Formal

Lab Report: Experiment 15: Quality Control for the Athenium Baking Soda Company

A Self-Directed Experiment

Erin Floresca

CHEM 1225 AMES

February 14, 2018

1
Introduction

If we were to bequeath the title of being a miracle product to an everyday item that can

be found in most households, the honor would probably go to baking soda. Baking soda, also

known as sodium bicarbonate (NaHCO3), is a relatively cheap compound that has a multitude of

uses in everyday life. It can zap bad smells, keeps teeth sparkly and white, make your bread rise

and even treat an upset stomach. It is able to neutralize acids and can break down many

proteins. Its ability to act as a neutralizer makes it a very effective deodorizer.

The Athenium Baking Soda Company had chosen to produce baking soda by reacting

crystalline ammonium hydrogen carbonate with brine as shown in the equation below (Eq. 1).

NH4HCO3(S) + NaCl(aq) à NaHCO3(aq) + NH4Cl(aq) (Eq. 1)

However, while brine consists mainly of sodium chloride dissolved in water, it can also contain

contaminants such as potassium chloride, lithium chloride and calcium chloride. Because of

this, when aqueous baking soda is dried and filtered, residues of these contaminants may be

present in the final product. To maintain quality during the manufacturing process, it is

important that Athenium Baking Soda Company perform periodic inspections to determine the

purity and composition of the baking soda it produces.

In this self-directed experiment, chemical analytical techniques will be employed to

determine the purity and composition of a sample of baking soda provided by the company.

The central question that this experiment will answer is, “What experimental techniques can be

used to determine the purity of a given sample of baking soda, and, if there are impurities,

determine the identity of the impurities?” Specifically, the goal is first to determine the percent

by mass of pure baking soda in the sample. Then, if the baking soda sample is found to be

impure, the next step is to identify the impurities present in the sample. The experimental

2
procedure would also address safety precautions necessary to ensure a smooth and accident-

free procedure. Additional questions such as how to ensure the accuracy of results will also be

addressed. To determine the percent by mass of pure sodium bicarbonate (NaHCO3) in the

sample, Thermal Gravimetric Analysis and Titration will be used. The identity of contaminants in

the sample will be determined using Emission Spectroscopy.

Thermal Gravimetric Analysis

Thermal gravimetric analysis is a laboratory procedure that finds the percent by mass of

a component in a mixture (Atwood, Stanton & Zhu). For this experiment, a known mass of the

sample baking soda will be added to a crucible and heated until it decomposes into its

components: solid sodium carbonate, gaseous carbon dioxide and water vapor as shown in Eq.

2 below.

∆
2NaHCO3(s) à Na2CO3(s) + CO2(g) + H2O(g) (Eq. 2)

The loss of mass from the sample mixture will be monitored until there is no longer any

detectable loss of mass after a heating cycle, at which point the reaction has gone to

completion and is said to be heated to a constant mass. Basically, the sample will be heated for

15–20 minutes for the first heating- cooling cycle, then cooled to room temperature. The

sample and its container are weighed. The sample is heated a second time for approximately 5

minutes, and again cooled to room temperature. The sample and its container are reweighed. If

the mass difference between the first and second heating-cooling cycles is no greater than

0.005 g or 0.01 g (depending on whether the balance measures to the nearest 0.001 g or 0.01

g), the sample has reached constant mass. Otherwise, a third 5-minute heating-cooling cycle is

3
required. Heating-cooling cycles are continued until the mass difference between two

consecutive cycles differ by no more than 0.005 g or 0.01 g.

When the sample baking soda mixture is heated to a sufficiently high temperature, the

sodium bicarbonate component in the mixture decomposes to form gaseous compound(s). The

other component(s) in the mixture will not decompose upon heating. The mass of the

component that decomposes is stoichiometrically related to the mass of the gaseous

compound(s) liberated. The balanced equation shown in Eq. 2 indicates that 1 mole of carbon

dioxide gas and 1 mole of water vapor are released when 2 moles of sodium bicarbonate

decompose. The determination of the mass of water vapor and carbon dioxide in this

decomposition reaction is shown below:

Mass of H2O lost per gram of NaHCO3

1.00 g NaHCO3 x (1 mol NaHCO3/84.01g NaHCO3) x (1 mol H2O/2 mol NaHCO3) x

(18.02 g H2O/1 mol H2O) = 0.1072g H2O (Eq.3)

