Lab 7 Parts A & B Using Acid/Base Titrations to Measure Vinegar Concentration and the Molar Mass of an Unknown Carboxylic Acid

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1 Lab 7 Parts A & B Using Acid/Base Titrations to Measure Vinegar oncentration and the Molar Mass of an Unknown arboxylic Acid hemistry B1A / by Daniel / Summer 2015 Purpose This is a 2 day lab. The first day you will use volumetric analysis to standardize a Na solution, and use that solution to measure the molarity and mass percent of acetic acid in vinegar. The second lab period you will use that standardized Na to titrate and calculate the molar mass of an unknown acid. aution A 1 M sodium hydroxide solution (which is ~5 times more concentrated that what we are using) has NPFA ratings of 3 (out of 4) for health, 0 for fire, and 1 for reactivity. The Kp has a 1 for health, 1 for fire, and 0 for reactivity. The vinegar has 1 for health, 0 fire, and 0 for reactivity. The Na solution is corrosive to skin and can cause serious eye damage. ne of the simplest, weak organic acids is acetic acid. Bacteria can oxidize carbohydrates such as starch and sugars into ethyl alcohol, and different bacteria can further oxidize the alcohol into acetic acid. This is one way wine goes bad, when the alcohol in wine turns into vinegar. Vinegar is mostly acetic acid dissolved in water, and it has many uses such as a food and as a food preservative. An example of using vinegar as a preservative is instead of letting your cucumbers spoil, you can protect them by placing them in vinegar, where little can grow, and you get a sour pickle. In today s lab we will use a titration to measure the concentration of acetic acid in vinegar. This will be done by titrating the weak acetic acid with sodium hydroxide, Na, a strong base. A titration is a procedure where a unknown concentration is determined by measuring an unknown solution s volume, and measuring the volume of a standard (known concentration) solution that quickly reacts with the unknown. In this experiment, we will use a (soon to be) known concentration of base to react with, or neutralize, the acetic acid. In a neutralization reaction, an acid and base combine to produce a salt and water. 1) Na (aq) Na (aq) + 2 (L) sodium hydroxide + acetic acid sodium acetate (a salt) + water When we add just enough moles of base to neutralize the moles of acid, we have reached the equivalence point. At this equivalence point, there is a large change in the concentration of acid ( +, or more accurately, 3 +, hydronium) and base ( - hydroxide) ions in water. ne measure of the concentration of acid ions in water is p. An indicator is a substance added to a solution, to help us see this large change in acid and base concentrations at the equivalence point, giving us an end point we can see. The indicator is chosen so the color change at the end point is near the equivalence point. ur indicator, phenolphthalein, goes from colorless in an acidic solution to pink in a basic solution. At this point, the moles of base equal the moles of acetic acid. By measuring the volume of base, and knowing it s concentration, you could calculate the moles of acetic acid present. Lab_7_Parts_A&B_Vinegar_Titration_MolarMass Page 1

2 2) V (ml) M mol Na ml Na x 1 mol Acetic Acid 1 mol Na = moles acid Since equation 1 has one mole of sodium hydroxide base reacting with one mole of acetic acid, volume of base multiplied by the Na molar concentration is equal to the moles of acetic acid. By knowing the volume of acetic acid (in liters), you could calculate the molarity of the acetic acid. moles Acetic Acid 3) M (acetic acid) = L To experimentally perform reaction 1 you need a standard sodium hydroxide solution. You could weight out pure Na and dissolve in water and calculate the molarity, if you had pure Na. The problem with Na, is it is hard to make it pure and keep it pure. It reacts with 2 in the air to make sodium carbonate, and it absorbs water from the air. Since the stockroom does not have pure Na, you need to standardize, or measure the concentration of the Na solution. You will titrate a weighed amount of a very pure acid salt called potassium hydrogen phthalate or KP ( g/mol), and measure the volume of Na needed to neutralize this acid. KP is called a primary standard because it is easily made pure and it does not react with or absorb substances from the air. Note the P in KP is an abbreviation for phthalate and not phosphorus. 4) Na (aq) + K (aq) Na K (aq) + 2 (L) Sodium hydroxide + KP Potassium Sodium phthalate + water Phthalic acid is a diprotic acid with the formula, , and the structure 3 Phthalic Acid Acetic Acid The structure is characteristic of organic acids, and it is also found in acetic acid. In KP one acidic hydrogen cation, (one of the s attached to the atom) is replaced by a potassium cation. Using the mass and molar mass of KP, you can calculate the moles of Kp, which is equal to moles of Na titrated, and you can calculate the molar concentration of Na by dividing the moles of Na by the volume in liters. In addition to measuring the concentrations of Na, and vinegar, you will also measure the p of some solutions using a wide range p paper. p is a measure of how acidic or basic a solution is. Lab_7_Parts_A&B_Vinegar_Titration_MolarMass Page 2

