Section L01
Determination of Bismuth in Pepto-Bismol Tablets by Gravimetric
Analysis and Flame Atomic Absorption Spectrometry
Lindsey McNaughton
Unknown #70
Dates Performed: 9/18-10/02 2017
ABSTRACT
Bismuth subsalicylate (BiS) tablets were dissolved in
HCl to form Bi3+(aq) solutions. Gravimetric analysis
by precipitation of BiPO4(s) and flame atomic
absorption spectrometry were then used to measure the
amounts of bismuth in aqueous solutions. A maximum
of 68.34% recovery of bismuth subsalicylate was
obtained indicative of error in technique. The
application of FAAS provided a blank correction
calibration plot with the linear formula 

y = 0.0142x + 0.0037 and approximately 260.6mg of
bismuth subsalicylate per tablet.
Keywords:
Gravimetric Analysis, Flame Atomic Absorption
Spectrometry, Quantitative Analysis, Bismuth
Subsalicylate
1. INTRODUCTION
Bismuth subsalicylate (abbreviated BiS), found in
Pepto-Bismol, has antibacterial properties and is often
used to treat gastrointestinal discomfort. The
recommended dosage for adults of this over the
counter drug is 262 - 1050mg every hour as needed.
Overdose of bismuth can have adverse effects;
therefore, it was the aim of this experiment to quantify
the amount of bismuth subsalicylate in each tablet in
comparison to the manufacturer’s claims. To test the
amount of bismuth found in each tablet, gravimetric
analysis and flame atomic absorbance spectrometry
were performed.
Gravimetric analysis can be used to quantify the
unknown compound by precipitating BiPO4 with the
application of Le Chatleier’s principle. The initial
reaction of BiS with hydrochloric acid leaves salicylic
acid as a byproduct after releasing the bismuth
oxychloride[1].
Unknown Results: 169.0mg BiS
Date Submitted: 10/16/2017

Although bismuth oxychloride is an insoluble
compound, applying Le Chatelier’s principle forces the
reaction to the left in the presence of a strong acid.
Bi3+(aq) + Cl-(aq) + H2O ⇌ BiOCl(s) + 2H+
Once the aqueous bismuth is reacted with excess
phosphate ions, solid bismuth phosphate is formed and
can be quantified using gravimetric analysis.
Bi3+(aq) + PO43-(aq) → BiPO4(s)
Flame atomic absorption spectrometry is a common
technique for detecting metals in samples. This
selective spectroscopic approach can be used to
measure the amount of bismuth in aqueous solutions. A
calibration equation plot can then be used to to
calculate the mass of bismuth present.
2. EXPERIMENTAL PROCEDURE
This experiment was divided into three sections
performed one section per week for a period of three
weeks.
2.1 Week One (9/18)
Three Pepto-Bismol tablets and 1 unknown sample in
solution were used in this experiment. The tablets were
quantitatively analyzed (Appendix A) prior to and
after crushing each tablet individually with a mortar
and pestle with the intent of recovering as much as
possible. Each tablet was treated as a separate sample (
1, 2, 3, and unknown) and dissolved in a volumetric
flask using approximately 5 mL of 2 M HCl. The
samples were diluted with 0.2 M HCl. The flask was
agitated until the reaction was complete, and the
samples were stored for one week.
2.2 Week Two (9/25)
Sample 1 was set aside to be used in flame atomic
absorbance spectrometry (FAAS) during week three
procedures. The remaining samples were treated
individually for precipitation and required additional 2
M HCl to remix the solution. The samples were
transferred to a larger beaker and rinsed with additional
HCl to ensure recovery of Bi3+. A minimum of 3.62mL
of Na3PO4(aq) was needed; however, 20mL was added
to each beaker before the results were observed
(Appendix A). Concentrated NH3 was then added by
drop until the pH was approximately 8-9 and a
precipitate formed. The samples were then filtered

