Aspirin Lab Write Up, Cheat Sheet of Chemistry

Write up for Aspirin lab for chem 112

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2020/2021

Uploaded on 10/11/2021

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Monitoring Acid-Base Titrations with a pH Meter
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.
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Monitoring Acid-Base Titrations with a pH Meter

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 =

[H 3 O

] [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.

  1. The initial pH of the solution for a weak acid is higher than that of a strong acid. For example, the pH of a 0.10 M HCI solution is 1.00, while the pH of a 0.10 M acetic acid solution is 2.87. This is due to the small amount of dissociation you have with a weak acid. Because the weak acid dissociates only slightly, less H 3 O+^ is present than with a strong acid that completely dissociates.
  2. The pH at the equivalence point is different. For a strong acid titration, the pH is neutral as discussed earlier. When you add base to a weak acid, you are converting the weak acid to its conjugate base: HA(aq) + OH - (aq) H^2 O(l)^ +^ A^ - (aq)

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

H 2 O(l) + A (^) (aq)

(aq) With an equilibrium expression for the dissociation of: Ka =

[OH

  • ] [HA] [A

] 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) H 2 O(l) +^ CH 3 COO^

(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.

  1. Rinse two more times with distilled water. C. Standardization of the Sodium Hydroxide Solution
  2. Set up your titration apparatus by obtaining a buret and using a clamp to attach it to a ring stand.
  3. Using a funnel, fill the buret to near the top with your sodium hydroxide solution.
  4. Open your stopcock and drain a little of the NaOH out of your buret into a waste beaker. This should remove any air bubbles from the tip of your buret that would introduce an error into your volume reading. You do not need to fill the buret to exactly 0.00 mL, somewhere between 0.00 and 2.00 is sufficient. The important thing you need to know is where you filled it to, record this initial volume on your data sheet.
  5. Weigh out about 0.500 grams of KHP into a 250 mL Erlenmeyer flask. Record the mass on your data sheet.
  6. Add 100 mL of water and two drops of phenolphthalein to your KHP. Swirl until all of the KHP dissolves.
  1. Record the initial volume in the buret on your data sheet. You need to read the buret to two decimal places.
  2. Titrate the solution by adding the sodium hydroxide from the filled buret. The endpoint occurs at the first permanent color change of the indicator from colorless to pink, The lighter the pink, the better the end point. To better visualize the change in color from clear to pink, place a piece of white paper under the erlenmeyer flask. As you closer to the end point, the pink color will take longer to disappear. When the end point is imminent, add sodium hydroxide one drop at a time or even a partial drop at a time. The color change is permanent when it stays despite swirling the sample.
  3. Once you have reached the end point, record the final volume in the buret, again to two decimal places.
  4. Refill the buret to between 0 - 2 mL as before.
  5. Repeat steps 2 through 8 using two additional samples of KHP. D. Preparation of the 5 grain (325 mg) Aspirin Tablet
  6. Take a commercial aspirin tablet. In a mortar and pestle, grind the tablet into a powder.
  7. Measure about 3 mL of methyl alcohol in a graduated cylinder. Add it to the mortar and pestle to dissolve the aspirin.
  8. Using your wash bottle, rinse the aspirin/methyl alcohol mixture from the mortar and pestle into a 100 mL graduated cylinder. Be sure to fully rinse both the mortar and pestle to get all the aspirin into the graduated cylinder.
  9. Fill the graduated cylinder up to the 100 mL mark using distilled water.
  10. Set up the suction filter apparatus as shown. Be sure to clamp the flask to your ring stand. Mortar and

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)

  1. If the buret hasn't been refilled to near the top with your sodium hydroxide solution, do so now.
  2. Record the initial buret reading to two decimal places, on your data sheet.
  3. Position the beaker containing the aspirin solution so that the glass membrane of the electrode is immersed in the solution. Position the buret containing the NaOH solution just inside the beaker, with the tip below the rim but above the solution surface, as shown below. Ask your instructor to check your equipment set-up.
  1. Adjust the function knob of your pH meter from standby to read.
  2. While swirling the aspiring solution continuously, begin slowly adding 1mL portions of NaOH solution. When the pH begins to climb more rapidly you will want to add smaller portions or the NaOH.
  3. After each addition, record the pH and the corresponding buret reading on your data sheet.
  4. Stop adding NaOH solution when the pH reaches 11.5.
  5. Return the pH meter to standby.
  6. Remove the electrode from the aspirin solution.
  7. Rinse and dry the electrode. 11. Repeat the analysis using a second aspiring tablet.
  8. Recap the electrode with water in the cap.
  9. Turn off the pH meter.
  10. Place all of your waste in the class waste beaker.

