CHM 2045C Chapter 3 Limit/Excess Reagent Experiment

Plop, Plop, Fizz, Fizz: The Mass Percent of NaHCO₃

Introduction

As we continue through lab this semester we will continue to revisit the concepts of stoichiometry and mole-mass relationships. One of the relationships that strengthens our understanding of both math involved in and the relevance of stoichiometry is mass percent. The mass percent of a compound or element within a mixture or another compound is often vital to the viability of a reaction. In a hydrate, for example, the mass of the salt portion of the molecule is often a low percentage of the overall molecular mass. Magnesium chloride hexahydrate (MgCl_2•6H₂0) is such a compound. The overall molecular mass is 203.3 g/mol, but the salt is only _˜46% of that mass. If I were manufacturing this compound we would have to take that into account since a majority of the product mass would not contain the salt compound I need.

Another place where mass percent is important is in medications. Very often the active ingredient in a medication is a very small portion of the overall mass of the tablet of capsule. The rest of the tablet is generally binders, flavors, or other medications designed to counteract side effects. The Alka –Seltzer tablets that we will investigate in this lab contain not only sodium bicarbonate, the acid neutralizing ingredient, but also two other ingredients, aspirin and citric acid. Our purpose in this lab is to determine the mass percent of the sodium bicarbonate in an Alka-Seltzer tablet and compare our results to the published chemical content given by the manufacturer.

Because the sodium bicarbonate cannot be measured directly as it reacts with the other ingredients in the tablet form water and carbon dioxide, we will measure the production of carbon dioxide and use stoichiometry to determine the initial mass of the sodium bicarbonate. This will also give you the opportunity to strengthen your understanding of mass to mole relationships. Using a balanced chemical reaction, any chemist can tell you how much product can be made from a given amount of reaction or conversely, as in this case, how much reactant was used to produce a particular amount of product.

Background

An Old Alka-Seltzer® commercial starts with “Plop-plop, fizz-fizz, oh what a relief it is…” However, what you’ve most likely never thought about is the actual mechanism by which Alka-Seltzer® provides its relief. According to its packaging, an Alka-Seltzer® tablet contains 1916 mg of sodium bicarbonate (NaHCO₃), 325 mg of acetylsalicylic acid (HC₉H₇O), and 1000 mg of citric acid (H₃C₆H₅O₇). When the tablet is dissolved in water, the sodium bicarbonate reacts with the two acids according to the following chemical reaction:

2NaHCO₃(s) + HC₉H₇O₄(s) + H₃C₆H₅O₇(s)→ 2H₂CO₃(aq) + NaC₉H₇O₄(aq) +NaH₂C₆H₅O₇(aq)

Though the above chemical equation appears absolutely terrifying at first glance, it is rather simplistic once we look at what is actually reacting in greater detail. Each reactant in the equation above acts as a weak electrolyte. This means that when dissolved in water each species breaks down its corresponding ions. For example, the sodium bicarbonate (NaHCO₃) gets broken down to H⁺ and C₉H₇O₄^- and the citric acid decomposes to H+ and H₂C₆H₅O₇^-. The compound holding the key to the relief in an Alka-Seltzer® tablet is the sodium bicarbonate. When dissolved in water, the bicarbonate ion from the NaHCO₃ undergoes an acid-base reaction with hydrogen ions from the HC₉H₇O₄ andH₃C₆H₅O₇. In simplified form, the reaction of interest here can then be written as:

HCO₃^-(aq) + H⁺(aq)→H₂CO₃(aq)

The product in this equation, carbonic acid(H₂CO₃), is unstable and quickly breaks down into water (H2O) and carbon dioxide (CO2) gas. Thus, our chemical equation now takes the form:

HCO₃^-(aq) + H⁺(aq)→ H₂O(l) + CO₂(g)

This release of CO₂ gas produces the bubbles seen when we add the tablet to water. Since the CO₂ molecule was originally part of the mass of the Alka-Seltzer® tablet, its release into the atmosphere results in a net loss of mass after the reaction is complete. Thus, if we know the mass of the water and tablet before the reaction and the mass of the remaining mixture after the reaction, the mass of CO₂ lost can be calculated by difference. Since there is a 1:1 ratio of CO₂ to HCO₃^- in the reaction, we can then calculate the amount of NaHCO₃ reacted and determine the mass percent of this species in the original Alka-Seltzer® tablet.