through a membrane filtration unit with the use of a
vacuum. The filtered membranes were dried in the
oven for approximately 25 minutes, weighed, and dried
an additional 5 minutes. Once it was confirmed the
samples were dry, a final mass was taken and percent
recovery of the samples was calculated (Appendix B).
2.3 Week Three (10/02)
To conclude the procedures, flame atomic absorbance
spectrometry (FAAS) was performed using a Bismuth
stock solution (Bi2O3 with a concentration of 1.1148g/
L in 0.2M HCl) provided by the instructor. A set of
standard solutions were prepared by serial dilution
with 2 M HCl containing the approximate
concentrations (mg/L) of 0, 2, 5, 10, and 20 of the
stock solution (Appendix C). The control solution
(sample 1) was also diluted with 2 M HCl. Using the
linear formula generated from the absorbance readings
of the FAAS, the concentration of the control solution
was calculated (Appendix D).
3. RESULTS
Gravimetric analysis of Sample 2 yielded 158.9mg of
bismuth subsalicylate with a 60.63% recovery of the
262mg BiS present in the tablets while Sample 3
yielded 179.1mg with a 68.34% recovery. The average
percent recovery for these samples was 64.49% and
was used to estimate the amount of BiS present in
unknown sample number 70 to be 169.0mg. The mean
mass of bismuth subsalicylate recovered was 169.0mg
with a standard deviation of 10.09mg.
Flame atomic absorbance spectrometry (FAAS)
provided the linear equation y = 0.0142x + 0.0037
where R2= 0.9992. Sample 1 used as a control yielded
concentration of bismuth of 3.711mg/L and 64.19mg
BiS with a 24.50 % recovery.
5. DISCUSSION
The analysis of bismuth subsalicylate found in tablets
of Pepto-Bismol by gravimetric analysis were below
the manufacture’s claim of 262mg per tablet with an
average recovery of 169.0mg or 64.49%. This low
percent recovery is indicative of error in laboratory
technique for gravimetric analysis.
On average, 0.05mg was lost during the initial crushing
of tablets, and a majority of the mass was lost during
the precipitation steps. Bismuth residue may have been
lost in the transfer from the volumetric flask to the
filtration membrane or the sample may not have been
properly dried, thus the mass of dry precipitates taken
for final calculations were inaccurate. Consistency
with the equipment used could have also contributed to
improperly weighed samples as the same scale was not
used between measurements due to conflicting spatial
requirements.
Section L01
The yield provided by FAAS was less consistent with
the manufacturer’s claim that approximately 262mg of
bismuth subsalicylate was present per tablet. This
analysis indicated that 64.19mg BiS was present in
Sample 1 with a 24.50% recovery. According to
Agilent Technologies, possible sources of error during
FAAS include a partially blocked nebulizer which can
occur if the solution contains a high dissolved solids
content or particulate matter. It is also necessary to
frequently agitate the solution to ensure particulate
matter is dispersed throughout solution[3]. It is possible
due to inadequate technique these errors were
expressed, resulting in a low absorbance.
6. CONCLUSIONS
Gravimetric analysis as performed in this experiment
was ineffective in accurately determining the amount
of bismuth subsalicylate due to inconsistencies in
technique, and provided on average 64.49% recovery.
Unknown number 70 was calculated to contain an
estimated 169.0mg of BiS according to gravimetric
analysis. Quantification through flame atomic
absorbance spectrometry was less effective in
determining the amount of BiS in the samples with
only 24.50% recovery. When performed correctly, the
combination of both techniques would be useful in the
quantification of bismuth subsalicylate present in
tablets offered over the counter as accurate
quantification of bismuth present is beneficial in the
prevention of toxic metal poisoning and proper dosage
recommendations.
7. ACKNOWLEDGEMENTS
I would like to thank Dr. Szechenyi for his assistance
in understanding the material of this lab and Emily for
her preparation of our laboratory materials. I would
also like to thank Laura Kinney for her contributions to
creating the standard solutions used during week three.
8. REFERENCES
[1] Davis, E.; Cheung, K.; Pauls, S.; Dick, J.; Roth, E.;
Zalewski, N.; Veldhuizen, C.; Coeler, J. Gravimetric
Analysis of Bismuth in Bismuth Subsalicylate Tablets:
A Versatile Quantitative Experiment for Undergraduate
Laboratories. Journal of Chemical Education 2015, 92
(1), 163–166.
[2] Szechenyi, S. Experiment #4: Determination of Bi
(Bismuth) in Pepto-Bismol tablets by gravimetric
analysis and flame atomic absorption spectrometry.
CHE 3010 Analytical Chemistry Laboratory 2017.
[3] Brodie, K.; Rowland, J. A Simple Fault-Finding
Guide to Flame Atomic Absorption Spectrometry.
Application Note 2010, Agilent Technologies.
www.agilent.com/chem
 Section L01

