Proposal for Quality

Control for Athenium

Baking Soda Company
CHEM 1211L, MS. NHI BUI, FRIDAY 8:00 AM
SELF DIRECTED EXPERIMENT 15
MARAH KORTH, SIDDHARTH GORE, SLOAN ANDERSON, BRANDY
SMITH, AND TRISTAN REED
OCTOBER 25TH, 2013

Introduction
Sodium bicarbonate, H2CO3, has numerous uses in our world. More
commonly known as baking soda, it is one of the most versatile compounds
out there, having countless applications in both day-to-day life as well as
industrial usage. For years, baking soda has been an essential tool in
countless home remedies and quick fixes. Examples range from using this
amazing substance as a deep-cleaning shampoo to brushing your teeth for
removing stains. Baking soda is also used widely in cooking as a leavening
agent- an agent which releases carbon dioxide and causes baked goods to
rise as they cook. In addition, it has many industrial applications, such as in
the textile and leather industries where it is an integral component of dyeing
and printing processes. (Discovery Health)
The Athenium Baking Soda Company produces this greatly in-demand
substance on an industrial scale. Due to the fact that they need to make
such large amounts of baking soda on a daily basis, they use the following
reaction wherein ammonium carbonate is added to aqueous sodium chloride,
known as brine in the industry:
NH4HCO3 (s)+ NaCl (aq) NaHCO3(aq)+ NH4Cl (aq)
Following this reaction, the products are dried to form the familiar
powdered state which is then ready for packaging. However, this process is
not flawless. The Athenium Baking Soda Company uses brine which,
although majorly composed of sodium chloride, also contains trace amounts
of the chlorides of calcium, potassium, and lithium. Observing the reaction
mentioned above while keeping in mind the reactivity series leads to the
conclusion that these impurities may, in fact, have an effect on the purity of
the solid baking soda that is produced. One must consider that a companys
main goal is to make a profit, and therefore economic considerations also
play a role in the process that the company has chosen. Although it is
economically unfeasible and almost virtually impossible to produce a 100%

pure product on an industrial scale, it is still of utmost importance that the

actual percentage of purity of the product is constantly checked in order to
make sure that it is within an acceptable range. In order to determine the
purity of the baking soda that the company is producing, a meta-analysis of
data collected from three different methods have been suggested in order
increase the accuracy and reliability of the results.
Thermal gravimetric analysis will be the first method employed to test
the purity of a sample of the baking soda provided by Athenium. In this
method, a sample of the product is heated in a crucible over a heat source.
This results in the baking soda decomposing according to the following
equation:
2NaHCO3 (s) Na2CO3 (s) + CO2 (g) + H2O (g)
By measuring the initial and final masses of the amount of substance
present in the crucible, the ratio of the combined masses of the gases that
are liberated to the mass of sodium carbonate can be determined. Using
stoichiometry and the known equation of the decomposition of baking soda,
it is possible to determine the difference and theoretical and experimental
values, and this error can be expressed as a percentage of the purity of the
compound. Ideally, it should be 100%, however if there are impurities, the
percentage deviate above or below this value. This is due to the fact that
KCl, LiCl, and CaCl2 have a different molar mass than NaHCO3. The equation
is assuming that reactant is pure NaHCO3, and therefore its molecular mass
will be used for calculations. Therefore, if impurities are present, they will
reflect as an increase in the discrepancy between the theoretical and
experimental values. However, this method on its own is not enough to
definitively comment on the purity of the baking soda. Therefore, additional
methods will be used to add a sense of certainty to the results.
As a second method of investigating the purity of the baking soda, a
titration will be carried out. First, a measured mass of solid sodium