Mass of CO2 lost per gram of NaHCO3

1.00 g NaHCO3 x (1 mol NaHCO3/84.01g NaHCO3) x (1 mol CO2/ 2 mol NaHCO3) x

(44.011 g CO2/1 mol CO2) = 0.2619g CO2 (Eq.4)

The total mass loss per gram of NaHCO3(s) heated is equal to the combined mass of H2O and CO2

lost:

0.1072g H2O + 0.2619g CO2 = 0.369 g of H2O and CO2 per gram of NaHCO3 (Eq. 5)

4
We will use the above stoichiometrically-determined ratio information to determine the mass

of NaHCO3 in the given sample of baking soda by multiplying it with the total mixture mass loss

after heating, as follows:

mass of H2O and CO2 liberated X (1 gram of NaHCO3/0.369 g of H2O and CO2) (Eq. 6)

Then, given the mass of pure NaHCO3 in the sample (Eq. 6), we can determine the percent mass

of NaHCO3 in the mixture by dividing it by the mass of the initial mixture placed in the crucible.

A computed value of less than 100% would indicate that there are contaminants in the sample.

Titration

The molarity and percent by mass of NaHCO3 can also be determined by performing a

titration. A titration is a process in which small increments of a solution of known concentration

are added to a specified volume of solution of unknown concentration until the stoichiometry

for that reaction is attained. The concentration of the unknown solution can be determined

using the quantity of the known solution required to complete the titration ((Atwood, Stanton

& Zhu). The purpose of the titration is to determine the equivalence point of the reaction,

which is reached when the quantity of one reactant is the exact amount necessary for

stoichiometric reaction with another reactant. For this experiment, the equivalence point

occurs when the moles of the base in the solution equals the moles of acid added in the

titration. A sudden change in the pH of the solution would signal that the equivalence point has

been reached.

For this experiment, we will titrate an NaHCO3 solution with a standardized HCl solution.

The HCl solution will be standardized by first preparing a primary standard base solution. This

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will be done by dissolving a weighed quantity of a pure base in a known volume of solution. We

will be using Na2CO3 as our primary standard base. To standardize a solution of HCl, a known

mass of Na2CO3 will be dissolved in enough water to completely dissolve it. A buret will be used

to titrate HCl into a beaker containing the Na2CO3 solution. The molarity of the HCl solution is

first determined by calculating the number of moles Na2CO3 dissolve in solution, as shown in

Eq. 7 below:

Na2CO3 (aq) + 2HCl(aq) à 2NaCl (aq) + H2O(l) + CO2 (Eq. 7)

This equation indicates that two moles of HCl is required to neutralize one mole of

Na2CO3. This stoichiometric ratio and the moles of Na2CO3 in solution will be used to calculate

the number of moles of HCl required to neutralize the Na2CO3. The volume of HCl used in the

titration is determined at the equivalence point from a plot of pH of the solution VS ml of HCl

added. The molarity of the HCl solution is calculated by dividing the moles HCl by the volume of

HCl in liters used to neutralize the Na2CO3 solution.

Once the Na2CO3 has been standardized, it will be used to titrate an aliquot of NaHCO3.

The equation for the reaction of sodium bicarbonate with HCl is:

NaHCO3(aq) + HCl(aq) à NaCl(aq) + H2O(l) + CO2(g) (Eq. 8)

Knowing the standardized HCl concentration and using Eq. 8, we can determine the molarity

and percent by mass of NaHCO3 in the solution.

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Emission Spectroscopy

Emission spectroscopy will be used to identify impurities (potassium chloride, lithium

chloride and calcium chloride) present in the sample baking soda, assuming the first 2

experiments confirmed that there are contaminants in the baking soda solution. In this

procedure, we will first determine the wavelengths in nm of the ions in the calcium chloride,

potassium chloride and lithium chloride samples provided by way of emission spectroscopy.

Then, using emission spectroscopy again, the most intense wavelengths present in an aqueous

sample of baking soda will be determined and compared against the emission wavelengths of

the contaminant metal ions. This process will allow determination of the metal ions actually

present in the sample of baking soda.

Safety Precautions

Students must wear departmentally-approved eye protection while performing the

experiments. Hands should be washed before touching eyes and after completing the

experiment. Waste should be disposed in the appropriate waste container(s). Do not leave the

lid off the waste can. Do not touch hot crucible, clay triangle or the iron ring with bare hands.