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

Prepare a titration curve for this titration (Trial 1). Identify the equivalence point on your graph.

Initial buret reading 0.00mL pH [H 3 O+] Buret reading (mL) Volume NaOH

  • 12.75 1.8 x 10^-13 28.00
  • 12.77 1.7 x 10^-13 30.00
  • pH at equivalence point 8. - Trial Volume of titrant required to reach the equivalence point of the titration. 14.7mL
    • 3.00 0.001 0.00 added (mL)
    • 3.12 7.6 x 10^-4 2.00
    • 3.17 6.8 x 10^-4 4.00
    • 3.23 6.3 x 10^-4 6.00
    • 3.25 5.6 x 10^-4 8.00
    • 3.41 3.9 x 10^-4 9.00
    • 3.50 3.2 x 10^-4 10.00
    • 3.55 2.8 x 10^-4 11.00
    • 3.79 1.6 x 10^-4 12.00
    • 4.01 9.8 x 10^-5 13.00
    • 4.32 4.8 x 10^-5 14.00
    • 4.73 1.9 x 10^-5 15.00
    • 11.50 3.2 x 10^-12 16.00
    • 12.03 9.3 x 10^-13 17.00
    • 12.35 4.5 x 10^-13 18.00
    • 12.56 2.8 x 10^-13 20.00
    • 12.74 1.8 x 10^-13 22.00
    • 12.77 1.7 x 10^-13 24.00
    • 13.00 1 x 10^-13 26.00
    • 13.01 9.8 x 10^-14 28.00
    • 13.01 9.8 x 10^-14 30.00
  • pH at equivalence point 8. Prepare a titration curve for this titration (Trial 2). Identify the equivalence point on your graph.

Percentage of claimed value Sample calculation: Average percentage Calculation:


POST-LABORATORY QUESTIONS

  1. Suppose you dissolved 2.4 g of solid NaOH instead of 2.0 g into the 500 mL bottle. Would the calculated percent aspirin be high, low, or unaffected? Explain your reasoning. The calculated percent aspirin would be lower than the actual percent aspirin. This is because you use a more concentrated solution of NaOH. As the concentration of NaOH increases, the volume of NaOH decreases. Using the equation below, V1 will thus decrease meaning the calculated M value will also decrease. M 1 V 1 (NaOH) = M 2 V 2 (Aspirin) M 2 = M 1 V 1 / V 2. Calculated V 1 value will be less so the M 2 value will be less
  2. The laboratory group next to you standardized the sodium the hydroxide to a very dark pink end point each time they performed the standardization. They did, however, titrate the aspirin to a very light end point. Would the calculated percent aspirin be high, low, or unaffected? Explain your reasoning. In this situation, the calculated NaOH volume will be higher than its actual value. This will affect the concentration calculations of NaOH. A higher volume will lead to a lower concentration value for NaOH. This is because we calculate concentration by dividing moles by volume. A lower calculated NaOH concentration value will this lead to a lower calculated percent aspirin value. This is shown by the equation below. M 1 V 1 (NaOH) = M 2 V 2 (Aspirin) M 2 = M 1 V 1 / V 2. Calculated M 1 value will be less so the M 2 value will be less
  3. The lab group behind you forgot to standardize the sodium hydroxide solution. Instead they used the mass of their NaOH to calculate the Molarity of the sodium hydroxide solution. Would their calculated percent aspirin be high, low, or unaffected? Explain your reasoning. In this situation, the students simply used the molar mass of NaOH to calculate the concentration of NaOH. When you simply divide the molar mass by the volume you get a much higher calculated concentration value than when dividing the moles by the volume. A higher calculated concentration value will lead to a higher percent aspirin value. As shown by the equation below. M 1 V 1 (NaOH) = M 2 V 2 (Aspirin) M 2 = M 1 V 1 / V 2. Calculated M 1 value will be higher so the M 2 value will be higher.
  4. Why might the solution turn pink initially but then clear up as it is swirled? Phenolphthalein is pink in a base and colorless in an acid. Thus, in this situation, the phenolphthalein first indicated a base and then an acid. As you titrate and add NaOH to the solution, there will be a pink color where the base is added, before the solution is swirled. In that small area that becomes pink, the base concentration is higher than the acid concentration, thus the

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.

  1. Read about how pH meters work and briefly describe. A pH meter works similarly to a voltmeter. It measures the voltage produced by a solution whose acidity we are interested in and compares it with the voltage of a known solution. The meter then uses the difference in voltage between them to find the difference in pH.