APPENDICES

 Section L01

Appendix A: Gravimetric Data


(data used for subsequent calculations outlined in green)

Unknown Standard
Sample 1 Sample 2 Sample 3 Mean
Sample: Deviation

Weigh Boat 0.795 0.903 0.810 NA

Mass (g)

Whole Tablet 1.465 1.570 1.481 NA

Mass (g)

Whole Tablet 0.6702 0.6674 0.6706 NA 0.6694 0.001744

Mass (g)
without weigh
boat

Powdered 1.441 1.551 1.463 NA

Tablet Mass
(g)

Powdered 0.6464 0.6485 0.6523 NA 0.6491 0.002991

Tablet
Mass(g)
without weigh
boat

Reaction bubble/white cloudiness/ cloudiness/ cloudiness/

Notes foam; filtered white foam; white foam; white foam;
x2 filtered x2 filtered x2 filtered x2

Precipitation Set aside for became became became

Notes FAAS cloudy, added cloudy, added cloudy, added
NH3 to end of NH3 to end of NH3 to end of
reaction reaction reaction

Membrane NA 47.83 48.72 48.06

Tare Mass (g)

Dry NA 47.96 48.87 48.07

Precipitate
Mass (g)

Dry NA 0.1301 0.1473 0.01100 0.09613 0.07423

Precipitate
Mass (g)
without
membrane

Crushed BiS NA 0.1550 0.1742 0.01310 0.1141 0.08799

(g)

Recovered NA 158.9 179.1 169.0 169.0 10.09

BiS (mg)

Percent NA 60.63 68.34 64.49 64.49 3.86

Recovery of
262 mg Bis/
tablet (%)
 Section L01

APPENDIX B: GRAVIMETRIC DATA CALCULATIONS



 Section L01

Appendix C: FAAS Serial Dilution and Sample 1 Absorbance


(data used for calculations outlined in green)

Bismuth trial 1 trial 2 trial 3 trail 4 trail 5 mean Blank Standard

(mg/L) Correction Deviation
(C1)

0.000 0.005000 0.006000 0.005000 0.006000 0.006000 0.005600 0 0.0005477

2.669 0.04700 0.04700 0.04700 0.04700 0.04140 0.0000

5.296 0.08600 0.08800 0.08700 0.08700 0.08140 0.0010

10.72 0.1650 0.1660 0.1660 0.1657 0.1601 0.0006

21.36 0.3100 0.3100 0.3100 0.3100 0.3044 0.0000

Sample 1 0.06200 0.06200 0.06200 0.06200 0.06200 0.06200 0.05640 0.0000

(X) = 3.711

Blank Corrected Calibration Plot

0.4
y = 0.0142x + 0.0037
R² = 0.9992
0.3
Absorbance

0.2

0.1

0
0.000 7.500 15.000 22.500 30.000
Concentration (mg/L)
 Appendix D: FAAS Data and Calculations

(data used for calculations outlined in green)

Bismuth weigh tare (g) addition of V1 (mL) Dilution with V2 (mL) C2 = C1V1/V2
Concentration solution (mL) HCl (mL) (mg/L)
(mg/L) (C1)

1148 15.16 16.08 0.9130 64.24 49.07 21.36

21.358 15.24 40.03 24.79 64.64 40.41 10.72

10.7183 15.45 39.99 24.54 65.12 49.67 5.296

5.29644 15.21 40.05 24.84 64.50 49.28 2.669

Sample 1: 15.28 15.79 0.5114 64.52 49.24 3.711

Calculated
value from
C2: 357.3