Place them on a wire gauze to cool. Avoid splattering 6 M HCl from the crucible. HCl is very

corrosive. If HCl contacts your skin, immediately wash the affected area with copious quantities

of water and inform your lab instructor.

7
Experimental

Materials

List of Chemicals List of Special Equipment

Sodium Carbonate (solid, primary standard MeasureNet spectrometer cuvettes, nichrome
base) wires
Baking Soda sample (mixture MeasureNet pH probe and drop counter
Approx. 1.0 M HCl solution Volumetric flasks
0.1 M Calcium chloride solution Beral pipettes
0.1 M Potassium chloride solution Kim wipes
0.1 M Lithium Chloride solution Crucible and lid

Steps:

Thermal Gravimetric Analysis (Atwood, Stanton & Zhu)

Obtain a crucible and lid. Clean the crucible by adding 2-3 milliliters of the given HCl solution.

Leave the HCl in the crucible for 2-3 minutes. Use a spatula to remove any residual material in

the crucible to remove any residual material in the crucible. Pour the acid and residual into the

waste container. Rinse the crucible with copious quantities of water. Decant the water into a

laboratory sink and thoroughly dry the crucible. Place a clay triangle on an iron ring supported

by a ring stand. Suspend the crucible and lid inside the clay triangle. Place the lid on the

crucible slightly ajar, do not completely cover the crucible. Heat the crucible with a Bunsen

burner for 5 minutes; the bottom of the crucible should glow red. Using crucible tongs

completely cover the crucible with the lid, and carefully place the hot crucible and lid on wire

gauze. Let the crucible cool to room temperature. Determine the mass of the cool crucible and

lid. Add approximately 1 gram of the baking soda mixture to the crucible. Determine the exact

mass of the baking soda mixture, crucible, and lid. From this measurement, determine the
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mass of the baking soda mixture itself. Place the crucible containing the mixture in the clay

triangle. Heat the baking soda mixture gently for 5 minutes. Adjust the air intake of the burner

to remove the inner blue cone of the flame to reduce the flame temperature. Periodically, use

crucible tongs to raise the lid and view the mixture. If the sample begins to melt, reduce the

temperature. After 5 minutes of gentle heating, adjust the burner air intake to produce a

distinct inner blue cone of the flame and vigorously heat for 15 minutes. Heat the mixture to

constant mass. Determine exact mass of the baking soda mixture, crucible, and lid after every

heating-cooling cycle until constant mass is reached. Record measured mass to the correct

number of significant figures according to the scale. Repeat the steps with a second 1 gram

sample of the baking soda mixture to perform a second trial to determine the percent by mass

of NaHCO3 in the mixture. Clean the crucible with given HCL solution and pour the acid and

residual material into the “Waste Container.” Rinse the crucible with water, decant water into a

sink, and thoroughly dry the crucible and lid. Calculate the stoichiometric ratio for the loss of

carbon dioxide (CO2) and water (H2O) for every gram of NaHCO3 that was decomposed.

Determine the CO2 and H2O liberated in the experiment. Calculate the mass of carbon dioxide

and water loss during heating for each trial. Calculate the mass of sodium hydrogen carbonate

in sample for each trial. Calculate the percent by mass of sodium hydrogen carbonate in sample

for each trial. Calculate the percent by mass of the impurities.

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Titration

Part A: Preparing standardized solution of HCl

The first titration is conducted to figure out the exact molarity of the HCl solution. The solution

will be about 1M, but in order for calculations to be accurate, do this titration. The molar ratio

of HCl and Na2CO3 will be 2:1 because of the following equation:

Na2CO3 + 2HCl à 2NaCl + CO2 + H2O

Prepare the solution by mixing one gram of solid Na2CO3 with 25-30 mL of distilled water.

Record the exact amount of solid Na2CO3 and the mL of water on your data sheet. Prepare the

pH electrode, buret assembly, and drop counter. Rinse a 50-mL buret with distilled water. Then

use 3-4 mL of the HCl solution to further rinse the buret. Pour the HCl in the

waste container provided. Make sure that the cockstop is sealed on the buret

and proceed to fill the buret with 50.00 mL of the HCl solution. Turn on and

calibrate the workstation. Once this has been done, enter the temperature of

the buffer solution provided, which has a pH of 7.00, into the work station.