3 In pure water at 25 water undergoes a small amount of autoionization. 4) 2 2 (L) 3 + (aq) + - (aq) At this temperature the hydrogen ion concentration is equal to the hydroxide concentration which is equal to 10-7 M. There is a balance between the concentrations of these two ions. 5) [ 3 + ] [ - ] = K w = 1.0 X The square brackets represents molarity, so K w should have units of M 2, however it is usually written without the units. This equation shows that as the concentration of the hydrogen ion, [ 3 + ] increases, the concentration of hydroxide decreases, and vice versa. Solutions where the hydrogen ion concentration is greater than the hydroxide concentration are said to be acidic, and where the hydroxide ion concentration are greater than the hydrogen ion concentration are said to be basic. In many aqueous solutions, the molar concentrations of 3 + and - are very small. Writing and comparing exponential values can be confusing. ne approach to comparing solutions is p, which is defined as; 6) p = - Log [ 3 + ] This is mathematically equivalent to saying; 7) [ 3 + ] = 10 -p So water at 25, has a [ 3 + ] = 10-7 M, and a p = 7. A 0.1 M (10-1 M) hydrochloric acid solution would be a p of 1, and it is one million (10 6 ) time more concentrated in 3 + than pure water. The following table shows how the two different ions concentrations change and how the p changes for different solutions. While performing the experiment below, you will be told to measure the p of several solutions. p Solution Acidic Acidic Neutral basic Basic [ 3 + ] = 10-1 M 10-4 M 10-7 M M M [ - ]= M M 10-7 M 10-4 M 10-1 M [ 3 + ] [ - ] Lab_7_Parts_A&B_Vinegar_Titration_MolarMass Page 3

4 Procedure Na is very hazardous to your skin and eyes, so avoid contact, and quickly wash off with water any that gets on you. 1. btain a 25 ml buret. btain about 100 ml of 0.2 M Na. Use about 3 ml of this dilute Na to rinse the buret as described by your instructor. Run this Na into the sink followed by water. Repeat. Fill the buret with your Na solution, and remove any air bubbles in the bottom tip by running the liquid out the tip. You will not use all of the Na in the first lab period, so you will need to save the excess sodium hydroxide and seal the flask between periods. 2. Na Standardization - Accurately weigh g of KP in a dry flask, and add about 25 ml of distilled water and 2-3 drops of phenolphthalein indicator. Measure the p of this Kp solution using p paper. Measure the initial volume of Na, estimating between the marks to the 0.01 ml. Slowly add Na to the KP solution with stirring. Addition of Na should produce a pink color that quickly disappears as you stir the KP solution. When you have added just enough Na to neutralize the acetic acid, you will get a faint pink color that last for more than 30 seconds. Measure the final volume of Na (to 0.01 ml). When you finish the titration, measure the p of the neutralized solution. Dispose of the neutralized solution and repeat this titration. You will need two clean and dry Erlenmeyer flask for the vinegar titrations, so rinse your Erlenmeyer with distilled water and put in oven. Save your Na for the next experiment. 3. Vinegar Titration - Weigh a dry Erlenmeyer flask, and add 3 ml of vinegar using the dispenser. Reweigh the flask with the vinegar. Measure the p of the vinegar using p paper. The volume of vinegar to 3 significant figures will be calculated later using density and mass. Add ~ 25 ml of water and 2-3 drops of phenolphthalein indicator. Measure the initial volume of Na (to 0.01 ml), and then slowly add the Na to the vinegar solution with stirring. As you add the Na a pink color is produced until it is mixed and reacted with the acetic acid. When you have added just enough Na to neutralize the acetic acid, you will get a faint pink color that last for more than 30 seconds. Record the final volume of Na to the nearest 0.01 ml, and measure the p of this neutralized solution. The final volume minus the initial volume will equal the volume of Na used. The neutralized solution can be disposed of in the sink. Rinse the flask with distilled water and set aside. Repeat the titration a second time again using a dry flask. 4. From the first set of titrations (in #2), you can calculate the moles of KP (equation 5), 5) g KP x mol KP g KP x mol Na mol KP = mol Na reacted with by KP 6) M (Na) = mol Na / V (L) used to neutralize KP which equal the moles of Na. Moles of Na divided by the titration volume of Na in liters (equation 6) will give you the molarity of Na. This should be approximately 0.2 M. In step 3 the volume of Na needed to titrate the vinegar and the molarity of Na multiplied together gives the moles of Na Lab_7_Parts_A&B_Vinegar_Titration_MolarMass Page 4

