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Write up for Aspirin lab for chem 112
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Titration is one of the techniques used in performing chemical analysis. The apparatus used for titration is called, a buret. The buret is a long tube marked for volumes, usually in increments of 0.10 mL. At the end of the tube there is a valve called a stopcock. The amount and rate of addition of the solution, titrant, is controlled by manipulating the stopcock. In a typical titration a solution containing an unknown amount of the substance to be analyzed is placed in a receiving flask. The next step is to add precisely measured volumes of a solution of known concentration, a standard solution, from the buret. The standard solution is added until the end of the reaction is reached. Since I can't see when the end of the reaction is reached I have to use a special dye called an indicator or an instrument called a pH meter to tell me when this point is reached. Once the end of the reaction is reached, the known amount of reactant added using the buret is used to stoichiometrically calculate the amount in the initial solution. Indicators An acid-base indicator is one color in acidic solution and another in basic solution. Phenolphthlein is an example of an indicator; it is colorless in acid and pink in base. The indicator changes color when the reaction has reached completion, for example the acid has been neutralized by the base. At this moment the titration is stopped. The equivalence point in the titration occurs when all the moles of acid present in the original solution have been reacted with an equivalent amount of base, moles acid = moles base. The end point of the titration occurs when a tiny excess of base, one drop past the equivalence point, is added. This last drop causes the solution which was neutral at the equivalence point to now be basic which causes the change in color of the indicator dye. In calculations we assume that this tiny excess of base is insignificant. Therefore the amount of base required to reach the equivalence point is essentially the same as the amount required to reach the end point. Phenolphthalein in acid solution Phenolphthalein in basic solution pH meters The instrument that can be used to measure pH is called a pH meter. This is the most accurate and precise method, with pH being determined to within +/- 0.01 pH units. Another advantage of a pH meter is that it can be used to follow the change in the pH during the entire titration. Unlike indicators which only tell you when a transition has taken place in the solution, the pH meter can give you the pH continuously. The ability to follow the pH of the solution continuously allows the equivalence point of the titration to be determined rather than just the end point.
Titration can be used to determine concentration for strong acids and bases as well as for weak acids and bases. We classify acids as strong or weak depending upon the extent to which they dissociate in water. When dissolved in water, strong acids completely dissociate releasing a hydrogen ion, H+, to a water molecule producing a hydronium ion, H 3 O+. HCl(aq) + H 2 O(l) H 3 O+(aq) + Cl-(aq) When weak acids are dissolved in water they do not completely dissociate. A large percentage of the acid remains together. For this reason, we write the arrow in one direction only when we give the equation for the dissociation of a strong acid and use equilibrium arrows when we write the equation for the dissociation of a weak acid. HA(aq) + H 2 O(aq) H 3 O
(aq) +^ A
- (aq) With an equilibrium expression for the dissociation: Ka =
] [A
- ] [HA] Example: We have 0.050L of an HCl of unknown concentration, we titrate this solution to the end point with 0.252 L of 0.125M NaOH. What is the molarity of the HCl solution? HCl(aq) + NaOH(aq) NaCl(aq) + H 2 O(l) Molarity = moles Liters 0.125 M = moles 0.252 L moles NaOH = (0.125M)(0.252L) = 0. based on the balanced equation one-to-one ratio we can determine the moles of HCl 0.0315 moles NaOH 1 moles HCl 1 moles NaOH = 0.0315 moles HCl to determine moles of NaOH required to neutralize the HCl to determine the Molarity of the unknown HCl Molarity = 0.0315 moles 0.050 L = 0.630 M This type of calculation can also be used if one of the reactants is a solid and not a solution.
Example for a strong acid and a strong base: HCl(aq) + NaOH(aq) NaCl(aq) + H 2 O(l) We can locate the equivalence point of the titration by drawing a vertical line through the midpoint of the steep portion of the curve. The x and y coordinates for this point give us the volume of the titrant added and the pH respectively. For the titration curve shown in Figure 1 for a strong acid and a strong base the pH at the equivalence point is 7 and the volume of titrant used is 20 mL. From this information the moles of base and thus the moles of acid can be calculated. Titration of a weak acid with a strong base is done in the same manner as the titration of a strong acid with a strong base. However, they're a few differences between the two. A typical titration curve for the titration of a weak acid with a strong base appears in Figure 1.