Then press “Enter.” When the pH value stabilizes, being somewhere around

7.00, press “Enter.” Accept all values entered. Next, take the pH electrode out of the buffer

solution. Rinse the electrode with distilled water and use a KimWipe to dry the tip of the

electrode. Support the pH probe by the drop counter and put it into the beaker containing the

sodium carbonate solution. If the tip of the pH probe is not submerged, add water to cover the

tip of the probe. Make sure at least 1.5 cm of the probe tip is submerged. Place the beaker with

the Na2CO3 solution on a magnetic stirrer and place a stir bar into the solution. Turn on the

magnetic stirrer to a low setting. Position the buret filled with HCl over the beaker of the

10
solution so that when the drops leave the buret they will go through the notch of the drop

counter that has been provided. Press Start, and read the volume of the HCl in the buret. Read

the volume off of the buret and enter that in as the initial volume at the workstation. Enter

exactly what the buret reads. Such as if you filled to the 0.0 ml mark you enter 0.0 as your initial

volume. Press “Enter.” Slowly open the buret valve to begin adding HCl such that the drop rate

is slow enough that each individual drop is counted. When the titration has finished (the graph

has leveled out), close the stopcock on the buret and press the “Stop” button on the

workstation. Enter the final volume (in milliliters) of HCl in the buret. Press “Enter.” Save the

graph and record and label the file name then press “Enter” to save your graph. Remove the stir

bar from the solution. You should next ask your T.A. whether to decant the solution in the

beaker into the lab sink or into the waste container. Rinse the pH probe and stir bar with

distilled water and wipe off with a Kimwipe. Clear the previous scan to get the workstation

ready for the next titration. Calculate the molarity of HCl and record it on your data sheet. Use

the following calculations (the mole ratio will depend on which inflection point you use):

(# of grams of Na2CO3) x (1mol Na2CO3 /105.9 g Na2CO3) = mol of Na2CO3

(mol of Na2CO3) x (2 mol HCl/1 mol Na2CO3) = mol HCl

(mL of HCl solution) x (1L/1000mL) = L of HCl

(Mol HCl/L HCl) = Molarity of solution

Part B: Titration of NaHCO3

At this point, we know the molarity of the standardized HCl solution, so we can now titrate the

NaHCO3 in order to calculate the percent by mass of the NaHCO3.

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Prepare a solution by mixing 1 gram of solid NaHCO3 with 25-30 mL of distilled water. Record

the exact amount of NaHCO3 and the mL of water on the data sheet. Repeat steps from Part A

using the baking soda solution in place of the sodium carbonate solution to complete the

titration of NaHCO3. Once the titration is complete, dispose of the HCl in the waste container.

Also, dispose of the baking soda solution in the sink and rinse with water. Clean the buret

thoroughly with distilled water. Turn off the workstation, and put away all materials. The

following equation will be used in order to determine the percent by mass of NaHCO3:

NaHCO3 + HCl à NaCl + CO2 + H2O

Calculate the moles of HCl that reacted by using the calculations from Part A. Calculate the

moles of NaHCO3 neutralized by the moles of HCl, and the molarity of the NaHCO3 solution by

using the following equations:

• (mol of HCl) X (1 mol NaHCO3 /1 mol HCl)= mol NaHCO3

• (mL of NaHCO3) X (1 L/1000 mL)= L NaHCO3

• (mol NaHCO3 /L NaHCO3) = Molarity of NaHCO3

Calculate the mass of NaHCO3 in the solution, and then divide the number grams of NaHCO3 by

the grams of solution and multiply the result by 100 in order to calculate the percent by mass.

Record this on the data sheet. Calculate the percent by mass of the impurities, by subtracting

the percent by mass of the NaHCO3 from 100%.

Emission Spectroscopy

Turn the spectrometer. Set to Emission. Set up minimum and maximum scan parameters: Y axis

min 0 max 1500, X axis to default settings. Clean the nichrome wire (dip it into 5 mL of 6 M HCl

12
in a beaker and swish around for 30-40 seconds, then rinse with water); pour used acid into a

waste container. Zero the spectrometer (until it is ready to scan. Press Intensity. Hold the

nichrome wire over the flame of a Bunsen burner until it is bright orange; the spectrometer

should display an instantaneous reading of between 2500 an 4000; press Intensity again. Place

a small amount of distilled water in a watch glass; heat the nichrome wire again until it is bright

orange. Place the watch glass slightly tilted near the air intake of the Bunsen burner; place the

heated nichrome wire in the water so that it spatters/evaporates into the air intake; repeat 3-4

times; this rinses the inside of the burner of any residue from previous experiments. Place 1 mL

of the first standard ion solution (calcium) into a watch glass; heat the nichrome wire again and

repeat the process, pressing Sample immediately before placing the nichrome wire in the

solution to spatter it into the air intake of the burner; record the color of the flame on the Data