carbonate, NaCO3, will used to prepare an aqueous solution. This solution will
be titrated the hydrochloric acid, HCl, which is a strong acid. Using
stoichiometry and the equation below, the true molarity of the HCl solution
can be ascertained.
Na2CO3 (aq) + 2HCl (aq) 2NaCl (s) + H2O (aq) + CO2 (g)
A carefully measured mass of the sample of baking soda from the
company will now be converted into an aqueous solution as well. The HCl will
now be used to titrate the aqueous solution of the sample, a process which is
described in detail in the Procedure section. Using a digital pH probe and a
drop counter, a titration curve can be plotted. The curve will initially start at
the pH of the aqueous sample of the baking soda. As baking soda is a base,
the pH will be high. As HCl is added drop by drop, the pH should be seen to
decrease at a slowly increasing rate, until it sharply drops down below the
equivalence point. By analyzing this curve, it is possible to determine what
mass of baking soda was required to reach equivalence point. If the baking
soda was pure, this value would be the same as the value that would be
expected by stoichiometric methods using the known mass of the sample
that was used to make the aqueous solution. If it is different, however, it is
clear that there is an impurity. Using the data, the percentage of the baking
soda that is actually NaHCO3 can be calculated. However, if it is found that
there are impurities, it would still be unclear as to what impurities are
actually present in the sample.
Looking at the data from the previous experiments, it will be clear at
this point whether or not the sample is contaminate or not. To identify which
of the chlorides are present in the sample, a third method called an emission
analysis will be conducted. It is given that the contaminants could be the
chlorides of lithium, potassium, or calcium. In this method, the presence of
the metal cations of these chlorides will be examined. Using emission
analysis on reference solutions of K+, Ca2+, and Li+, emission spectra will be

produced to be used for comparison. The most intense wavelengths on the

emission spectrum for each of the metal cations will be noted down. By
conducting an emission analysis on the baking soda sample and comparing
the emission spectrum that is produced to the values from the reference
solutions of the metal cations, it can be determined which of the metal
cations are present.
Having used these three separate methods to collect data, a holistic
analysis can be done in order to determine which, if any, of the impurities
are present in the sample of baking soda. In addition, the purity of the baking
soda can be determined as a percentage. This data is sure to help Athenium
Baking Soda Company evaluate whether or not the product they are
producing is of an acceptable grade.

Chemicals Required for Investigation:

1.)
2.)
3.)
4.)
5.)
6.)

Sodium carbonate
Baking soda sample
Approximately 1.0 M hydrochloric acid solution
0.1 M Calcium chloride solution
0.1 M Potassium chloride solution
0.1 M Lithium chloride solution

Special Equipment Required for Investigation:

1.)
2.)
3.)
4.)
5.)
6.)

MeasureNet spectrophotometer, cuvettes and nichrome wires

MeasureNet pH probe and drop counter.
Volumetric flasks
Beral pipets
Kimwipes1
Crucible and lid
Safety Precautions:
As in all cases of dealing with chemicals, extreme care must be taken when
transferring, measuring, moving, and interacting with the chemicals in any
way. Numerous chemicals in this lab are very corrosive, such as hydrochloric

acid. Lab goggles should be worn at all times. Ensure that clothing covers all
extremities and that all individuals are wearing close toed footwear.

Part I
Thermal Gravimetric Analysis will be used to determine if there are any
impurities in the baking soda sample provided. When baking soda (Na2CO3)
decomposes (as a result of being heated to a high enough temperature), it
yields sodium carbonate (Na2CO3), carbon dioxide gas (CO2), and water vapor
(H2O). This is its chemical formula:
2NaHCO3(s) Na2CO3(s) + CO2(g) + H2O(g)
After this reaction occurs, the final weight should only consist of the sodium
carbonate (Na2CO3).

Procedure:
1.) The first step in Part I of this experiment is to determine the
stoichiometric ratio of the mass loss of carbon dioxide gas and water vapor
per one gram of NaHCO3.
1.000 grams NaHCO3 x