An assumption in the discussion above is that all of the NaHCO₃ in the tablet is reacted when the tablet dissolves. However, one purpose of Alka-Seltzer® is to neutralize excess stomach acid. This can’t happen if all of the NaHCO₃ reacts when the tablet is dissolved! Instead the tablet contains an excess of NaHCO₃. In order to react this excess of NaHCO₃. In order to react this excess acid, we will use acetic acid (HC₂H₃O₂) to stimulate stomach acid. Overall, the experimental reaction is now:

HC₂H₃O₂(aq) + NaHCO₃(s)→ NaC₂H₃O₂(aq) + H₂CO₃(aq)→ H₂O(l) + CO₂(g) +NaC₂H₃O₂(aq)

In order to determine the amount of excess of NaHCO₃, Alka-Seltzer® tablets will be added to eight different solutions, each with a larger amount of acid. By comparing the amount of CO₂ produced by the reaction of Alka-Seltzer® with water tot eh amount of CO₂ produced by the reaction in the acetic acid solutions, the maximum possible mass of NaHCO₃ in a tablet can be calculated. The mass percent, which is defined as shown below, will then be calculated for each trial with a plot of mass percent versus volume of vinegar being generated to experimentally determine the total amount of sodium bicarbonate in an Alka-Seltzer® tablet.

Mass%=	^MassNaHCO3
	MassTablet

Procedures:

Safety Notes: Although the acetic acid being used is not a strong acid, it can cause irritation if gotten in the eyes or left in prolonged contact with your skin. The Alka-Seltzer® can react vigorously enough to “spray” some acid out of the beakers so wear eye protection at all times.

General Instructions: Students should work in teams of four to complete this experiment with each student completing two of the eight runs required. One student will perform steps 1-11 as written below; the others will perform the variations described in step 12. Be sure you have a complete set of data before leaving the laboratory.

1) Weigh a clean, dry 250 ml beaker and small watch glass to the closest milligram, (0.001g) (Use the Top Loader balance on the instructor’s desk). Record the weight in your lab notebook. Considering the question of balance capacity our Analytical balance (0.0001g) has a 60 gram maximum and can not be used. Check the 0.001 Top Loader as it has a capacity to record the glassware and contents. If not use the 0.01 g top loaders on each lab bench.

2) Using a graduated cylinder, place 35 mL of distilled (DI)water in the 250mL beaker you weighed

3) Reweigh the beaker with the water. Make certain the outside of the beaker is dry and use Kimwips to remove any fingerprints or dust etc. Record the weight in your lab notebook.

4) Collect an Alka-Seltzer tablet. Carefully weigh the tablet to the closet milligram.

5) Add the weighed tablet to the beaker with the water in it. Place the pre-weighed watch glass over the top of the beaker to deflect any splatter. Swirl the content to ensure the tablet is dissolved completely.

6) After the reaction appears to be complete (stopped bubbling), use a hot plate set at it lowest heat to heat the beaker and contents slightly. Be careful not to over heat so that no evaporation of water occurs. The heat should drive the reaction to completion. Record the mass of the beaker, the remaining solution and the watch glass.

7) Empty the contents of the beaker down the sink and rinse the beaker with DI water. Dry the beaker and watch glass thoroughly using paper towels and Kimwipes. Check your dry weight to be certain it matches your first weighing, otherwise use the new empty beaker weight in your next calculation.

8) Using a graduated cylinder, place 30mL of distilled (DI) water in the previously weighted 250mL beaker.

9) Using another graduated cylinder add 5 mL of vinegar to the beaker so that the total volume is 35mL. Note- use of two separate graduate cylinders will eliminate the need to clean and dry the cylinder in between additions of each chemical. Swirl the contents of the beaker to mix the solution.

10) Reweigh the beaker with the solution. Make sure the outside of the beaker is dry and use Kimwipes to remove any fingerprints or dust, etc. record the weight in your lab notebook.

11) Add the second tablet to the beaker with the acid mixture in it and cover with the watch glass as before. Swirl the content to ensure the tablet dissolves completely.

12) After the reaction appears complete, reweigh the beaker, its solution, and the watch glass. Again gently heat the solution on the hot plate and reweigh to see if any additional weight loss has occurred (Reaction goes to completion). Record the weight in your lab notebook. (Note if too much weight loss occurs after heating, you possibly vaporized some of the water and use the weighing before heating.

13) Divide the tasks between lab partners and Repeat steps 7-12 Using 10, 15, 20, 25, 30, and 35 mL of vinegar and the appropriate volume of water to give a total of 35mL of solution

Report contents and Questions

The purpose should be two or three sentences stating why this lab was done, including but not limited to key concepts and techniques. Be sure to mention the criteria that will be used to determine success.

The procedure section for this experiment can cite the lab manual but should include notes with any changes made to the experiment during lab, and noting which sections you actually performed and which data came from other students, along with their names.

A data table similar to the example below should be completed and presented in the data section.

It might be time to start having them design their own data table, perhaps as part of the Pre-Lab exercise.

A Completed table such as the one below should be included.

Volume			Mass before Reaction (g)					Mass After Reaction (g)			CO2		NaHCO3
Run	Vinegar	Water	Tablet	Beaker	Beaker and solution	Watch Glass	Total Mass	Beaker and Solution	Watch Glass	Mass Glass	Grams	Moles	Moles	Grams	Mass %
1	0	35
2	5	30
3	10	25
4	15	20
5	20	15
6	25	10
7	30	5
8	35	0

The mass before reaction and mass after reaction sections should have all been recorded in your lab notebook and copied into your lab report. Be sure that you have the correct number of significant figures for the balance you used.

