows that the relationship between the two is not linear, rather it follows the exponential equation given in the lab manual. The theoretical values for the mass fraction that we should have gotten at each time can also be seen on the attached graph. These show that our data had the correct shape, and approximately the right curve, however at mass fractions of antifreeze less than approximately 0.50 there was a noticeable increase of about 0.05 mass fraction antifreeze at every point. Recommendations: We recommend that for best results the tank be left running with only water for a minimum of at least fifteen minutes without any change in the volume of water in the tank before the water is drained and replaced with antifreeze. Ideally, the pure water portion of the washout would be ran for significantly longer than the experiment is expected to take, however that would not be feasible with the time constraints of this lab. Therefore, we feel that fifteen minutes should be sufficient, as the washout portion of the experiment took only thirty minutes for us to complete, and if it is known that the volume of the tank will not change at all in the first fifteen minutes, is most likely will not change significantly in the second fifteen minutes. Appendix: Table 1: Refractometer calibration data Degrees Brix mass fraction antifreeze 17.4 1 14.4 0.832191781 12.2 0.6 10.6 0.530567686 9 0.472762646 8 0.421875 7 0.375579598 6.2 0.337969402 5.4 0.299261084 5 0.258510638 4.2 0.248466258 4 0.216964286 3.6 0.180803571 2.2 0.144470868 1.6 0.104876996 Table 2: Washout experiment data: Degrees Brix Time (Min) Mass fraction Antifreeze 17.4 0 1 15.4 1 0.85 14.8 2 0.82 13 3 0.72 12 4 0.66 10.6 5 0.58 10 6 0.55 9.2 7 0.5 8.6 8 0.47 7 10 0.38 5.4 12 0.29 4.8 14 0.26 4 16 0.21 3 18 0.16 2.4 20 0.13 2 22 0.1 1.8 24 0.09 1.4 26 0.07 1 28 0.05 0.6 30 0.03 Figure 1: Refractometer calibration curve Figure 2: Washout mass fraction versus time