44.0 grams CO 2
1 mole CO 2

1 mole CO 2
2 moles NaHCO 3

= .2619 g CO2 liberated

1.000 grams NaHCO3 x

18.0 grams H 2 O
1 mole H 2O

1 mole NaHCO 3
84.0069 grams NaHCO 3

1 mole NaHCO 3
84.0069 grams NaHCO 3

1mole H 2 O
2 mole NaHCO 3

= .1071 g H2O liberated

.2619 g + .1071 g = .369 g of CO2 and H2O liberated

Stoichiometric Ratio for the mass loss of CO2 and H20 per gram of NaHCO3:
1.000 grams NaHCO 3
.369 grams CO 2H 2O
According to these mathematical calculations, if 1.000 gram of NaHCO3
(baking soda) is heated, 0.369 grams of CO2 and H20 should be liberated.
The remaining sample should only consist of Na2CO3 (sodium carbonate) and
should only weigh .631 grams (1.000 0.369).
2.) Clean a crucible and its lid with approximately 2- 3 milliliters of a 6 M
hydrochloric acid solution (HCl). Leave the HCl in the crucible for around a
few minutes so that it can dissolve residue of past experiments and then use
a spatula to remove any residual material. Dispose of the HCl in the Waste
container.
3.) Rinse the crucible with plenty of water in lab sink.
4.) Put a clay triangle on the ring stand. Then place the crucible and its lid
inside the clay triangle. Place the lid on the crucible slightly ajar.
5.) For 5 minutes, heat the crucible with a Bunsen burner (bottom of crucible
should glow red).
6.) Now, fully cover the crucible with its lid and remove the crucible from the
ring stand with a pair of tongs. Place it on wire gauze to cool.
7.) Once the crucible is cool, weigh it (with its lid on) on a scale. Record this
number.
8.) Then, add 1 gram of the baking soda sample. Then weigh the crucible
(with lid still on) again with the baking soda sample in it. Record the exact
mass from the balance.
9.) Put the crucible back onto the clay triangle.

10.) Heat the sample gently for five minutes. Then for 15 minutes, heat
the crucible vigorously.
11.) After 15 minutes of heating, remove the crucible from the clay triangle
and place it back on the wire gauze. Wait for it to cool.
12.) Once the crucible has cooled weigh it on a scale (with lid on).
13.) Repeat the required steps. For second heating, only heat for 5 minutes.
Let it cool and reweigh it again (lid still on).
14.) If the difference in mass is no greater than 0.01 grams (or .005 grams),
your sample has reached constant mass. If not, continue the heating and
cooling cycle until the mass difference is within the desired limits.
15.) Clean work station. Clean the crucible with the 6 M HCl solution. Then
rinse the crucible with water. Dispose of the HCl in the waste container.
16.) Determine the mass of CO2 and H2O liberated in this experiment. You
do this by subtracting the initial weight of the crucible (with lid on and
sample in it) with the final weight of the crucible (after however many
heatings). The change in weight accounts for the CO2 and H2O liberated from
sample.
17.) Now, multiply the amount of CO2 and H2O liberated by the stoichiometric
ratio for the mass loss of CO2 and H2O per 1 gram of NaHCO3 (calculated
earlier). This answer will give you the mass of baking soda that has
decomposed in order to release the gases. To calculate the purity of the
sample as a percentage, do the following:
Mass percentage of NaHCO3= (Calculated mass/Initial mass) 100%
Then, the mass percentage of impurities is nothing but:
100% - ((Calculated mass/Initial mass) 100%)

Data Collection for Part 1:

1. Record the data for the trials using the data table provided below.
Mass of crucible (with lid) (g)
Mass of crucible (with lid) and sample
(g)
Mass of crucible (with lid) and sample
(1st heating) (g)
Mass of crucible (with lid) and sample
(2nd heating) (g)
Mass of crucible (with lid) and sample
(3rd heating) (g)

2. What is the stoichiometric ratio for loss of carbon dioxide and water per
gram of sodium bicarbonate?

3. Using the recorded initial and final masses, calculate the mass of water
and carbon dioxide that were liberate when the sample was heated for
each of the trials.

4. What is the percent of NaHCO3 per unit mass of the sample? Therefore,
what percentage of the sample is made up of impurities?

Part II
A titration will be carried out as a second method to determine the purity of
the sample. Note the following:
The neutralization of Na2CO3(aq) with HCI(aq) occurs in two steps.
Na2CO3(aq) + HCI(aq) NaHCO3(aq) + NaCl(aq)
NaHCO3(aq) + HCI(aq) NaCl(aq) + CO2(g) + H2O(I)
The pH graph of this reaction, therefore, has two equivalence points. The first
is seen when the first mole of HCl has reacted with the sodium carbonate to
form one mole each of sodium bicarbonate and sodium chloride, and this is
the one that will be considered for this experiment. The pH at the
equivalence point of this reaction happens to correspond very closely to the
pH range where phenolphthalein changes color, and therefore
phenolphthalein will be used as an indicator.