Sheet. Pour any leftover standard ion solution into the waste container and rinse the watch

glass. Save the data into a file and record the number you saved the file as, and email them to

members of your group. Clear the scan and begin a new one. Clean the nichrome wire again and

repeat the steps for the standard ion solutions of potassium and lithium, and for the baking

soda solution. Clean the Bunsen burner one last time. To plot the spectrums recorded on the

spectrometer, open an Excel worksheet and open the files of the scans (File Open); click Next

through the three steps of the Text Import Wizard. Highlight columns A and B, click Insert, and

choose to graph it in XY smooth line scatter plot. Click Layout and press Chart Title, Above

Chart (the title is the name of the plot). Click Axis Title, Primary Horizontal Axis Title, Title

Below Axis; enter Wavelength, nm as the title of the x axis. Click Axis Title, Primary Vertical

Axis Title, Rotated Title; enter Intensity as the title of the y axis. Repeat the steps for the

spectra of the potassium and lithium standard ion solutions and the baking soda solution; Copy

13
and Paste to a Word document and Print. Complete the table of wavelengths emitted by each

standard metal solution, and record the color of the flame on the Data Sheet. Perform

calculations for the energy of light emitted per atom for the 2 most intense emission

wavelengths observed in each emission spectrum, then record on the Data Sheet. Identify the

impurities present in the baking soda (either calcium, potassium, or lithium salts) by comparing

emission wavelengths of the three standard solutions with the emission spectrum of the baking

soda solution.

Results

Thermal Gravimetric Analysis

UNKNOWN #: 117

Trial 1 Trial 2
Mass of crucible and lid 18.450 g 20.660g
Mass of crucible, lid and mixture 19.417 g 21.277 g
Mass of mixture 0.9670 g 0.6170 g
Mass of crucible, lid and residue after 15 minutes 19.135 g 21.093 g
heating
Mass of crucible, lid, and residue after 1st 3-minute 19.104 g 21.061 g
heating
Mass of crucible, lid, and residue after 2nd 3-minute 19.103 g 21.060 g
heating

1. Calculate the stoichiometric ratio for the mass loss of carbon dioxide and water per gram of

sodium bicarbonate (Equations 3, 4,5).

Na: 23 X 1 = 23 H: 1.01 X 2 = 2.02 C: 12.01 X 1 = 12.02

H: 1.01 X 1= 1.01 O: 16 X 1 = 16 O: 16 X 2 = 32
C: 12.01 X 1 = 12.01 18.02 moles of H2O/g of H2O 44.02 moles of CO2/ g of CO2
O: 16 X 3 = 48
84.02 moles of NaHCO3/g of
NaHCO3

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Mass of H2O lost per gram of NaHCO3

1.00 g NaHCO3 x (1 mol NaHCO3/84.02g NaHCO3) x (1 mol H2O/2 mol NaHCO3) x

(18.02 g H2O/1 mol H2O) = 0.1072 g H2O (Eq.3)

Mass of CO2 lost per gram of NaHCO3

1.00 g NaHCO3 x (1 mol NaHCO3/84.02g NaHCO3) x (1 mol CO2/ 2 mol NaHCO3) x

(44.02 g CO2/1 mol CO2) = 0.2619g CO2 (Eq.4)

The total mass loss per gram of NaHCO3(s) heated is equal to the combined mass of H2O and CO2

lost: 0.1072g H2O + 0.2619g CO2 = 0.3691 g of H2O and CO2 per gram of NaHCO3 (Eq. 5)

2. Determine the total mass of carbon dioxide and water lost upon heating for each trial.

Trial 1 Trial 2
Beginning Mass of crucible, lid and mixture 19.417 g 21.277 g
Ending Mass of crucible, lid and mixture after 19.103 g 21.060 g
Heating #3
Total Mass Lost 0.3140 g 0.2170 g

3. Calculate the mass of sodium bicarbonate in the mixture for each trial (Equation 6).

Trial 1 Trial 2
mass of H2O and CO2 0.3140 g X (1 g NaHCO3/0.3691 g 0.2170 g X (1 g NaHCO3/0.3691
liberated X (1 gram of of H2O and CO2) = 0.8507 grams g of H2O and CO2) = 0.5879
NaHCO3/0.369 g of H2O of NaHCO3 grams of NaHCO3
and CO2)

15
4. Calculate the percent by mass of sodium bicarbonate by dividing the mass computed in the

previous step above by the mass of the initial mixture placed in the crucible.