The CO₂ and NaHCO₃ sections can be calculated using your stoichiometry skills. First determine the correct balanced chemical equation from the background section. Write this equation in your data section above your data table. To determine the grams of CO₂, subtract the total mass after the reaction from the total mass before the reaction. Once you have the grams of CO₂, convert the grams of CO₂ into moles of CO₂ using the molecular weight of CO₂. Then, using the mole ratio from the balanced chemical equation, find the moles of NaHCO₃. Determine the grams of NaHCO₃ using the molecular weight of NaHCO₃. Finally determine the mass % of NaHCO₃.

For the calculation section show one sample calculation for each calculation done to complete the data table. Make sure that this section is typed or written in ink; use correct units. This section should also include the calculation for the percent error in the mass and mass% for each run. This can be determined by using the information provided in the background section regarding the known amount of NaHCO₃ in a tablet. Be sure that all of your units are the same before substituting them into the following equation:

%error=	Ac Actual Value – Experimental X 100%
		Actual value

Also include a graph of the mass% of NaHCO₃ versus mL of the acetic acid, placing mass% of NaHCO₃ on the y-axis and volume of acid on the x-axis. Remember all graphing guidelines apply here; refer to Appendix 2 for further information on graphing. Use the graph to determine the mass % of NaHCO₃ in a tablet by noting where the graph begins to level off. From that value, calculate the graphically determined value for the mass of NaHCO₃ in the tablet. Calculate the % error of the graphically determined value of the mass of NaHCO₃ per tablet compared to the label declaration.

The conclusion section should be several paragraphs in length. It should include a discussion of the trends in mass of CO_2, mass of NaHCO₃, and mass % found from your data table and a comparison with the mass % determined graphically. Be sure to include values in your discussion. The conclusion should also state the minimum volume of acid required to react with all of the NaHCO₃ present in an Alka-Seltzer tablet, and explain how you determined this value. A discussion of the % error in each run should be included as well as any errors in the experiment which may have led to the discrepancies in values.

Answer the following questions:

1. Explain why the mass percent in half a tablet is same as the mass percent in a whole tablet of Alka-Seltzer.

2. Explain how the graph of mass % of NaHCO₃ versus mL of acetic acid helps you determine the amount of NaHCO₃ in an Alka-Seltzer tablet.

RESULTS TABLE

Volume			CO2		NaHCO3
Run	Vinegar	Water	Grams	Moles	Moles	Grams	Mass %	% ERROR
1
2
3
4
5
6
7
8

This will make it easier in your lab notebook and set you up for the report.

Calculating % error

There is an error in the lab handout regarding how to calculate % error. The correct formula is experimental value – actual value / actual value X 100%. This way, the error is a positive number if the experimental value is too high, and is a negative number if the experimental value is too low. Otherwise, the signs do not make sense.

The point of the Lab

In one part of the series of runs, one reactant is limiting and in another part, the other is the limiting reactant. From your results, you can determine which is which and when it switches. This will be illustrated in your graph. Calculate the % error in your graphically determined mass% NaHCO₃ vs. the one calculated from the label statement.

Agenda to Plop, Plop, Fizz, Fizz

The authors of this lab used a balance with capacity of only 100g, making it necessary to weigh the beaker and watch glass separately. We will weigh them together since our balances can weigh in that range, and the weights will be more accurate (less chance of losing some of the liquid clinging to the watch glass).

The reaction is endothermic, meaning it absorbs heat from the surroundings and the reaction mixture cools as the reaction progresses. This causes the reaction to slow down and you could easily think the reaction was over before it was complete. For accurate results, your reaction must go to completion. Turn a hot plate on low heat and place your beaker on it once the first vigorous bubbling ceases. Swirl occasionally and when there is no evidence of more gas evolution, weigh the beaker. Put it back on the hot plate for a few more minutes and see if the weight changes any further. Once you get two identical weights a few minutes apart, the reaction should be done. Be careful not to overheat the mixture as this will cause water vapor to be lost as well as CO₂, and would lead to an overestimate of the mass of CO₂ evolved. Ideally, the solution should be slightly warm, but not hot.

The data table in the lab assumes weighing the watch glass separately, and so includes columns you will not need. Also putting all data and results in a single table makes the table very wide and unwieldy. I suggest you break it into two tables, one for data (experimental numbers) and one for results (calculated numbers), as in the following example:

DATA TABLE

Volume (mL)			Mass After Reaction (g)				Mass after reaction (g)	Mass Difference
Run	Vinegar	Water	½ Tablet	Beaker and W.G.	Beaker, W.G. and solution	Total Mass	Beaker, W.G. and Solution	CO2 evolved (g)
1
2
3
4
5
6
7
8