Procedure:
First, the HCl must be standardized to ascertain its molarity.
Standarization:
1.) Rinse a 100mL beaker, first with tap water and then with distilled or
deionized water.
2.) Separate a small mass of the Na2CO3, approximately 1g. Record the exact
mass using a top pan balance.
3.) Add the Na2CO3 to a beaker, being careful not to drop any, and then add
about 25 mL of water to the beaker.
a. Make sure to rinse the tip of a 50-mL burette with distilled water.
Rinse the burette with 3-4mL of HCl. Then dispose of the HCl.
b. Making sure the buret is closed filled the burette with 50.00mL of
HCl. Make sure there are no air bubbles in the burette.
c. Set up the MeasureNet to record pH versus volume.
d. Press Main Menu, then press F3 pH/mV then press F2 pH v.
Volume.
e. Make sure the MeasureNet pH probe is in a beaker of pH 7.00
buffer solution. Press calibrate, enter the temperature, then
press Enter.
f. To accept all values press Display.
g. Remove the pH electrode from the buffer solution, rinse with
distilled water, and dry with a Kimwipe. Test the pH probe with
the acid solution. The pH probe should read that the pH of the
acid is less than 2.
h. Place the probe in the acid solution making sure the tip of the
probe is about 1-2 cm from the bottom of the beaker.
i. Place the stir bar in the beaker making sure the stir bar does not
touch the probe.
j. Place the burette over the beaker and the eye of the drop
counter.
k. Start the stirring on a medium speed.
l. Press Start on the MeasureNet. Enter the initial volume making
sure if the burette is completely filled to enter 0.00 mL

(Remember: the readings of the volume of burettes are

backwards). Then press Enter.
m. Press Start and open the burette value and begin adding the HCl
drop-wise. Make sure every time the drop goes through the eye
of the drop counter and blinks red.
n. The titration is concluded when the pH falls sharply then levels
off around the pH 1-3 range. Once titration is concluded close the
burette then press Stop.
o. Read the final volume of the burette, input it into the MeasureNet
then press Enter.
p. To save the file press File Options, then F3. Enter a 3 digit code to
name the file then press Enter.
q. Dispose of the solution in the beaker into the Waste Container
making sure to remove the stir bar from the beaker first.
r. Rinse off the stir bar and the pH probe with distilled water.
s. Place the pH probe back into the pH 7 buffer solution.
t. Dispose of the rest of the HCl in the Waste Container and rinse
the burette with distilled water.
u. Use the data recorded to plot a graph of pH vs. Volume of HCl.
v. Press Display to clear the screen and start a new titration.
4.) Calculate the number of moles of HCl contained in the volume of HCl
used, and record that value. Using the molar mass of Na2CO3, calculate
the number of moles of Na2CO3 that were present in the aqueous solution
in the beaker.
5.) Using stochiometric equations, calculate the molarity of the HCl solution
that was used.
Finding Purity Percentage of the Baking Soda:
Repeat the steps 1-3j. for the previous titration, but instead of Na2CO3, use
the baking soda. Once the volume of HCl required to neutralize the NaHCO3is
ascertained, use the formula:
Moles= Molarity Volume

to find the moles of HCl that participated in the reaction. Use stoichiometry
to find the number of moles of NaHCO3 present in the baking soda. Use the
formula:
Mass= Molar Mass Number of moles
To find the purity of the sample, divide this mass by the mass of the baking
soda sample that was initially recorded.
1.) From the files create a plot of the pH verses volume of HCl in Microsoft
Excel.

Data Collection for Part 2:

Standardization:
Initial volume of HCl for standardization
Final volume of HCl for standardization
Mass of Na2CO3 use for standardization
File name used for standardization
Determination of purity:
Initial volume of HCl for determination of
purity
Final volume of HCl for determination of
purity
Mass of baking soda used for
determination of purity
File name used for standardization

1. From the files saved using the MeasureNet pH probe, prepare graphical
plots of the pH vs Volume plots for both of the titrations conducted.

2. Looking at these graphs, where are the equivalence points? Therefore,

what volume of HCl was needed to titrate the baking soda mixture? Record
all relevant data.

3. Note down the exact mass of baking soda in the solution and the molar
mass of baking soda. Using the formulas given in the procedure, calculate
the mass of baking soda that reacted, and using the initial known mass of
the baking soda sample, determine the purity percentage.

The sample contains

. % of Impurities.

Part III
To identify which of the chlorides are present in the sample, a third method
called an emission analysis will be conducted. Note: Data from previous
emission analysis lab may be used.