Trial 1 Trial 2
Percent by Mass of NaHCO3 (0.8507 g/0.9670 g) X 100 = (0.5879 g/0.6170 g) X 100 =
= (amount of NaHCO3 in the
mixture/starting mass of the 87.97% 95.28%
mixture) X 100

5. Calculate the average percent by mass of sodium bicarbonate by averaging the values

obtained in step 9 for trial and trial 2.

Average Percent by Mass of NaHCO3 = (87.97% + 95.28%)/2 = 91.625%

6. Percent by mass of impurities: 100% -91.625% = 8.375%

Titration

Part A: (See Graphs 1 and 2)

Data: Standardization of HCl with Na2CO3

Trial 1 Trial 2
ml of distilled water used to dissolve 27.5 ml 29.5 ml
Na2CO3
Na2CO3 mass 1.007 g 1.017 g
Starting Volume of HCl 24.5 ml 2.3 ml
Ending Volume of HCl 46.1 24.5

Grams per mole of Na2CO3

Na: 23 X 2 = 46
C: 12 X 1 = 12
O: 16 X 3 = 48
106 g/mol

16
Na2CO3 (aq) + 2HCl(aq) à 2NaCl (aq) + H2O(l) + CO2
Trial 1 Trial 2
Equivalence Point (volume of Na2CO3 14.078 ml = 0.014078 L 15.042 ml= 0.015042 L
used to neutralize HCl
Molarity of HCl 1.007 g Na2CO3 X (1 mol 1.017 g Na2CO3 X (1 mol
Na2CO3/106 g Na2CO3) X (2 Na2CO3/106 g Na2CO3) X
mol HCl/1 mol Na2CO3) X (2 mol HCl/1 mol Na2CO3)
(1/0.014078 L of HCl)= X (1/0.015042 L of HCl) =
1.35 M 1.28 M
Average Molarity of HCl : (1.35 M + 1.28 M)/2 = 1.32 M

Part B: (See Graphs 3 & 4)

Data: Titration of NaHCO3 with standardized HCl data

Trial 1 Trial 2
ml of solution 28.0 ml 25.0 ml
mass of NaHCO3 1.099 g 1.077 g
Starting Volume of HCl 6.3 ml 15.4 ml
Ending Volume of HCl 15.4 35.9

Note: For Part B of the titration, two(2) trials were performed. Unfortunately, the graph for

trial 1 appears to be invalid, i.e., no obvious equivalent point (see graph 3). So, it was decided

that only data from trial 2 will be used for analysis.

Trial 1 Trial 2
Volume of HCl required to neutralize NaHCO3 See note 7.5750 ml
Calculate the molarity of NaHCO3 0.40M
Calculate the percent by mass of the baking soda 78.00%

Percent by Mass of impurities in the mixture 22.00%

17
Computations:

Grams per ml of NaHCO3

Na: 23 X 1 = 23
H: 1 x 1= 1
C: 12 X 1 = 12
O: 16 X 3 = 48
-----------------------
84 grams/mol of NaHCO3

Molarity of NaHCO3

Trial 1: not computed; invalid data

Trial 2:

(1.32 mol of HCL/1 L of HCl) X 0.007575 L X (1mol NaHCO3/1 mol HCl) X (1/0.0250) = 0.40 M

Molarity of NaHCO3 = 0.40 M

Percent by Mass of NaHCO3 in the mixture

Trial 1: not computed; invalid data

Trial 2: (1.32 mol of HCl/1 L of HCl) X 0.007575 L HCl = 9.999 X10-3 mol HCl

NaHCO3(aq) + HCl(aq) à NaCl(aq) + H2O(l) + CO2(g)

Moles of NaHCO3 in the mixture = 9.999 X10-3 mol HCl

(9.999 X10-3 mol HCl of NaHCO3 ) X (84 g of NaHCO3/ mol of NAHCO3) = 0.8400 g of NaHCO3

(0.8400 g of NaHCO3/1.077 g of NaHCO3 mixture) X 100 = 78.00%

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Percent by Mass of NaHCO3: 78.00%