5 7) V (ml) Na x M mol Na 1000 ml Na x 1 mol Acetic Acid 1 mol Na = mol Acetic Acid in Vinegar used, which is equal to moles of acetic acid in the vinegar sample. The density of vinegar is 1.05 g/ml. Use the density and mass of the vinegar solution, to calculate the volume of vinegar. Moles of acetic acid divided by the volume in liters will give you the molarity of acetic acid. It should be less than 1 M. The moles of acetic acid and it s molar mass can be used to calculate the mass of acetic acid. 6) 8) Moles X molar mass g mol acetic acid The mass percent of acetic acid will be; mass acetic acid 9) Mass % = X 100% mass vinegar Typically distilled vinegar is ~ 5 % acetic acid. = Mass of acetic acid Report - Part A - Please complete the p table and the Na standardization table. Your report will have a typed cover sheet including the lab title, your name and partner s full name, lab section and due date. Type a vinegar titration table including average Na molarity (from table 2), initial, final, and total volume of Na used, moles of Na used (which equals moles of acetic acid titrated), mass of vinegar, calculated volume of vinegar, moles of acetic acid, molarity of acetic acid, mass percent of acetic acid, and per cent error compared to 4% by mass. Type or neatly write your calculations below your tables. Answer the problem on page 7 and attach to your report following the above. (As usual, this data should be recorded in your lab notebook.) Lab_7_Parts_A&B_Vinegar_Titration_MolarMass Page 5

6 Table 1 -p of different solutions Distilled Water, Diluted Na Solution, Kp Solution, Vinegar, and the other provided solutions. Solution p ~ [ 3 + ] / M ~[ - ] / M Acidic or Basic / A or B? Distilled Water ~0.2 M Na Kp Vinegar Soda Milk Fruit or Fruit Juice Milk of Magnesia ven leaner Na 3 P 4 Na 2 3 This is a model data table for your lab notebook and report. Vinegar ID Density of Vinegar Table 2 Na Standardization 1. Mass of Kp / g Final Volume Na / ml Initial volume Na / ml 2. Volume Na Used / ml 3. Moles KP = Moles Na 4. Molarity Na = Moles Na/Volume L Na 5. Average 6. Average Deviation Titration 1 Titration 2 Lab_7_Parts_A&B_Vinegar_Titration_MolarMass Page 6

7 Lab 7 Part A Problem - The typical error in this experiment is overshooting the endpoint by adding too much Na. Assume you added two drops of Na too many to your first vinegar titration. Use the approximation of 25 drops / ml, convert 2 drops into ml, and subtract this volume from the Na volume used in the second titration on the previous page. Use this estimated error correction, to calculate a mass percent of acetic acid and compare it to what you calculated earlier. alculate what percent error these two drops introduce. Show your calculations and results below: Lab_7_Parts_A&B_Vinegar_Titration_MolarMass Page 7

8 Lab 7 B Using Molar Mass to determine an Acid s Identity We have used titrations to standardize sodium hydroxide and to measure the concentration of acetic acid in a commercial vinegar solution. In this lab you will use a titration to identify an organic acid by determining its molar mass. The titration will measure the volume of a known Na concentration needed to neutralize an unknown acid, calculate the number of moles of acid neutralized, and from this and the mass of acid you can determine the molar mass of the acid, which will help identify the unknown acid. I hope you remember that a neutralization reaction is a double replacement reaction where the products are water and a salt. A (aq) + Na (aq) NaA (aq) + 2 (L) A is a symbol for any monoprotic acid. Most of the acids used today are diprotic acids where two hydrogen cations can react. You will need to use this 2:1 ratio in your calculations. 2 A (aq) + 2 Na (aq) Na 2 A (L) Materials: Your standardized Na An Indicator An unknown acid from the following, (all are diprotic unless noted) Lab_7_Parts_A&B_Vinegar_Titration_MolarMass Page 8

9 Tartaric Acid NFPA-2 ealth, 1 Fire, 0 Reactivity g/mol 2 () 2 2 Malonic Acid NFPA-2 ealth, 1 Fire, 0 Reactivity Succinic Acid NFPA-2 ealth, 0 Fire, 0 Reactivity xalic Acid dehydrate NFPA-2 ealth, 0 Fire, 0 Reactivity Benzoic Acid (Monoprotic) NFPA-2 ealth, 1 Fire, 0 Reactivity ( 2 ) To have 3 significant figures from the solid, unknown acid, you need a mass of g or more. The diprotic acid that would need the largest volume of base would be the malonic acid. (ould you explain in an essay why?) Since our burettes only hold 25 ml of a liquid, calculate the mass of malonic acid that 20 ml of your base will react with. This gives you an upper limit on the mass of acid to use, since you do not want to need more than 25 ml of base, (calculating using 20 ml gives a safety margin). Show your instructor this calculation before weighting out your unknown. Do as many titrations as you think are adequate. Because the acids may not be very soluble in water, you may need to go slow to give the solid acid time to dissolve in water as the titration proceeds. We may need to repeat the titration of KP with Na to determine if the Na concentration changed since you measured it. Report Part B - Your report will be a typed data table with your unknown identifier, mass of unknown, initial, final, and total volume of Na, moles of Na, moles of diprotic acid and Lab_7_Parts_A&B_Vinegar_Titration_MolarMass Page 9

10 monoprotic acid, molar mass if unknown is diprotic and molar mass if unknown is monoprotic, identification of unknown, and percent error based on identification. Lab_7_Parts_A&B_Vinegar_Titration_MolarMass Page 10

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