Procedure
1. Set up your MeasureNet spectrophotometer by following these steps
a. Be sure the spectrophotometer is on. Then press the On/Off
button to power on the workstation. Press Main Menu, then F5
Spectroscopy, and then F1 Emission.
b. Press Setup and then F1 to set up the limits of the scan, using
the left and right arrow keys move from the min to max and from
X to Y. An * signifies which one will change.
c. The Y axis represents the intensity, or brightness, of the light.
Set the maximum intensity to 1500, and then press Enter. Leave
the minimum at 0.
d. The X axis represents the wavelength and should be left at the
default settings.
e. Finally, press Display to enter values into the MeasureNet. The
station is prepared for an emission recording.
2. Make approximately 1 mL of an aqueous solution of the baking soda by
dissolving approximately 1 gram of the sample in 30 ml of distilled
water. In addition, obtain a nichrome wire.
3. Clean the nichrome wire by using 5 mL of 6 MHCl in a 50 mL beaker.
Swish the wire around in the HCl for 30 40 seconds to remove any
ions from previous experiments.
4. Now rinse the nichrome wire with 30 to 50 mL of distilled water.
Dispose of the HCl in the waste container.
5. Return to the MeasureNet spectrophotometer. Press Station Number
and enter yours by pressing Enter. It should read Ready to scan.
6. Completely cover the fiber optic cable of the MeasureNet with your
finger and press ZERO. Hold your finger there until it reads Ready to
scan.

7. Press Intensity. Heat the nichrome wire over a Bunsen burner flame
until it is glowing orange. Adjust the position of the Bunsen burner so
that the Intensity reading is between 2500-4000. Press Intensity.
Ready to scan should appear.
8. Pour some distilled water into a watch glass. Heat the nichrome wire
until it glows orange.
9. Place the watch glass next to the air intake of the Bunsen burner and
tilt it so the liquid is as close to the air intake as possible. Completely
submerge the hot nichrome wire in the water with the watch glass still
positioned close to the air intake.
10.
Repeat this 3-4 times to rid the Bunsen burner of any
contamination from previous experiments. Clean the wire and the
Bunsen burner every time you change solutions.
11.
Heat the nichrome wire until it glows orange again.
12.
Place approximately 1 mL of the baking soda solution into the
watch glass.
13.
Position it near the air intake and quickly submerge the heated
wire into the solution. You need to have a lab partner to hit Sample the
moment the nichrome wire is submerged.
14.
Record the color of the flame that you can see.
15.
Check the results to see if the intensity is above that of the
original cap of 1500. If it is, then press Setup. Then press F2 to re-plot
and set a new maximum value and then press Display to accept the
new established maximum.
16.
Press File Options and then F3 to save. Enter a 3 digit code to
note the trial. Press Enter.
17.
Press Display to clear the station and turn off the work station
once finished.
18.
Create a graph of the emission using Excel.
19.
Using the peaks of the graph, calculate the joules per atom of
each spike in intensity using the following equation
hc
Energy =
Where c is the speed of light, h is Plancks constant, and is the
wavelength of the light

20.

Once all spikes in intensity are accounted for, use the known

intensities of Lithium, Calcium, and Potassium to determine which of

those chloride compounds are present in the baking soda.

Data Collection for Part 3:

1.) Record the peak wavelength for each of the following metal ions using the
graphs of the emission spectra produced using the MeasureNet system and
Microsoft Excel. If there is more than one peak wavelength, you may record
both. In addition, record the color of their flames. Note: Data from previous
experiments may also be used in this part.
Ca2+

Li+

K+
2.) Using the data above, look at the emission spectrum for the sample and
identify the metal ion(s) present.
Metal ions present in sample

Conclusion:
After having conducted a series of quality control experiments on a sample of
Athenium Baking Soda Companys product, it can be concluded that the baking
soda is

.% pure, and the impurities are due to the presence of

Bibliography:
1.) Stanton, Bobby, Lin Zhu, and Charles H. Atwood. Experiments in General
Chemistry Featuring MeasureNet. Belmont, CA: Thomson Brooks/Cole, 2006. Print.
2.) Anonymous. "Quality Control." STUDYBLUE. N.p., 4 Nov. 2009. Web. 24 Oct.
2013.
3.) "Uses of Baking Soda." Discovery Fit and Health. N.p., n.d. Web. 24 Oct. 2013.