Percent by mass of impurities: 100.00% - 78.00 = 22.00%

Emission Analysis

(Standards: Graphs 5, 6, 7; unknown: Graph 8)

Standard Present in
Wavelength(s)\ Solution?
Metal Ion (in nm) (Y/N)
Ca2+ 623.20 no

K+ 766.65, 589.42 yes

Li+ 671.02 no
NaHCO3 589.42, 766.65 n/a

Discussion

Using both thermal gravimetric analysis (TGA) and titration, we have determined that

the sample of NaHCO3 tested contains impurities. Thermal gravimetric analysis results show

that the average percent by mass of NaHCO3 in the mixture is 91.625%, which implies that

8.375% of the mixture is accounted for by contaminants. Titration of the NaHCO3 mixture with

standardized HCl showed that the percent by mass of NaHCO3 is 78.00%, which confirms the

result of the thermal gravimetric analysis that the baking soda sample contains impurities. The

roughly 14% difference between the results from TGA and titration is most likely due to

experimental errors. Note that for the titration portion of the experiment, data from only one

trial (trial 2) was used for analysis because the other trial yielded invalid results (no discernible

equivalence point). Emission analysis confirmed that there are indeed contaminants in the

sample of NaHCO3. Two distinct wavelengths were found in the emission spectrum of the

19
sample baking soda: 589.42 nm and 766.65 nm. Comparing these wavelengths to the

wavelengths of the metal ions of the 3 potential contaminants, it appears that the contaminant

is potassium chloride (KCl), as the spikes in wavelengths match those found in the baking soda

sample (589.42 nm and 766.65 nm, respectively).

There are possible sources of error in this laboratory experiment. One possible source of

error is that the nichrome wire used for the emission spectroscopy portion of this experiment

was not completely purged of impurities in between samples. This would give erroneous and

confusing wavelength readings. To minimize the possibility of impurities affecting the results of

the experiment, it is best to follow the steps for cleaning the nichrome wire as detailed in the

procedure section prior to introducing any analyte on the nichrome wire. Mislabeling error is

another potential source of invalid results. If the samples are not labeled appropriately, the

samples could get mixed up, giving rise to bad experimental data (garbage in, garbage out). To

minimize labeling errors, it is good practice to label samples as they are being prepared. Also,

care should be taken to not melt the baking soda sample in the thermal gravimetric analysis

procedure; molten Na2CO3 can react with silica in the crucible releasing additional CO2, which

will lead to an erroneous percent by mass of NaHCO3 in the mixture.

Conclusion

In summary, this experiment attempted to ascertain the purity of a sample of baking

soda from the Athenium Baking Soda Company using Thermal Gravimetric Analysis and

Titration. The purity of the sample is judged according to the percent by mass of baking soda

actually present in the sample. 100% percent by mass would mean that the sample is 100%

pure. In this case, the percent by mass obtained from both Thermal Gravimetric Analysis and

Titration were less than 100%, which indicates that the sample is not 100% pure. Thermal

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Gravimetric Analysis revealed that the sample is 91.625% pure while titration gave a much

lower value of 78.00%. Once it was determined that the sample contained impurities, emission

spectroscopy was used to determine the identity of the contaminants. Emission spectroscopy

showed that potassium chloride account for the impurities in the sample. To answer the central

question presented at the beginning of this lab report, both thermal gravimetric analysis and

titration are useful in determining the purity of a chemical sample. As data from the experiment

show, titration results confirmed the results from the thermal gravimetric analysis(TGA) – that

the baking soda sample contains impurities. The wide difference (91.625% for TGA VS 78.00%

for Titration) in percent by mass obtained from the 2 procedures could be attributed to

experimental errors, which could be minimized by careful labeling of samples, accurate

measurements and recording, and meticulous cleaning of tools between samples. The bottom

line is that both procedures confirmed that the baking soda sample tested contains impurities.

To determine the identity of contaminants in the sample, emission spectroscopy was used to

compare the emission wavelengths found in the baking soda sample with the emission

wavelengths of the three common contaminants in the brine that was used in the production of

baking soda; i.e., potassium chloride, lithium chloride and calcium chloride. In this experiment,

we found that potassium chloride is the contaminant in the sample baking soda.

Bibliography

Atwood, C., Stanton, B. and Zhu, L. (2010). Experiments in General Chemistry Featuring

MeasureNet. 2nd ed. California, USA: Cengage Learning.

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