Consequently, at the equivalence point we have water and the conjugate base of the weak acid, which produces OH -^ ion in water. HA(aq) + OH
(aq) With an equilibrium expression for the dissociation of: Ka =
] Therefore the pH of the solution at the equivalence point is basic, higher then 7. Example for a weak acid and a strong base is: CH 3 COOH(aq) + OH
(aq) Once again we can locate the equivalence point of the titration by drawing a vertical line through the midpoint of the steep portion of the curve. The x and y coordinates for this point give us the volume of the titrant added and the pH respectively. For the titration curve shown in Figure 1 the pH at the equivalence point is 9 and the volume of titrant used is 20 mL. From this information the moles of base and thus the moles of acid can be calculated. Standardization of the Sodium Hydroxide You will prepare the sodium hydroxide solution, a strong base, by weighing out the NaOH pellets and dissolving the pellets in water. Normally you calculate the concentration of the base using the amount weighed on the balance, the molar mass of the base, and the final volume of the solution. Unfortunately, sodium hydroxide in the solid form readily absorbs moisture from the air. Hence, the mass of the pellets on the balance is the mass of the sodium hydroxide plus the mass of the absorbed water. For the precise work required, the absorbed water will create too large an error in the calculated concentration. Consequently, the best we can do at this point is to calculate an approximate concentration of the base. To get an exact concentration, we need to first analyze the prepared solution against an acid that is extremely stable, one that can be accurately weighed on the balance. The acid we will use is potassium hydrogen phthalate. The formula for potassium hydrogen phthalate is KHC 8 H 4 O 4 but, for simplicity, we abbreviate it as KHP.
There are a number of different pH meters in the laboratory. Obtain the instructions for the meter that you are using from your instructor. Glass electrodes are fragile and expensive. Do not bump the glass membrane against anything. F. Analysis of the Aspirin Tablet You will now use titration to analyze the actual aspiring, acetyl salicylic acid, content of your aspirin tablet. The reaction of the aspirin with the NaOH titrant is: C 9 H 8 O4(aq) + NaOH(aq) H 2 O(l) + Na+(aq) + C 9 H 7 O 4 - (aq)
Avg. Concentration of NaOH (M) Calculation: Titration of aspirin with standardized NaOH solution Trial 1 Initial buret reading 0.00mL pH [H 3 O+] Sample calculation: Buret reading (mL) Volume NaOH added (mL) Sample calculation: 2.25 0.0056 0.00 0 2.45 0.0035 2.00 2 2.50 0.0032 4.00 4 2.60 0.0025 6.00 6 2.80 0.0016 8.00 8 2.90 0.0013 9.00 9 3.05 8.9 x 10^-4 10.00 10 3.25 5.6 x 10^-4 11.00 11 3.56 2.8 x 10^-4 12.00 12 4.18 6.6 x 10^-5 13.00 13 5.09 8.1 x 10^-6 14.00 14 10.80 1.6 x 10^-11 15.00 15 11.43 3.7 x 10^-12 16.00 16 11.73 1.9 x 10^-12 17.00 17 12.00 1 x 10^-12 18.00 18 12.34 4.6 x 10^-13 20.00 20 12.71 1.9 x 10^-13 22.00 22 12.73 1.9 x 10^-13 24.00 24 12.75 1.8 x 10^-13 26.00 26
Initial buret reading 0.00mL pH [H 3 O+] Buret reading (mL) Volume NaOH
Percentage of claimed value Sample calculation: Average percentage Calculation:
molecules for alcohol is similar to the affinity of alcohol molecules for each other. Whereas the affinity of water for aspirin is not as great as the affinity of water for itself. Thus, aspirin is more soluble in alcohol.